Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
- Original Message - From: "Thomas Kelly" <[EMAIL PROTECTED]> To: Sent: Wednesday, June 07, 2006 3:02 PM Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results Joe, Good idea, but ... no, I don't have any unused Zeolite. I dried them on a cool, clear day low humidity. I find it hard to believe that they could have absorbed 10% of their weight in water from the air but that would account for the weight gain by the control. I'll try drying the zeolite from the control gently ... raise the temp slowly & cool slowly. It seems that regenerating them w. heat (400F) damages the pores expansion and contraction. Gentle heat w. vacuum is the way to go. A vacuum pump may be in my near future. A compressor from a tossed (junk) refrigerator works great for a vacuum pump - I use one all the time to dewater my WVO, and am getting set up to use another for dewatering the finished BD... Just make sure someone (that knows how) has reclaimed the freon in the system before you start hacking the compressor out... I'll try to get close to the original mass. It's raining again. Should we ever get another cool, clear day w. low humidity I'll let the zeolite sit outside in the same shallow baking pans and see if they gain mass. Tom - Original Message - From: "Joe Street" <[EMAIL PROTECTED]> To: Sent: Wednesday, June 07, 2006 3:42 PM Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results Hi Tom; Do you have any unopened zeolite? If it is vacuum dried (and I suspect it is) at the manufacturer, it may gain mass due to adsorption of moisture from the air. Take some out and weigh it and let it sit out in the same conditions as the other stuff you are air drying and then weigh it again. Joe Thomas Kelly wrote: > Hello to all, > > I have some concerns re: my recent results using 3A Molecular Sieve to > dry recovered methanol. > > Concerns: > > 1. I distilled 4 gal ( Containers #1 & 2), and had to interrupt > > the process. > > Last 4 gal were distilled two days later (Containers #3 & 4). > > > > 2. Air drying: The Zeolite from the Control as well as from > > Containers # 1 & 2 were air-dried at the same time, for the > > same duration under “identical” conditions. > > Due to interruption of distillation and a week of rain, the > > Zeolite from Containers 3 & 4 was removed from the methanol > > after the same time period (24 hrs) as C, #1, & #2, but stored > > in covered plastic containers until weather permitted, and then were > air-dried for the same length of time as the others under as similar > > conditions as could be reasonably expected. > > > >I air-dried the Zeolite until it looked uniformly light in color. > > The idea was to simply remove moisture (methanol) from the > > surface. > > > > 3. The Control gained mass. Although the methanol in the > > Control was not a newly-opened barrel, I reason to believe it > > to be reasonably pure. > > I had a concern going into the experiment that > > 3A Molecular Sieve might allow methanol to enter > > (3A = 3 angstrom units ~ size of pores in the beads) It is > > used to dehydrate ethanol. Water molecule = 2.8 angstrom > > units, ethanol = 4.4 angstrom units, methanol = I don’t know. > > I suspected/hoped methanol was larger than the pore size. > > I suspect that water adheres more strongly than methanol to > > the inner walls of the beads and tends to remain attached. > > Additional air-drying Zeolite from C, #1, and #2 (done after > > surface was dry and original measurements were recorded) > > resulted in continued loss in mass. At temps of only > > 72 F (22.2 C) and filtered light I don’t suspect much of the > > weight loss is due to water. > > > > 4. Zeolite, under the best of circumstances (exposed to vapor > > under pressure) can absorb up to 25% of its weight in water. > > Zeolite from container 3 increased in mass 23.1 % and > > zeolite from Container 4 gained 28.8%. What gives? > > > >The results are interesting in that a comparison of the > > zeolite exposed to the recovered methanol to the control > > suggests that there was little water in the first 4 gallons > > recovered. This is corroborated by the fact that I used the > > Control and the first 2 recovered gallons + about 1 gal. from > > the barrel to make a 91L batch of BD that passed the > > “methanol quality” test. I pan to use the second 2 gal. in the > > next batch. (Maybe after a couple of hours of dry zeolite > > treatment). >
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Hi Tom; Well from what I can find methanol should be larger than 3 angstroms BUT I would also be surprised if the zeolite had an absolute pore size. It is probably avareage pore size so it would adsorb a little methanol I would guess. But while ambient air does always contain some water it does not for all intents and purposes contain methanol so your air drying should result in methanol diffusing out of the material eventually whereas water would diffuse out from saturated zeolite (or into dry zeolite)until an equilibrium is reached between external and internal water content. even in the oven you have not removed all of it. In fact you never will. Desorbtion is always an exponential decay scene. An evacuated desicator heated by the sun might work just fine. You might have to re-evacuate it a few times. When doing this if you first backfill the container with a hot dry gas it will help scavenge the water from the system. Admitting air to the hot container will approximate this but heated dry N2 would be preferable. BTW having a vacuum pump around does have a lot of advantages, you are right. For instance storing caustic in a vacuum bell prevents carbonation and also keeps it dry :) Joe Thomas Kelly wrote: > The Zeolite from the Control (3A Molecular Sieve and Methanol > Recovery) increased in mass by 13.6%. This was a bit alarming. > Joe Street suggested that it might be water absorbed from the air > while air-drying. > Tom Irwin suggested that while this is true, it might also have > absorbed methanol, as methanol might be small enough to fit through the > pores of the zeolite. > > Thinking that any methanol absorbed would not bind as strongly as > water to the zeolite, it might be driven off with very gentle heat. > > Oven temp 170F/ 77C > > Time (min) Mass(g)Change in Mass% Change > 0454.0-- > 15 447.6 - 6.4 1.4 > 30 445.4 - 8.6 1.9 > 45 444.5 - 9.5 2.09 > 60 444.1 - 9.9 2.18 > Does the loss of mass @ 170F represent "easy water" or methanol? (only > 2% of the 13.6% change in Control) > (Temp raised to 250F/ 121C) (total change; including 170F) > 0 443.9- >30 438.7 - 5.2 (15.3) >60 434.7 - 9.2 (19.3) >90 433.6- 10.3 (20.4)(4.5) > 120 431.8- 12.1 (22.2)(4.9) > (Temp raised to 350F/ 177C) > 0 431.8 - > 30 424.2- 7.6 (29.8) > 60 415.1-16.7 (38.9) (8.6) > (Temp raised to 400F/ 204C) > 0 415.1 - > 30 403.3-11.8 (50.7) (11.2) > 60 397.7-17.4 (56.3) (12.4) > > 12.4% of the 13.6% gain in mass a lot of energy expended doing so. > > Apologies to anyone who sees this as a waste of time and energy. It > was intended to help save time and energy during methanol recovery. > > Zeolite works best when it is absorbing water from vapors. > Regeneration requires very high energy input. Vacuum should be > included to reduce energy requirements. > Joe Street's idea of a heated trap upstream of the condenser, > collecting water vapor from the methanol vapors, and capable of heat + > vacuum regeneration, in situ, seems the way to go. It is, however beyond > what I had hoped to get away with. > Vacuum pump on a sealed solar oven? > Tom > > > > - Original Message - > *From:* Thomas Kelly <mailto:[EMAIL PROTECTED]> > *To:* biofuel@sustainablelists.org > <mailto:biofuel@sustainablelists.org> > *Sent:* Thursday, June 08, 2006 8:28 AM > *Subject:* Re: [Biofuel] 3A molecular Sieve and Methanol recovery > Results > > Tom Irwin, > You wrote: > " I think methanol may be smaller than 3A just based on your results." > > I was afraid of that, but it would explain the numbers. > > > "I don't know if water is more polar than methanol." > > I think water is more polar than methanol. > + + > H H >
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
The Zeolite from the Control (3A
Molecular Sieve and Methanol Recovery) increased in mass by 13.6%. This
was a bit alarming.
Joe Street suggested that it
might be water absorbed from the air while air-drying.
Tom Irwin suggested that while
this is true, it might also have absorbed methanol, as methanol might be small
enough to fit through the pores of the zeolite.
Thinking that any methanol absorbed
would not bind as strongly as water to the zeolite, it might be driven off with
very gentle heat.
Oven temp 170F/ 77C
Time (min)
Mass(g) Change in Mass % Change
0
454.0
-
-
15
447.6 -
6.4 1.4
30
445.4
-
8.6 1.9
45
444.5
-
9.5 2.09
60 444.1
- 9.9
2.18
Does the loss of mass @ 170F represent "easy water" or
methanol? (only 2% of the 13.6% change in Control)
(Temp raised to 250F/
121C) (total change; including 170F)
0 443.9-
30
438.7 - 5.2
(15.3)
60
434.7 -
9.2 (19.3)
90
433.6-
10.3 (20.4)
(4.5)
120
431.8- 12.1
(22.2)(4.9)
(Temp raised to 350F/ 177C)
0 431.8
-
30
424.2 -
7.6 (29.8)
60
415.1 -16.7
(38.9) (8.6)
(Temp raised to 400F/ 204C)
0 415.1
-
30 403.3
-11.8 (50.7) (11.2)
60
397.7 -17.4
(56.3) (12.4)
12.4% of the 13.6% gain in mass a lot of
energy expended doing so.
Apologies to anyone who sees this
as a waste of time and energy. It was intended to help save time and energy
during methanol recovery.
Zeolite works best when it is
absorbing water from vapors.
Regeneration requires very high
energy input. Vacuum should be included to reduce energy
requirements.
Joe Street's idea of a heated
trap upstream of the condenser, collecting water vapor from the methanol vapors,
and capable of heat + vacuum regeneration, in situ, seems the way to go. It is,
however beyond what I had hoped to get away with.
Vacuum pump on a sealed solar
oven?
Tom
- Original Message -
From:
Thomas
Kelly
To: biofuel@sustainablelists.org
Sent: Thursday, June 08, 2006 8:28
AM
Subject: Re: [Biofuel] 3A molecular Sieve
and Methanol recovery Results
Tom Irwin,
You wrote:
" I think methanol may be
smaller than 3A just based on your results."
I was afraid of that, but it
would explain the numbers.
"I don't know if water is more polar than
methanol."
I think water is more polar
than methanol.
+ +
H
H
O vs.
methanol w. region
-
- of charge
only around the
alcohol (-OH) group
"If not I don't think it will drive
off bound water."
I'm going to gently heat (100 - 150F) the zeolite from
the Control. I think that if there is significant loss of mass, it would be
due to methanol rather than water leaving the beads. If there is little/no
loss of mass, much of the gain was due to atmos. water, as it is
more tightly bound to the inner surface of the zeolite.
" I recall carbon dioxide being one of the most
strongly held gasses."
Interesting, because CO2 is
charged, but not polar i.e.
- O = C
= O - The inner surfaces of Zeolite is
+
charged ?
" I hope this helps."
It gives me direction for something to try
on a rainy day.
If the zeolite does "dry" significantly at low temp,(drove off methanol)
then I'll have some fairly dry sieve to test the effect of absorption of
water from air on mass . cool clear weather forecast for
Sat.
Thanks Tom,
Tom K.
- Original Message -
From:
Tom Irwin
To: biofuel@sustainablelists.org
Sent: Wednesday, June 07, 2006 5:47
PM
Subject: Re: [Biofuel] 3A
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Joe, The "drying" was referring to any methanol that may have wandered in (assuming methanol is small enough to get through the 3A pores.I don't think it adheres very strongly to zeolite. If I could remove the methanol I'd get an idea of the mass gain due to water adsorption. In the zeolite from the Control, I think this would be mainly due to absorption from the air (while air - drying) Maybe you would look at the results I'm about to post and see what you can make of them. Thanks for the info in your previous post. You have made me a believer in the value of vacuum in drying zeolite. Tom Tom - Original Message - From: "Joe Street" <[EMAIL PROTECTED]> To: Sent: Thursday, June 08, 2006 10:14 AM Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results > Hi Tom;; forget about this idea that you can dry zeolite gently at > atmospheric pressure with low temps. You cannot do it man. Water > molecules at STP move at supersonic kinematic velocities! You either > need high temps or vacumm sorry. > > Joe > > Thomas Kelly wrote: > >> Tom Irwin, >> You wrote: >> " I think methanol may be smaller than 3A just based on your results." >> >> I was afraid of that, but it would explain the numbers. >> >> >> "I don't know if water is more polar than methanol." >> >> I think water is more polar than methanol. >> + + >> H H >> O vs. methanol w. region >> - -of charge only around >> the >> alcohol (-OH) group >> >> "If not I don't think it will drive off bound water." >> >> I'm going to gently heat (100 - 150F) the zeolite from the Control. I >> think that if there is significant loss of mass, it would be due to >> methanol rather than water leaving the beads. If there is little/no loss >> of mass, much of the gain was due to atmos. water, as it is more tightly >> bound to the inner surface of the zeolite. >> >> >> " I recall carbon dioxide being one of the most strongly held gasses." >> >> Interesting, because CO2 is charged, but not polar i.e. >> >> - O = C = O - The inner surfaces of Zeolite is >> + charged ? >> >> " I hope this helps." >> >> It gives me direction for something to try on a rainy day. >> If the zeolite does "dry" significantly at low temp,(drove off methanol) >> then I'll have some fairly dry sieve to test the effect of absorption of >> water from air on mass . cool clear weather forecast for Sat. >> Thanks Tom, >> Tom K. >> >> - Original Message - >> *From:* Tom Irwin <mailto:[EMAIL PROTECTED]> >> *To:* biofuel@sustainablelists.org >> <mailto:biofuel@sustainablelists.org> >> *Sent:* Wednesday, June 07, 2006 5:47 PM >> *Subject:* Re: [Biofuel] 3A molecular Sieve and Methanol recovery >> Results >> >> Hi Tom, Joe and all, >> >> Air drying without heat is probably not the best way to go. Zeolites >> will absorb moisture from the air. When I was ai Air products we >> used to heat to 400C under nitrogen flow to a real low dew point >> that I cannot remember exactly but -40 is stuck in my memory. Then >> we would cool it under nitrogen flow then run our gas separations. >> That's probably overkill for water/methanol separations but it was >> pretty much our SOP for zeolites. It they saw air then you >> regenerated prior to a test. >> Some of what you are seeing could be chemisorption of the methanol >> on the surface but the numbers seem too high. I think methanol may >> be smaller than 3A just based on your results. I don't know if water >> is more polar than methanol. If not I don't think it will drive off >> bound water. I recall carbon dioxide being one of the most stongly >> held gasses. I hope this helps. >> >> Tom Irwin >> >> >> >> >> *From:* Joe Street [mailto:[EMAIL PROTECTED] &g
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Hi Tom; Don't be surprised. Water is everywhere. It is chemisorbed onto the surface of everything including metal and ceramic. In ultra high vacuum systems it is getting rid of water that allows pumping into the UHV range (and then hydrogen ...but that mostly comes from the water anyways). Remember that zeolite is extremely convoluted and water molecules bounce around on the surface and wander into the holes where they continue to bounce around in a direction biased by moisture gradient. It is a matter of statistical probabilities but so long as there is less moisture inside, water molecules will continue to wanter into the maze. Drying the zeolite is reversing the process. To encourage this it must be much drier outside the material. Raising temperature decreases relative humidity of the air surrounding the material but it doesn't get rid of the water, it just increases the capacity of that air to adsorb more water. Heating the zeolite also adds kinetic energy to the molecules inside increasing the probability of wandering around to an exit. It is nanotech actually. Vacuum creates a strong bias toward removing water since the vacuum environment is DRY by definition and heat helps speed the process of water finding it's way out of the porous material. Microwave energy can energize water molecules directly but if they get too energetic they may begin to hammer the walls of the labyrinth too enthusiastically and punch holes in the walls (imagine the analogy of drunken engineering students returning from a pub crawl where there were a few too many gorgeous babes). To give you an idea of how they are used commercially look here http://www.lesker.com/newweb/Traps_and_Filters/Foreline_Traps/MolecularSieveTraps/StraightInline_QF_ISOFlange.cfm?CFID=1162010&CFTOKEN=68358832§ion=molecsieve&init=skip That's a long one so make sure you paste the whole line in your browser bar. See how the design allows the material to be placed in line with the vacuum system? It has a built in heater and regenerating it then just involves turning on the heater and pumping on the system for an hour or two until the vacuum improves and the sieves are dry again. These traps are expensive I agree but when you see how they work you could make something yourself if you have the skill. It is nothing complicated, just a vacuum vessel with an internal heater well. The heater is like one of these... http://www.omegaheater.com/pg11.htm Hope it helps Joe Thomas Kelly wrote: > Joe, > Good idea, but ... no, I don't have any unused Zeolite. > > I dried them on a cool, clear day low humidity. I find it hard to > believe that they could have absorbed 10% of their weight in water from the > air but that would account for the weight gain by the control. > > I'll try drying the zeolite from the control gently ... raise the > temp slowly & cool slowly. It seems that regenerating them w. heat (400F) > damages the pores expansion and contraction. Gentle heat w. vacuum is > the way to go. A vacuum pump may be in my near future. > I'll try to get close to the original mass. It's raining again. Should > we ever get another cool, clear day w. low humidity I'll let the zeolite sit > outside in the same shallow baking pans and see if they gain mass. > Tom > >- Original Message - > From: "Joe Street" <[EMAIL PROTECTED]> > To: > Sent: Wednesday, June 07, 2006 3:42 PM > Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results > > > Hi Tom; > > Do you have any unopened zeolite? If it is vacuum dried (and I suspect > it is) at the manufacturer, it may gain mass due to adsorption of > moisture from the air. Take some out and weigh it and let it sit out in > the same conditions as the other stuff you are air drying and then weigh > it again. > > Joe > > Thomas Kelly wrote: > > >>Hello to all, >> >>I have some concerns re: my recent results using 3A Molecular Sieve to >>dry recovered methanol. >> >>Concerns: >> >>1. I distilled 4 gal ( Containers #1 & 2), and had to interrupt >> >>the process. >> >>Last 4 gal were distilled two days later (Containers #3 & 4). >> >> >> >>2. Air drying: The Zeolite from the Control as well as from >> >>Containers # 1 & 2 were air-dried at the same time, for the >> >>same duration under “identical” conditions. >> >>Due to interruption of distillation and a week of rain, the >> >>Zeolite from Containers 3 & 4 was removed from the methanol >> >>after the same time period (24 hrs) as C, #1, &
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Hi Tom;; forget about this idea that you can dry zeolite gently at atmospheric pressure with low temps. You cannot do it man. Water molecules at STP move at supersonic kinematic velocities! You either need high temps or vacumm sorry. Joe Thomas Kelly wrote: > Tom Irwin, > You wrote: > " I think methanol may be smaller than 3A just based on your results." > > I was afraid of that, but it would explain the numbers. > > > "I don't know if water is more polar than methanol." > > I think water is more polar than methanol. > + + > H H > O vs. methanol w. region > - -of charge only around the > alcohol (-OH) group > > "If not I don't think it will drive off bound water." > > I'm going to gently heat (100 - 150F) the zeolite from the Control. I > think that if there is significant loss of mass, it would be due to > methanol rather than water leaving the beads. If there is little/no loss > of mass, much of the gain was due to atmos. water, as it is more tightly > bound to the inner surface of the zeolite. > > > " I recall carbon dioxide being one of the most strongly held gasses." > > Interesting, because CO2 is charged, but not polar i.e. > > - O = C = O - The inner surfaces of Zeolite is > + charged ? > > " I hope this helps." > > It gives me direction for something to try on a rainy day. > If the zeolite does "dry" significantly at low temp,(drove off methanol) > then I'll have some fairly dry sieve to test the effect of absorption of > water from air on mass . cool clear weather forecast for Sat. >Thanks Tom, > Tom K. > > - Original Message - > *From:* Tom Irwin <mailto:[EMAIL PROTECTED]> > *To:* biofuel@sustainablelists.org > <mailto:biofuel@sustainablelists.org> > *Sent:* Wednesday, June 07, 2006 5:47 PM > *Subject:* Re: [Biofuel] 3A molecular Sieve and Methanol recovery > Results > > Hi Tom, Joe and all, > > Air drying without heat is probably not the best way to go. Zeolites > will absorb moisture from the air. When I was ai Air products we > used to heat to 400C under nitrogen flow to a real low dew point > that I cannot remember exactly but -40 is stuck in my memory. Then > we would cool it under nitrogen flow then run our gas separations. > That's probably overkill for water/methanol separations but it was > pretty much our SOP for zeolites. It they saw air then you > regenerated prior to a test. > Some of what you are seeing could be chemisorption of the methanol > on the surface but the numbers seem too high. I think methanol may > be smaller than 3A just based on your results. I don't know if water > is more polar than methanol. If not I don't think it will drive off > bound water. I recall carbon dioxide being one of the most stongly > held gasses. I hope this helps. > > Tom Irwin > > > > > *From:* Joe Street [mailto:[EMAIL PROTECTED] > *To:* biofuel@sustainablelists.org > *Sent:* Wed, 07 Jun 2006 16:42:11 -0300 > *Subject:* Re: [Biofuel] 3A molecular Sieve and Methanol > recovery Results > > Hi Tom; > > Do you have any unopened zeolite? If it is vacuum dried (and I > suspect > it is) at the manufacturer, it may gain mass due to adsorption of > moisture from the air. Take some out and weigh it and let it sit > out in > the same conditions as the other stuff you are air drying and > then weigh > it again. > > Joe > > Thomas Kelly wrote: > > > Hello to all, > > > > I have some concerns re: my recent results using 3A Molecular > Sieve to > > dry recovered methanol. > > > > Concerns: > > > > 1. I distilled 4 gal ( Containers #1 & 2), and had to interrupt > > > > the process. > > > > Last 4 gal were disti
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Tom Irwin,
You wrote:
" I think methanol may be smaller
than 3A just based on your results."
I was afraid of that, but it
would explain the numbers.
"I don't know if water is more polar than
methanol."
I think water is more polar than
methanol.
+ +
H
H
O vs.
methanol w. region
-
- of charge
only around the
alcohol (-OH) group
"If not I don't think it will drive off
bound water."
I'm going to gently heat (100 - 150F) the zeolite from the
Control. I think that if there is significant loss of mass, it would be due to
methanol rather than water leaving the beads. If there is little/no loss of
mass, much of the gain was due to atmos. water, as it is more tightly
bound to the inner surface of the zeolite.
" I recall carbon dioxide being one of the most
strongly held gasses."
Interesting, because CO2 is
charged, but not polar i.e.
- O = C =
O - The inner surfaces of Zeolite is
+
charged ?
" I hope this helps."
It gives me direction for something to try on
a rainy day.
If the zeolite does "dry" significantly at low temp,(drove off methanol)
then I'll have some fairly dry sieve to test the effect of absorption of
water from air on mass . cool clear weather forecast for
Sat.
Thanks Tom,
Tom K.
- Original Message -
From:
Tom Irwin
To: biofuel@sustainablelists.org
Sent: Wednesday, June 07, 2006 5:47
PM
Subject: Re: [Biofuel] 3A molecular Sieve
and Methanol recovery Results
Hi Tom, Joe and all,
Air drying without heat is probably not the best way to go. Zeolites will
absorb moisture from the air. When I was ai Air products we used to heat to
400C under nitrogen flow to a real low dew point that I cannot remember
exactly but -40 is stuck in my memory. Then we would cool it under nitrogen
flow then run our gas separations. That's probably overkill for water/methanol
separations but it was pretty much our SOP for zeolites. It they saw air
then you regenerated prior to a test.
Some of what you are seeing could be chemisorption of the methanol on the
surface but the numbers seem too high. I think methanol may be smaller than 3A
just based on your results. I don't know if water is more polar than methanol.
If not I don't think it will drive off bound water. I recall carbon dioxide
being one of the most stongly held gasses. I hope this helps.
Tom Irwin
From: Joe Street [mailto:[EMAIL PROTECTED]To:
biofuel@sustainablelists.orgSent: Wed, 07 Jun 2006 16:42:11
-0300Subject: Re: [Biofuel] 3A molecular Sieve and Methanol
recovery ResultsHi Tom;Do you have any unopened
zeolite? If it is vacuum dried (and I suspect it is) at the
manufacturer, it may gain mass due to adsorption of moisture from the
air. Take some out and weigh it and let it sit out in the same
conditions as the other stuff you are air drying and then weigh it
again.JoeThomas Kelly wrote:> Hello to
all,> > I have some concerns re: my recent results using 3A
Molecular Sieve to > dry recovered methanol.> >
Concerns:> > 1. I distilled 4 gal ( Containers #1 & 2),
and had to interrupt> > the process.> > Last 4
gal were distilled two days later (Containers #3 & 4).> >
> > 2. Air drying: The Zeolite from the Control as well as
from> > Containers # 1 & 2 were air-dried at the same
time, for the> > same duration under “identical”
conditions.> > Due to interruption of distillation and a week
of rain, the> > Zeolite from Containers 3 & 4 was removed
from the methanol> > after the same time period (24 hrs) as C,
#1, & #2, but stored> > in covered plastic containers
until weather permitted, and then were > air-dried for the same
length of time as the others under as similar> > conditions as
could be reasonably expected.> > > > I air-dried
the Zeolite until it looked uniformly light in color.> > The
idea was to simply remove moisture (methanol) from the> >
surface.> > > > 3. The Control gained mass.
Although the methanol in the> > Control was not a newly-opened
barrel, I reason to believe it> > to be reasonably
pure.> > I had a concern going into the
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Joe, Good idea, but ... no, I don't have any unused Zeolite. I dried them on a cool, clear day low humidity. I find it hard to believe that they could have absorbed 10% of their weight in water from the air but that would account for the weight gain by the control. I'll try drying the zeolite from the control gently ... raise the temp slowly & cool slowly. It seems that regenerating them w. heat (400F) damages the pores expansion and contraction. Gentle heat w. vacuum is the way to go. A vacuum pump may be in my near future. I'll try to get close to the original mass. It's raining again. Should we ever get another cool, clear day w. low humidity I'll let the zeolite sit outside in the same shallow baking pans and see if they gain mass. Tom - Original Message - From: "Joe Street" <[EMAIL PROTECTED]> To: Sent: Wednesday, June 07, 2006 3:42 PM Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results Hi Tom; Do you have any unopened zeolite? If it is vacuum dried (and I suspect it is) at the manufacturer, it may gain mass due to adsorption of moisture from the air. Take some out and weigh it and let it sit out in the same conditions as the other stuff you are air drying and then weigh it again. Joe Thomas Kelly wrote: > Hello to all, > > I have some concerns re: my recent results using 3A Molecular Sieve to > dry recovered methanol. > > Concerns: > > 1. I distilled 4 gal ( Containers #1 & 2), and had to interrupt > > the process. > > Last 4 gal were distilled two days later (Containers #3 & 4). > > > > 2. Air drying: The Zeolite from the Control as well as from > > Containers # 1 & 2 were air-dried at the same time, for the > > same duration under “identical” conditions. > > Due to interruption of distillation and a week of rain, the > > Zeolite from Containers 3 & 4 was removed from the methanol > > after the same time period (24 hrs) as C, #1, & #2, but stored > > in covered plastic containers until weather permitted, and then were > air-dried for the same length of time as the others under as similar > > conditions as could be reasonably expected. > > > >I air-dried the Zeolite until it looked uniformly light in color. > > The idea was to simply remove moisture (methanol) from the > > surface. > > > > 3. The Control gained mass. Although the methanol in the > > Control was not a newly-opened barrel, I reason to believe it > > to be reasonably pure. > > I had a concern going into the experiment that > > 3A Molecular Sieve might allow methanol to enter > > (3A = 3 angstrom units ~ size of pores in the beads) It is > > used to dehydrate ethanol. Water molecule = 2.8 angstrom > > units, ethanol = 4.4 angstrom units, methanol = I don’t know. > > I suspected/hoped methanol was larger than the pore size. > > I suspect that water adheres more strongly than methanol to > > the inner walls of the beads and tends to remain attached. > > Additional air-drying Zeolite from C, #1, and #2 (done after > > surface was dry and original measurements were recorded) > > resulted in continued loss in mass. At temps of only > > 72 F (22.2 C) and filtered light I don’t suspect much of the > > weight loss is due to water. > > > > 4. Zeolite, under the best of circumstances (exposed to vapor > > under pressure) can absorb up to 25% of its weight in water. > > Zeolite from container 3 increased in mass 23.1 % and > > zeolite from Container 4 gained 28.8%. What gives? > > > >The results are interesting in that a comparison of the > > zeolite exposed to the recovered methanol to the control > > suggests that there was little water in the first 4 gallons > > recovered. This is corroborated by the fact that I used the > > Control and the first 2 recovered gallons + about 1 gal. from > > the barrel to make a 91L batch of BD that passed the > > “methanol quality” test. I pan to use the second 2 gal. in the > > next batch. (Maybe after a couple of hours of dry zeolite > > treatment). > > Tom > > > > > > - Original Message - > *From:* Thomas Kelly <mailto:[EMAIL PROTECTED]> > *To:* biofuel@sustainablelists.org > <mailto:biofuel@sustainablelists.org> > *Sent:* Wednesday, June 07, 2006 11:41 AM > *Subject:* Re: [Biofuel] 3A molecular Sieve and Methanol recovery > Results > > Hello all, > > > 3A Molecular Sieve and Methanol Recovery > > I first s
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Hi Tom, Joe and all, Air drying without heat is probably not the best way to go. Zeolites will absorb moisture from the air. When I was ai Air products we used to heat to 400C under nitrogen flow to a real low dew point that I cannot remember exactly but -40 is stuck in my memory. Then we would cool it under nitrogen flow then run our gas separations. That's probably overkill for water/methanol separations but it was pretty much our SOP for zeolites. It they saw air then you regenerated prior to a test. Some of what you are seeing could be chemisorption of the methanol on the surface but the numbers seem too high. I think methanol may be smaller than 3A just based on your results. I don't know if water is more polar than methanol. If not I don't think it will drive off bound water. I recall carbon dioxide being one of the most stongly held gasses. I hope this helps. Tom Irwin From: Joe Street [mailto:[EMAIL PROTECTED]To: biofuel@sustainablelists.orgSent: Wed, 07 Jun 2006 16:42:11 -0300Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery ResultsHi Tom;Do you have any unopened zeolite? If it is vacuum dried (and I suspect it is) at the manufacturer, it may gain mass due to adsorption of moisture from the air. Take some out and weigh it and let it sit out in the same conditions as the other stuff you are air drying and then weigh it again.JoeThomas Kelly wrote:> Hello to all,> > I have some concerns re: my recent results using 3A Molecular Sieve to > dry recovered methanol.> > Concerns:> > 1. I distilled 4 gal ( Containers #1 & 2), and had to interrupt> > the process.> > Last 4 gal were distilled two days later (Containers #3 & 4).> > > > 2. Air drying: The Zeolite from the Control as well as from> > Containers # 1 & 2 were air-dried at the same time, for the> > same duration under “identical” conditions.> > Due to interruption of distillation and a week of rain, the> > Zeolite from Containers 3 & 4 was removed from the methanol> > after the same time period (24 hrs) as C, #1, & #2, but stored> > in covered plastic containers until weather permitted, and then were > air-dried for the same length of time as the others under as similar> > conditions as could be reasonably expected.> > > > I air-dried the Zeolite until it looked uniformly light in color.> > The idea was to simply remove moisture (methanol) from the> > surface.> > > > 3. The Control gained mass. Although the methanol in the> > Control was not a newly-opened barrel, I reason to believe it> > to be reasonably pure.> > I had a concern going into the experiment that> > 3A Molecular Sieve might allow methanol to enter> > (3A = 3 angstrom units ~ size of pores in the beads) It is> > used to dehydrate ethanol. Water molecule = 2.8 angstrom> > units, ethanol = 4.4 angstrom units, methanol = I don’t know.> > I suspected/hoped methanol was larger than the pore size.> > I suspect that water adheres more strongly than methanol to> > the inner walls of the beads and tends to remain attached.> > Additional air-drying Zeolite from C, #1, and #2 (done after > > surface was dry and original measurements were recorded)> > resulted in continued loss in mass. At temps of only> > 72 F (22.2 C) and filtered light I don’t suspect much of the> > weight loss is due to water.> > > > 4. Zeolite, under the best of circumstances (exposed to vapor> > under pressure) can absorb up to 25% of its weight in water.> > Zeolite from container 3 increased in mass 23.1 % and> > zeolite from Container 4 gained 28.8%. What gives?> > > > The results are interesting in that a comparison of the> > zeolite exposed to the recovered methanol to the control> > suggests that there was little water in the first 4 gallons> > recovered. This is corroborated by the fact that I used the> > Control and the first 2 recovered gallons + about 1 gal. from> > the barrel to make a 91L batch of BD that passed the> > “methanol quality” test. I pan to use the second 2 gal. in the> > next batch. (Maybe after a couple of hours of dry zeolite> > treatment).> > Tom> > > > > > - Original Message -> *From:* Thomas Kelly [EMAIL PROTECTED]>> *To:* biofuel@sustainablelists.org> biofuel@sustainablelists.org>> *Sent:* Wednesday, June 07, 2006 11:41 AM> *Subject:* Re: [Biofuel] 3A molecular Sieve and Methanol recovery> Results> > Hello all,> > > 3A Molecular Sieve and Methanol Recovery> > I first separated the glycerine mix using Phosphoric Acid.> This fragment has a high percentage of the excess methanol> > used to produce methyl esters.> > I then recovered the meth
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Hi Tom; Do you have any unopened zeolite? If it is vacuum dried (and I suspect it is) at the manufacturer, it may gain mass due to adsorption of moisture from the air. Take some out and weigh it and let it sit out in the same conditions as the other stuff you are air drying and then weigh it again. Joe Thomas Kelly wrote: > Hello to all, > > I have some concerns re: my recent results using 3A Molecular Sieve to > dry recovered methanol. > > Concerns: > > 1. I distilled 4 gal ( Containers #1 & 2), and had to interrupt > > the process. > > Last 4 gal were distilled two days later (Containers #3 & 4). > > > > 2. Air drying: The Zeolite from the Control as well as from > > Containers # 1 & 2 were air-dried at the same time, for the > > same duration under “identical” conditions. > > Due to interruption of distillation and a week of rain, the > > Zeolite from Containers 3 & 4 was removed from the methanol > > after the same time period (24 hrs) as C, #1, & #2, but stored > > in covered plastic containers until weather permitted, and then were > air-dried for the same length of time as the others under as similar > > conditions as could be reasonably expected. > > > >I air-dried the Zeolite until it looked uniformly light in color. > > The idea was to simply remove moisture (methanol) from the > > surface. > > > > 3. The Control gained mass. Although the methanol in the > > Control was not a newly-opened barrel, I reason to believe it > > to be reasonably pure. > > I had a concern going into the experiment that > > 3A Molecular Sieve might allow methanol to enter > > (3A = 3 angstrom units ~ size of pores in the beads) It is > > used to dehydrate ethanol. Water molecule = 2.8 angstrom > > units, ethanol = 4.4 angstrom units, methanol = I don’t know. > > I suspected/hoped methanol was larger than the pore size. > > I suspect that water adheres more strongly than methanol to > > the inner walls of the beads and tends to remain attached. > > Additional air-drying Zeolite from C, #1, and #2 (done after > > surface was dry and original measurements were recorded) > > resulted in continued loss in mass. At temps of only > > 72 F (22.2 C) and filtered light I don’t suspect much of the > > weight loss is due to water. > > > > 4. Zeolite, under the best of circumstances (exposed to vapor > > under pressure) can absorb up to 25% of its weight in water. > > Zeolite from container 3 increased in mass 23.1 % and > > zeolite from Container 4 gained 28.8%. What gives? > > > >The results are interesting in that a comparison of the > > zeolite exposed to the recovered methanol to the control > > suggests that there was little water in the first 4 gallons > > recovered. This is corroborated by the fact that I used the > > Control and the first 2 recovered gallons + about 1 gal. from > > the barrel to make a 91L batch of BD that passed the > > “methanol quality” test. I pan to use the second 2 gal. in the > > next batch. (Maybe after a couple of hours of dry zeolite > > treatment). > > Tom > > > > > > - Original Message - > *From:* Thomas Kelly <mailto:[EMAIL PROTECTED]> > *To:* biofuel@sustainablelists.org > <mailto:biofuel@sustainablelists.org> > *Sent:* Wednesday, June 07, 2006 11:41 AM > *Subject:* Re: [Biofuel] 3A molecular Sieve and Methanol recovery > Results > > Hello all, > > > 3A Molecular Sieve and Methanol Recovery > > I first separated the glycerine mix using Phosphoric Acid. > This fragment has a high percentage of the excess methanol > > used to produce methyl esters. > > I then recovered the methanol using a simple still and > condenser. The methanol flowed into containers that each had 5 pounds > > (2270g) of new zeolite. Each container was marked > > such that in addition to the zeolite, there would be 2 gal (7.6L) of > methanol. Container #1 received the first 2 gal of recovered > > methanol, container #2 the next 2 gal, etc. > > My hope was, that by comparing final mass of zeolite to initial > mass, I could get a sense of how much water was coming > > over with the methanol and what was a reasonable cut-off point for > the process. A Control was included. The Control had 5 pounds > > of zeolite plus 2 gal of methanol from a methanol barrel.
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Hello to all, I have some concerns re: my recent results using 3A Molecular Sieve to dry recovered methanol. Concerns: 1. I distilled 4 gal ( Containers #1 & 2), and had to interrupt the process. Last 4 gal were distilled two days later (Containers #3 & 4). 2. Air drying: The Zeolite from the Control as well as from Containers # 1 & 2 were air-dried at the same time, for the same duration under identical conditions. Due to interruption of distillation and a week of rain, the Zeolite from Containers 3 & 4 was removed from the methanol after the same time period (24 hrs) as C, #1, & #2, but stored in covered plastic containers until weather permitted, and then were air-dried for the same length of time as the others under as similar conditions as could be reasonably expected. I air-dried the Zeolite until it looked uniformly light in color. The idea was to simply remove moisture (methanol) from the surface. 3. The Control gained mass. Although the methanol in the Control was not a newly-opened barrel, I reason to believe it to be reasonably pure. I had a concern going into the experiment that 3A Molecular Sieve might allow methanol to enter (3A = 3 angstrom units ~ size of pores in the beads) It is used to dehydrate ethanol. Water molecule = 2.8 angstrom units, ethanol = 4.4 angstrom units, methanol = I dont know. I suspected/hoped methanol was larger than the pore size. I suspect that water adheres more strongly than methanol to the inner walls of the beads and tends to remain attached. Additional air-drying Zeolite from C, #1, and #2 (done after surface was dry and original measurements were recorded) resulted in continued loss in mass. At temps of only 72 F (22.2 C) and filtered light I dont suspect much of the weight loss is due to water. 4. Zeolite, under the best of circumstances (exposed to vapor under pressure) can absorb up to 25% of its weight in water. Zeolite from container 3 increased in mass 23.1 % and zeolite from Container 4 gained 28.8%. What gives? The results are interesting in that a comparison of the zeolite exposed to the recovered methanol to the control suggests that there was little water in the first 4 gallons recovered. This is corroborated by the fact that I used the Control and the first 2 recovered gallons + about 1 gal. from the barrel to make a 91L batch of BD that passed the methanol quality test. I pan to use the second 2 gal. in the next batch. (Maybe after a couple of hours of dry zeolite treatment). Tom - Original Message - From: Thomas Kelly To: biofuel@sustainablelists.org Sent: Wednesday, June 07, 2006 11:41 AM Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results Hello all, 3A Molecular Sieve and Methanol Recovery I first separated the glycerine mix using Phosphoric Acid. This fragment has a high percentage of the excess methanol used to produce methyl esters. I then recovered the methanol using a simple still and condenser. The methanol flowed into containers that each had 5 pounds (2270g) of new zeolite. Each container was marked such that in addition to the zeolite, there would be 2 gal (7.6L) of methanol. Container #1 received the first 2 gal of recovered methanol, container #2 the next 2 gal, etc. My hope was, that by comparing final mass of zeolite to initial mass, I could get a sense of how much water was coming over with the methanol and what was a reasonable cut-off point for the process. A Control was included. The Control had 5 pounds of zeolite plus 2 gal of methanol from a methanol barrel. This was presumed to be relatively pure methanol. This was done in my basement and backyard; not under stringent laboratory conditions. I have some concerns regarding the procedure followed, and the results produced. The following is simply a chart of the results gotten. Feel free to question/comment. Container Initial Mass(g) Final Mass (g) Change % Change % Change in Mass(g) in Mass vs Control Control 2270 2577.7 + 307.7 + 13.6 - 1 2270 2636.3 + 366.3 + 16.1 + 2.5 2 2270 2671.5 + 401.5 + 17.7 + 4.1 3 2270 2795.3 + 525.3 + 23.1 + 9.5 4 2270 2924.4
Re: [Biofuel] 3A molecular Sieve and Methanol recovery Results
Hello all,
3A Molecular Sieve and
Methanol Recovery
I first separated the
glycerine mix using Phosphoric Acid. This fragment has a high percentage of
the excess methanol
used to produce methyl
esters.
I then recovered the
methanol using a simple still and condenser. The methanol flowed into containers
that each had 5 pounds
(2270g) of new
zeolite. Each container was marked
such that in addition to
the zeolite, there would be 2 gal (7.6L) of methanol. Container #1 received the
first 2 gal of recovered
methanol, container #2 the
next 2 gal, etc.
My hope was, that by
comparing final mass of zeolite to initial mass, I could get a sense of how much
water was coming
over with the methanol and
what was a reasonable cut-off point for the process. A Control was included. The
Control had 5 pounds
of zeolite plus 2 gal of
methanol from a methanol barrel. This was presumed to be relatively pure
methanol.
This was done in my basement
and backyard; not under stringent laboratory conditions. I have some concerns
regarding
the procedure followed,
and the results produced. The following is simply a chart of the results
gotten.
Feel free to
question/comment.
Container Initial Mass(g) Final Mass (g) Change
% Change %
Change
in Mass(g) in
Mass
vs
Control
Control
2270
2577.7
+ 307.7
+ 13.6
-
1
2270
2636.3
+ 366.3
+ 16.1 +
2.5
2
2270 2671.5
+ 401.5
+ 17.7
+
4.1
3
2270
2795.3
+ 525.3
+ 23.1
+ 9.5
4
2270
2924.4
+ 654.4
+ 28.8 +
15.2
Container
Temp Range of Mix During Distillation
1
150 165 F (66 - 74
C)
2
165 177 F (74 - 81
C)
3
175
- 188 F (79.5 87
C)
4
188 210 F
(87.5 99 C)
Tom
- Original Message -
From:
Thomas
Kelly
To: biofuel
Sent: Tuesday, May 23, 2006 8:37 AM
Subject: [Biofuel] 3A molecular Sieve and
Methanol recovery
Hello to all,
3A molecular sieve is on
its way. As I understand it, selectively absorbs water from a water-alcohol
solution thereby drying the alcohol . sounds too good to be
true.
In my previous attempt
at recovering methanol from the crude glycerine split from the glycerine
cocktail, a combination of greed and stupidity on my part resulted in methanol
w. water in it. ("Water in Recovered Methanol?" 4/28/06).
I've tweaked the
condenser. I've tied the cooling of methanol vapors (> much hot water)
to my wash tank. Will use the hot water generated by the cooling of methanol
to washing a batch of BD.
I will keep close eye on
temp. and be patient. Do not allow the temp to rise above 160F until
distillation stops at this temp.
Distillate produced in
150 - 160F range was mostly methanol. Temp increase seemed to slow
down at 150F. I take this to mean a phase change is occurring (added heat is
converting liquid Methanol to gaseous Methanol). Above 160F temp seemed to
rise more quickly. I take this to mean that much of the methanol is
gone.
My plan is to have 4
containers, each with 5 lbs (~ 2.24 Kg) of 3A molecular sieve. Allow 2 gallons
of distillate to flow into each container. Occasionally swirl the contents of
the containers over the next 24 hrs.
I'll strain out the 3A
molecular sieve and re-weigh. If it works, I should be able to dry the
methanol and from the changes in mass of the molecular sieve, get a sense of
the actual volume of methanol I can reasonably hope to recover from a given
volume of crude glycerine. I also hope to get a sense of the temp cut-off
point.
As I understand it, 3A
molecular Sieve will absorb about 25% of its weight in water. If, for
example the molecular sieve in container 1 (1st 2 gal distillate) increases by
5%, the next by 8%, the next by 15%, and the last by 25%, and additional Mol.
Sieve continues to gain mass, I would think that 6 or 7 gallons of methanol is
a reasonable
expectation for the volume of co-product I'm
distilling.
Suggestions ... including
"Stop, you have it all wrong!"
would be appreciated. It's tues. Friday looks
like a good day to brew; Saturday,
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
Jason & Katie,
I finally got around to reading the article. You're right,
vacuum is the best way to regenerate the beads. Maybe a combination of
vacuum and heat will work.
I have a concern. The 3A molecular sieve has openings 3 angstroms in
diameter. This allows water 2.8 angstroms to enter, but not ethanol 4.4
angstroms. I suspect that methanol is larger than water, but have not been
able to find its diameter. It would be a real shame if the methanol
molecules can also pass through the pores.
Tom
- Original Message -
From: "Jason& Katie" <[EMAIL PROTECTED]>
To:
Sent: Wednesday, May 24, 2006 5:37 PM
Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery
> that will work, absolutely, but i have a paper
> (http://www.ethanol.org/documents/Ethanol101.7.pdf) that describes passing
> hot alcohol vapors over 3A sieve under a slight pressure to achieve the
> same
> results. im not sure if it is any more or less efficient or simple, but it
> also works. and this paper also describes how and why the zeolite loses
> its
> viability after a time. if you bake it the heat breaks down the crystals.
> (better to use vacuum as well as heat =lower temps)
>
>
> - Original Message -
> From: "Keith Addison" <[EMAIL PROTECTED]>
> To:
> Sent: Tuesday, May 23, 2006 11:11 PM
> Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery
>
>
>> >i was researching alcohol production about a year ago, and many of
>>>the pages i visited (including JTF) suggested that wet alcohol
>>>vapors from a distillery's boiler could be passed over 3A sieve
>>>instead of normal column packing material (marbles, SS wool, ceramic
>>>rings, etc) to produce 99.5% 0r higher grade alcohol.
>>
>> That's not right. From the boiler it has to go through the
>> distillation column first, and after that the distillate goes through
>> 3A sieve.
>>
>> Best
>>
>> Keith
>>
>>>since methanol is similar in composition to ethanol, i would wager
>>>that applies to both scenarios. use an inverted soda bottle or some
>>>similarly shaped vessel full of 3A and inject the alcohol vapors
>>>into the wide end while collecting fresh dry methanol from
>>>the narrow end. you could set up multiple cannisters for this so
>>>you always have a ready sieve while others are being re- baked.
>>>
>>>- Original Message -
>>>From: <mailto:[EMAIL PROTECTED]>Thomas Kelly
>>>To: <mailto:Biofuel@sustainablelists.org>biofuel
>>>Sent: Tuesday, May 23, 2006 7:37 AM
>>>Subject: [Biofuel] 3A molecular Sieve and Methanol recovery
>>>
>>>Hello to all,
>>> 3A molecular sieve is on its way. As I understand it,
>>>selectively absorbs water from a water-alcohol solution thereby
>>>drying the alcohol . sounds too good to be true.
>>> In my previous attempt at recovering methanol from the crude
>>>glycerine split from the glycerine cocktail, a combination of greed
>>>and stupidity on my part resulted in methanol w. water in it.
>>>("Water in Recovered Methanol?" 4/28/06).
>>> I've tweaked the condenser. I've tied the cooling of methanol
>>>vapors (> much hot water) to my wash tank. Will use the hot
>>>water generated by the cooling of methanol to washing a batch of BD.
>>> I will keep close eye on temp. and be patient. Do not allow the
>>>temp to rise above 160F until distillation stops at this temp.
>>> Distillate produced in 150 - 160F range was mostly methanol.
>>>Temp increase seemed to slow down at 150F. I take this to mean a
>>>phase change is occurring (added heat is converting liquid Methanol
>>>to gaseous Methanol). Above 160F temp seemed to rise more quickly. I
>>>take this to mean that much of the methanol is gone.
>>> My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of
>>>3A molecular sieve. Allow 2 gallons of distillate to flow into each
>>>container. Occasionally swirl the contents of the containers over
>>>the next 24 hrs.
>>> I'll strain out the 3A molecular sieve and re-weigh. If it
>>>works, I should be able to dry the methanol and from the changes in
>>>mass of the molecular sieve, get a sense of the actual volume of
>>>methanol I can reasonably hope to recover from a given volume of
>>>crude glycerine. I also hope to get a sense of the temp cut-off
>>>point.
>>> As I understand it, 3A molecular Si
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
that will work, absolutely, but i have a paper
(http://www.ethanol.org/documents/Ethanol101.7.pdf) that describes passing
hot alcohol vapors over 3A sieve under a slight pressure to achieve the same
results. im not sure if it is any more or less efficient or simple, but it
also works. and this paper also describes how and why the zeolite loses its
viability after a time. if you bake it the heat breaks down the crystals.
(better to use vacuum as well as heat =lower temps)
- Original Message -
From: "Keith Addison" <[EMAIL PROTECTED]>
To:
Sent: Tuesday, May 23, 2006 11:11 PM
Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery
> >i was researching alcohol production about a year ago, and many of
>>the pages i visited (including JTF) suggested that wet alcohol
>>vapors from a distillery's boiler could be passed over 3A sieve
>>instead of normal column packing material (marbles, SS wool, ceramic
>>rings, etc) to produce 99.5% 0r higher grade alcohol.
>
> That's not right. From the boiler it has to go through the
> distillation column first, and after that the distillate goes through
> 3A sieve.
>
> Best
>
> Keith
>
>>since methanol is similar in composition to ethanol, i would wager
>>that applies to both scenarios. use an inverted soda bottle or some
>>similarly shaped vessel full of 3A and inject the alcohol vapors
>>into the wide end while collecting fresh dry methanol from
>>the narrow end. you could set up multiple cannisters for this so
>>you always have a ready sieve while others are being re- baked.
>>
>>- Original Message -
>>From: <mailto:[EMAIL PROTECTED]>Thomas Kelly
>>To: <mailto:Biofuel@sustainablelists.org>biofuel
>>Sent: Tuesday, May 23, 2006 7:37 AM
>>Subject: [Biofuel] 3A molecular Sieve and Methanol recovery
>>
>>Hello to all,
>> 3A molecular sieve is on its way. As I understand it,
>>selectively absorbs water from a water-alcohol solution thereby
>>drying the alcohol . sounds too good to be true.
>> In my previous attempt at recovering methanol from the crude
>>glycerine split from the glycerine cocktail, a combination of greed
>>and stupidity on my part resulted in methanol w. water in it.
>>("Water in Recovered Methanol?" 4/28/06).
>> I've tweaked the condenser. I've tied the cooling of methanol
>>vapors (> much hot water) to my wash tank. Will use the hot
>>water generated by the cooling of methanol to washing a batch of BD.
>> I will keep close eye on temp. and be patient. Do not allow the
>>temp to rise above 160F until distillation stops at this temp.
>> Distillate produced in 150 - 160F range was mostly methanol.
>>Temp increase seemed to slow down at 150F. I take this to mean a
>>phase change is occurring (added heat is converting liquid Methanol
>>to gaseous Methanol). Above 160F temp seemed to rise more quickly. I
>>take this to mean that much of the methanol is gone.
>> My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of
>>3A molecular sieve. Allow 2 gallons of distillate to flow into each
>>container. Occasionally swirl the contents of the containers over
>>the next 24 hrs.
>> I'll strain out the 3A molecular sieve and re-weigh. If it
>>works, I should be able to dry the methanol and from the changes in
>>mass of the molecular sieve, get a sense of the actual volume of
>>methanol I can reasonably hope to recover from a given volume of
>>crude glycerine. I also hope to get a sense of the temp cut-off
>>point.
>> As I understand it, 3A molecular Sieve will absorb about 25%
>>of its weight in water. If, for example the molecular sieve in
>>container 1 (1st 2 gal distillate) increases by 5%, the next by 8%,
>>the next by 15%, and the last by 25%, and additional Mol. Sieve
>>continues to gain mass, I would think that 6 or 7 gallons of
>>methanol is a reasonable
>>expectation for the volume of co-product I'm distilling.
>>Suggestions ... including "Stop, you have it all wrong!"
>>would be appreciated. It's tues. Friday looks like a good day to
>>brew; Saturday, to wash/distill. There's time for suggestions.
>>Tom
>
>
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> messages):
>
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
Hi Tom; Your post made it to the list. There is a switch for self delivery did you inadvetantly turn it off lately when changing settings for the list server? Anyways Ken says zeolite once in use will reliably only adsorb more like 10% of it's weight in water. Sorry I thought you were running a vacuum processor like me. Yes the line from the tank must be insulated. It is handy to insert a thermometer beneath this insulation to monitor vapour temperature while things proceed. A molecular sieve is normally fitted with a heated and insulated jacket which allows it to be regenerated in situ using the vacuum system to assist drying. Often these are used to prevent oil from a mechanical pump backstreaming under molecular flow conditions ( below 50 millitorr as a general rule but depends on geometries) into the rest of the vacuum system. In that case the sieve is fitted just upstream of the pump. In our case I would put it just above the condenser at a point where vapours can flow vertically downward through it. If I really wanted to be clever I could build a fractionating column and use the zeolite beads as the fractionating media and kill two birds with one stone. The process would involve recovering methanol and then as a final step the trap would be heated and the vacuum pump used to dry the zeolite. The water would then precipitate out and be collected in a separate container from the methanol. The actual amount of water removed would then be known. Process endpoint would be decided by an improvement in the vacuum at a fixed pumping rate. Best regards. Let us know what you learn. Joe Thomas Kelly wrote: > Joe, > I got your response, but my post never appeared in my mail nor did any > response w. numbers? from Ken. > Maybe they'll show up in my spam trap later. > > 25 lbs (11.2 Kg) of 3A molecular sieve arrived a little while ago. > > You wrote: > "You could put the seives in a trap upstream of your condenser. " > > Run the vapors through the sieve? Won't they cool and condense? I had > to insulate the short tube leading to the condenser because methanol was > condensing in the line before the condenser. > > Also: > "If the trap is fitted with heater you can then heat them in situ with > vacuum and dry them in place later ..." > > If you are talking about regenerating the zeolite, I'm thinking of a > solar oven ... suggested by Todd. I have plans, materials, etc. Seems > rather simple enough also, perhaps, too good to be true? > > Quite a bit of interesting stuff includes using vacuum pumps. I don't > know how to use one ... that is, apply it to anything. There's a vacuum > pump on sale at Harbor Freight for under $20 US. "Venturi-type vacuum pump > removes water from air conditioning systems. .. produces a vacuum of > 28.3" of mercury at sea level w. 90 psi. 1/4" NPT." $15.99 (Same w. > 1/2" connector $16.99). Do I need something better than a $20 pump to > generate vacuum to help dry my WVO or for what you are suggesting here? > Always good to hear from you. I hope Ken's numbers come through. I'd > like to see them. > Tom > > - Original Message - > From: "Joe Street" <[EMAIL PROTECTED]> > To: > Sent: Tuesday, May 23, 2006 4:01 PM > Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery > > > >>Great news Tom; >> >>I'm waiting to hear what the weight change happens in your seives >>material. Let it dry first as it will be wet with methanol on the >>outside but the adsorbed water will not evaporate easily so air drying >>should not result in apreciable water loss as long as you don't overdo >>it. Ken's numbers may seem depressing but are probably realistic. You >>could put the seives in a trap upstream of your condenser. If the trap >>is fitted with heater you can then heat them in situ with vacuum and dry >>them in place later when you get everything sorted out. However the >>recovered methanol may be less than 10% water (I hope) so it would be >>fine. I am holding my breath waiting to find out! >> >>Joe >> >>Thomas Kelly wrote: >> >> >>>Hello to all, >>> 3A molecular sieve is on its way. As I understand it, selectively >>>absorbs water from a water-alcohol solution thereby drying the alcohol >>>. sounds too good to be true. >>> In my previous attempt at recovering methanol from the crude >>>glycerine split from the glycerine cocktail, a combination of greed and >>>stupidity on my part resulted in
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
>i was researching alcohol production about a year ago, and many of
>the pages i visited (including JTF) suggested that wet alcohol
>vapors from a distillery's boiler could be passed over 3A sieve
>instead of normal column packing material (marbles, SS wool, ceramic
>rings, etc) to produce 99.5% 0r higher grade alcohol.
That's not right. From the boiler it has to go through the
distillation column first, and after that the distillate goes through
3A sieve.
Best
Keith
>since methanol is similar in composition to ethanol, i would wager
>that applies to both scenarios. use an inverted soda bottle or some
>similarly shaped vessel full of 3A and inject the alcohol vapors
>into the wide end while collecting fresh dry methanol from
>the narrow end. you could set up multiple cannisters for this so
>you always have a ready sieve while others are being re- baked.
>
>- Original Message -
>From: <mailto:[EMAIL PROTECTED]>Thomas Kelly
>To: <mailto:Biofuel@sustainablelists.org>biofuel
>Sent: Tuesday, May 23, 2006 7:37 AM
>Subject: [Biofuel] 3A molecular Sieve and Methanol recovery
>
>Hello to all,
> 3A molecular sieve is on its way. As I understand it,
>selectively absorbs water from a water-alcohol solution thereby
>drying the alcohol . sounds too good to be true.
> In my previous attempt at recovering methanol from the crude
>glycerine split from the glycerine cocktail, a combination of greed
>and stupidity on my part resulted in methanol w. water in it.
>("Water in Recovered Methanol?" 4/28/06).
> I've tweaked the condenser. I've tied the cooling of methanol
>vapors (> much hot water) to my wash tank. Will use the hot
>water generated by the cooling of methanol to washing a batch of BD.
> I will keep close eye on temp. and be patient. Do not allow the
>temp to rise above 160F until distillation stops at this temp.
> Distillate produced in 150 - 160F range was mostly methanol.
>Temp increase seemed to slow down at 150F. I take this to mean a
>phase change is occurring (added heat is converting liquid Methanol
>to gaseous Methanol). Above 160F temp seemed to rise more quickly. I
>take this to mean that much of the methanol is gone.
> My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of
>3A molecular sieve. Allow 2 gallons of distillate to flow into each
>container. Occasionally swirl the contents of the containers over
>the next 24 hrs.
> I'll strain out the 3A molecular sieve and re-weigh. If it
>works, I should be able to dry the methanol and from the changes in
>mass of the molecular sieve, get a sense of the actual volume of
>methanol I can reasonably hope to recover from a given volume of
>crude glycerine. I also hope to get a sense of the temp cut-off
>point.
> As I understand it, 3A molecular Sieve will absorb about 25%
>of its weight in water. If, for example the molecular sieve in
>container 1 (1st 2 gal distillate) increases by 5%, the next by 8%,
>the next by 15%, and the last by 25%, and additional Mol. Sieve
>continues to gain mass, I would think that 6 or 7 gallons of
>methanol is a reasonable
>expectation for the volume of co-product I'm distilling.
>Suggestions ... including "Stop, you have it all wrong!"
>would be appreciated. It's tues. Friday looks like a good day to
>brew; Saturday, to wash/distill. There's time for suggestions.
>Tom
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Re: [Biofuel] 3A molecular Sieve and Methanol recovery
On May 23, 2006, at 5:51 PM, Thomas Kelly wrote: When you say "it settles down into a more disappointingperformance." do you mean it doesn't regenerate fully?It may be that, or it may be that the zeolite becomespoisoned to some extent with something else that won'tleave the pores -- not sure.As far as regenerating the sieve, I am under the impressionthat 350F for a few hours (days?) would do it . wrong???It might -- I was using the "broil" setting of my electric oven,for maybe half an hour. I believe that's 400-450. Pulling somevacuum helps immensely, if you can do it... I am looking at plans for a solar oven that suposedlyheats to 350 - 400F.Solar would definitely be the energy-efficient way to go.Let us know your results :-)-K___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
Ken, You wrote: "25% would be very successful -- 10% might be more realistic. It works better the first few times, then settles downinto a more disappointing performance :-)" 10% might not be so bad. When you say "it settles down into a more diappointing performance." do you mean it doesn't regenerate fully? As far as regenerating the Sieve, I am under the impression that 350F for a few hours (days?) would do it . wrong??? I am looking at plans for a solar oven that suposedly heats to 350 - 400F. I distilled about 24 gal of glycerine/methanol on my first attempt at methanol recovery. It takes several weeks to generate and that much crude glycerine. That gives me several weeks to regenerate the sieve. Even w. cloudy weather, a self-respecting solar oven should do the trick. I suspect a reasonable yield of methanol will be about 6 gallons (23 L) from 24 gallons (91L) of glycerine that has been split from about 32 gal. (112L) of cocktail from 320+ gal (1215L)of WVO processed, requiring over 60 gal (228L) of methanol. The first 4 gal or so is relatively pure methanol (good enough to use to make BD). It's the next 2 (or even 3) gal that the molecular sieve will prove its worth. The 3A molecular sieve arrived today, so we'll see what we shall see. I'm thinking about passing the vapor through the sieve, but that will probably have to wait until next time. Thanks Ken, Tom - Original Message - From: Ken Provost To: biofuel@sustainablelists.org Sent: Tuesday, May 23, 2006 10:52 AM Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery On May 23, 2006, at 5:37 AM, Thomas Kelly wrote: My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of 3A molecular sieve. Allow 2 gallons of distillate to flow into each container. Occasionally swirl the contents of the containers over the next 24 hrs.. As I understand it, 3A molecular Sieve will absorb about 25% of its weight in water. What you're suggesting will work, but maybe not as well as you hope. 25% would be very successful -- 10% might be more realistic. It works better the first few times, then settles down into a more disappointing performance :-) Note that sieve works better when it extracts water from a VAPOR phase. I never did that because I found the equipment too complex, but it's much more efficient that way. You haven't mentioned your plans for regenerating the sieve after each use. That can be a very energy-intensive process. -K ___Biofuel mailing listBiofuel@sustainablelists.orghttp://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.orgBiofuel at Journey to Forever:http://journeytoforever.org/biofuel.htmlSearch the combined Biofuel and Biofuels-biz list archives (50,000 messages):http://www.mail-archive.com/biofuel@sustainablelists.org/ ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
Jason & Katie,
I got the idea for
using the molecular sieve from the JTF site re: ethanol production. Ken P.
mentioned it.
I think it will dry
alcohol, whether methyl or ethyl, but I suspect it will produce 99+% if you
start w. 90 or 95%.
I'm fairly confident that the first 4 gallons of
recovered methanol will be in this range. (The first time I recovered
methanol, the first 4.5 gal were used to make a batch of BD that washed and
dried OK, but failed the methanol quality test.) The next 2 gallons are what I'm
interested in , and the last 2 gal. are there just to see what
happens.
I've been concerned that
the vapor would condense in a trap (I was thinking 3 foot length of 2" PVC
filled w. sieve). That might happen initially(150's F vapor), when methanol
conc. is very high and water very low = sieve not needed anyway. As
more methanol condensed and moved through the sieve the trap would heat up. As
the temp of the vapor reached 160F and higher (when methanol is decreasing and
water is increasing), it might no longer condense on the hot sieve.In other words, the sieve would be in a condition to function
best at the time it was needed most.
- Original Message -
From:
Jason& Katie
To: biofuel@sustainablelists.org
Sent: Tuesday, May 23, 2006 6:37 PM
Subject: Re: [Biofuel] 3A molecular Sieve
and Methanol recovery
i was researching alcohol production about a year
ago, and many of the pages i visited (including JTF) suggested that wet
alcohol vapors from a distillery's boiler could be passed over 3A sieve
instead of normal column packing material (marbles, SS wool, ceramic rings,
etc) to produce 99.5% 0r higher grade alcohol. since methanol is similar in
composition to ethanol, i would wager that applies to both scenarios. use an
inverted soda bottle or some similarly shaped vessel full of 3A and
inject the alcohol vapors into the wide end while collecting fresh
dry methanol from the narrow end. you could set up multiple
cannisters for this so you always have a ready sieve while others are being
re- baked.
- Original Message -
From:
Thomas
Kelly
To: biofuel
Sent: Tuesday, May 23, 2006 7:37
AM
Subject: [Biofuel] 3A molecular Sieve
and Methanol recovery
Hello to all,
3A molecular sieve is
on its way. As I understand it, selectively absorbs water from a
water-alcohol solution thereby drying the alcohol . sounds too good to
be true.
In my previous attempt
at recovering methanol from the crude glycerine split from the glycerine
cocktail, a combination of greed and stupidity on my part resulted in
methanol w. water in it. ("Water in Recovered Methanol?"
4/28/06).
I've tweaked the
condenser. I've tied the cooling of methanol vapors (> much hot
water) to my wash tank. Will use the hot water generated by the cooling of
methanol to washing a batch of BD.
I will keep close eye
on temp. and be patient. Do not allow the temp to rise above 160F until
distillation stops at this temp.
Distillate produced in
150 - 160F range was mostly methanol. Temp increase seemed to slow
down at 150F. I take this to mean a phase change is occurring (added heat is
converting liquid Methanol to gaseous Methanol). Above 160F temp seemed to
rise more quickly. I take this to mean that much of the methanol is
gone.
My plan is to have 4
containers, each with 5 lbs (~ 2.24 Kg) of 3A molecular sieve. Allow 2
gallons of distillate to flow into each container. Occasionally swirl the
contents of the containers over the next 24 hrs.
I'll strain out the 3A
molecular sieve and re-weigh. If it works, I should be able to dry the
methanol and from the changes in mass of the molecular sieve, get a sense of
the actual volume of methanol I can reasonably hope to recover from a given
volume of crude glycerine. I also hope to get a sense of the temp cut-off
point.
As I understand it, 3A
molecular Sieve will absorb about 25% of its weight in water. If, for
example the molecular sieve in container 1 (1st 2 gal distillate) increases
by 5%, the next by 8%, the next by 15%, and the last by 25%, and additional
Mol. Sieve continues to gain mass, I would think that 6 or 7 gallons of
methanol is a reasonable
expectation for the volume of co-product I'm
distilling.
Suggestions ... including
"Stop, you have it all wrong!"
would be appreciated. It's tues. Friday looks
like a good day to brew; Saturday, to wash/distill. There's time for
suggestions.
Tom
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
i was researching alcohol production about a year
ago, and many of the pages i visited (including JTF) suggested that wet alcohol
vapors from a distillery's boiler could be passed over 3A sieve instead of
normal column packing material (marbles, SS wool, ceramic rings, etc) to produce
99.5% 0r higher grade alcohol. since methanol is similar in composition to
ethanol, i would wager that applies to both scenarios. use an inverted soda
bottle or some similarly shaped vessel full of 3A and inject the alcohol vapors
into the wide end while collecting fresh dry methanol from
the narrow end. you could set up multiple cannisters for this so you
always have a ready sieve while others are being re- baked.
- Original Message -
From:
Thomas
Kelly
To: biofuel
Sent: Tuesday, May 23, 2006 7:37 AM
Subject: [Biofuel] 3A molecular Sieve and
Methanol recovery
Hello to all,
3A molecular sieve is on
its way. As I understand it, selectively absorbs water from a water-alcohol
solution thereby drying the alcohol . sounds too good to be
true.
In my previous attempt
at recovering methanol from the crude glycerine split from the glycerine
cocktail, a combination of greed and stupidity on my part resulted in methanol
w. water in it. ("Water in Recovered Methanol?" 4/28/06).
I've tweaked the
condenser. I've tied the cooling of methanol vapors (> much hot water)
to my wash tank. Will use the hot water generated by the cooling of methanol
to washing a batch of BD.
I will keep close eye on
temp. and be patient. Do not allow the temp to rise above 160F until
distillation stops at this temp.
Distillate produced in
150 - 160F range was mostly methanol. Temp increase seemed to slow
down at 150F. I take this to mean a phase change is occurring (added heat is
converting liquid Methanol to gaseous Methanol). Above 160F temp seemed to
rise more quickly. I take this to mean that much of the methanol is
gone.
My plan is to have 4
containers, each with 5 lbs (~ 2.24 Kg) of 3A molecular sieve. Allow 2 gallons
of distillate to flow into each container. Occasionally swirl the contents of
the containers over the next 24 hrs.
I'll strain out the 3A
molecular sieve and re-weigh. If it works, I should be able to dry the
methanol and from the changes in mass of the molecular sieve, get a sense of
the actual volume of methanol I can reasonably hope to recover from a given
volume of crude glycerine. I also hope to get a sense of the temp cut-off
point.
As I understand it, 3A
molecular Sieve will absorb about 25% of its weight in water. If, for
example the molecular sieve in container 1 (1st 2 gal distillate) increases by
5%, the next by 8%, the next by 15%, and the last by 25%, and additional Mol.
Sieve continues to gain mass, I would think that 6 or 7 gallons of methanol is
a reasonable
expectation for the volume of co-product I'm
distilling.
Suggestions ... including
"Stop, you have it all wrong!"
would be appreciated. It's tues. Friday looks
like a good day to brew; Saturday, to wash/distill. There's time for
suggestions.
Tom
___Biofuel mailing
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Re: [Biofuel] 3A molecular Sieve and Methanol recovery
a solar concentrator should work well, if it has some form of tracking system - Original Message - From: Ken Provost To: biofuel@sustainablelists.org Sent: Tuesday, May 23, 2006 9:52 AM Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery On May 23, 2006, at 5:37 AM, Thomas Kelly wrote: My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of 3A molecular sieve. Allow 2 gallons of distillate to flow into each container. Occasionally swirl the contents of the containers over the next 24 hrs.. As I understand it, 3A molecular Sieve will absorb about 25% of its weight in water. What you're suggesting will work, but maybe not as well as you hope. 25% would be very successful -- 10% might be more realistic. It works better the first few times, then settles down into a more disappointing performance :-) Note that sieve works better when it extracts water from a VAPOR phase. I never did that because I found the equipment too complex, but it's much more efficient that way. You haven't mentioned your plans for regenerating the sieve after each use. That can be a very energy-intensive process. -K ___Biofuel mailing listBiofuel@sustainablelists.orghttp://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.orgBiofuel at Journey to Forever:http://journeytoforever.org/biofuel.htmlSearch the combined Biofuel and Biofuels-biz list archives (50,000 messages):http://www.mail-archive.com/biofuel@sustainablelists.org/ No virus found in this incoming message.Checked by AVG Free Edition.Version: 7.1.392 / Virus Database: 268.7.0/345 - Release Date: 5/22/2006 ___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
Joe,
I got your response, but my post never appeared in my mail nor did any
response w. numbers? from Ken.
Maybe they'll show up in my spam trap later.
25 lbs (11.2 Kg) of 3A molecular sieve arrived a little while ago.
You wrote:
"You could put the seives in a trap upstream of your condenser. "
Run the vapors through the sieve? Won't they cool and condense? I had
to insulate the short tube leading to the condenser because methanol was
condensing in the line before the condenser.
Also:
"If the trap is fitted with heater you can then heat them in situ with
vacuum and dry them in place later ..."
If you are talking about regenerating the zeolite, I'm thinking of a
solar oven ... suggested by Todd. I have plans, materials, etc. Seems
rather simple enough also, perhaps, too good to be true?
Quite a bit of interesting stuff includes using vacuum pumps. I don't
know how to use one ... that is, apply it to anything. There's a vacuum
pump on sale at Harbor Freight for under $20 US. "Venturi-type vacuum pump
removes water from air conditioning systems. .. produces a vacuum of
28.3" of mercury at sea level w. 90 psi. 1/4" NPT." $15.99 (Same w.
1/2" connector $16.99). Do I need something better than a $20 pump to
generate vacuum to help dry my WVO or for what you are suggesting here?
Always good to hear from you. I hope Ken's numbers come through. I'd
like to see them.
Tom
- Original Message -
From: "Joe Street" <[EMAIL PROTECTED]>
To:
Sent: Tuesday, May 23, 2006 4:01 PM
Subject: Re: [Biofuel] 3A molecular Sieve and Methanol recovery
> Great news Tom;
>
> I'm waiting to hear what the weight change happens in your seives
> material. Let it dry first as it will be wet with methanol on the
> outside but the adsorbed water will not evaporate easily so air drying
> should not result in apreciable water loss as long as you don't overdo
> it. Ken's numbers may seem depressing but are probably realistic. You
> could put the seives in a trap upstream of your condenser. If the trap
> is fitted with heater you can then heat them in situ with vacuum and dry
> them in place later when you get everything sorted out. However the
> recovered methanol may be less than 10% water (I hope) so it would be
> fine. I am holding my breath waiting to find out!
>
> Joe
>
> Thomas Kelly wrote:
>
>> Hello to all,
>> 3A molecular sieve is on its way. As I understand it, selectively
>> absorbs water from a water-alcohol solution thereby drying the alcohol
>> . sounds too good to be true.
>> In my previous attempt at recovering methanol from the crude
>> glycerine split from the glycerine cocktail, a combination of greed and
>> stupidity on my part resulted in methanol w. water in it. ("Water in
>> Recovered Methanol?" 4/28/06).
>> I've tweaked the condenser. I've tied the cooling of methanol
>> vapors (> much hot water) to my wash tank. Will use the hot water
>> generated by the cooling of methanol to washing a batch of BD.
>> I will keep close eye on temp. and be patient. Do not allow the
>> temp to rise above 160F until distillation stops at this temp.
>> Distillate produced in 150 - 160F range was mostly methanol. Temp
>> increase seemed to slow down at 150F. I take this to mean a phase change
>> is occurring (added heat is converting liquid Methanol to gaseous
>> Methanol). Above 160F temp seemed to rise more quickly. I take this to
>> mean that much of the methanol is gone.
>> My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of 3A
>> molecular sieve. Allow 2 gallons of distillate to flow into each
>> container. Occasionally swirl the contents of the containers over the
>> next 24 hrs.
>> I'll strain out the 3A molecular sieve and re-weigh. If it works, I
>> should be able to dry the methanol and from the changes in mass of the
>> molecular sieve, get a sense of the actual volume of methanol I can
>> reasonably hope to recover from a given volume of crude glycerine. I
>> also hope to get a sense of the temp cut-off point.
>> As I understand it, 3A molecular Sieve will absorb about 25% of its
>> weight in water. If, for example the molecular sieve in container 1 (1st
>> 2 gal distillate) increases by 5%, the next by 8%, the next by 15%, and
>> the last by 25%, and additional Mol. Sieve continues to gain mass, I
>> would think that 6 or 7 gallons of methanol is a reasonable
>> expectation for the volume of co-product I'm distilling.
>>
Re: [Biofuel] 3A molecular Sieve and Methanol recovery
Great news Tom;
I'm waiting to hear what the weight change happens in your seives
material. Let it dry first as it will be wet with methanol on the
outside but the adsorbed water will not evaporate easily so air drying
should not result in apreciable water loss as long as you don't overdo
it. Ken's numbers may seem depressing but are probably realistic. You
could put the seives in a trap upstream of your condenser. If the trap
is fitted with heater you can then heat them in situ with vacuum and dry
them in place later when you get everything sorted out. However the
recovered methanol may be less than 10% water (I hope) so it would be
fine. I am holding my breath waiting to find out!
Joe
Thomas Kelly wrote:
> Hello to all,
> 3A molecular sieve is on its way. As I understand it, selectively
> absorbs water from a water-alcohol solution thereby drying the alcohol
> . sounds too good to be true.
> In my previous attempt at recovering methanol from the crude
> glycerine split from the glycerine cocktail, a combination of greed and
> stupidity on my part resulted in methanol w. water in it. ("Water in
> Recovered Methanol?" 4/28/06).
> I've tweaked the condenser. I've tied the cooling of methanol
> vapors (> much hot water) to my wash tank. Will use the hot water
> generated by the cooling of methanol to washing a batch of BD.
> I will keep close eye on temp. and be patient. Do not allow the
> temp to rise above 160F until distillation stops at this temp.
> Distillate produced in 150 - 160F range was mostly methanol. Temp
> increase seemed to slow down at 150F. I take this to mean a phase change
> is occurring (added heat is converting liquid Methanol to gaseous
> Methanol). Above 160F temp seemed to rise more quickly. I take this to
> mean that much of the methanol is gone.
> My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of 3A
> molecular sieve. Allow 2 gallons of distillate to flow into each
> container. Occasionally swirl the contents of the containers over the
> next 24 hrs.
> I'll strain out the 3A molecular sieve and re-weigh. If it works, I
> should be able to dry the methanol and from the changes in mass of the
> molecular sieve, get a sense of the actual volume of methanol I can
> reasonably hope to recover from a given volume of crude glycerine. I
> also hope to get a sense of the temp cut-off point.
> As I understand it, 3A molecular Sieve will absorb about 25% of its
> weight in water. If, for example the molecular sieve in container 1 (1st
> 2 gal distillate) increases by 5%, the next by 8%, the next by 15%, and
> the last by 25%, and additional Mol. Sieve continues to gain mass, I
> would think that 6 or 7 gallons of methanol is a reasonable
> expectation for the volume of co-product I'm distilling.
> Suggestions ... including "Stop, you have it all wrong!"
> would be appreciated. It's tues. Friday looks like a good day to brew;
> Saturday, to wash/distill. There's time for suggestions.
> Tom
>
>
>
>
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Re: [Biofuel] 3A molecular Sieve and Methanol recovery
On May 23, 2006, at 5:37 AM, Thomas Kelly wrote: My plan is to have 4 containers, each with 5 lbs (~ 2.24 Kg) of 3A molecular sieve. Allow 2 gallons of distillate to flow into eachcontainer. Occasionally swirl the contents of the containers overthe next 24 hrs.. As I understand it, 3A molecular Sieve will absorb about 25% of its weight in water. What you're suggesting will work, but maybe not as well asyou hope. 25% would be very successful -- 10% might be morerealistic. It works better the first few times, then settles downinto a more disappointing performance :-)Note that sieve works better when it extracts water from aVAPOR phase. I never did that because I found the equipmenttoo complex, but it's much more efficient that way. You haven't mentioned your plans for regenerating the sieveafter each use. That can be a very energy-intensive process.-K___ Biofuel mailing list Biofuel@sustainablelists.org http://sustainablelists.org/mailman/listinfo/biofuel_sustainablelists.org Biofuel at Journey to Forever: http://journeytoforever.org/biofuel.html Search the combined Biofuel and Biofuels-biz list archives (50,000 messages): http://www.mail-archive.com/biofuel@sustainablelists.org/
[Biofuel] 3A molecular Sieve and Methanol recovery
Hello to all,
3A molecular sieve is on
its way. As I understand it, selectively absorbs water from a water-alcohol
solution thereby drying the alcohol . sounds too good to be
true.
In my previous attempt at
recovering methanol from the crude glycerine split from the glycerine cocktail,
a combination of greed and stupidity on my part resulted in methanol w. water in
it. ("Water in Recovered Methanol?" 4/28/06).
I've tweaked the
condenser. I've tied the cooling of methanol vapors (> much hot water) to
my wash tank. Will use the hot water generated by the cooling of methanol to
washing a batch of BD.
I will keep close eye on
temp. and be patient. Do not allow the temp to rise above 160F until
distillation stops at this temp.
Distillate produced in 150
- 160F range was mostly methanol. Temp increase seemed to slow down at
150F. I take this to mean a phase change is occurring (added heat is converting
liquid Methanol to gaseous Methanol). Above 160F temp seemed to rise more
quickly. I take this to mean that much of the methanol is gone.
My plan is to have 4
containers, each with 5 lbs (~ 2.24 Kg) of 3A molecular sieve. Allow 2 gallons
of distillate to flow into each container. Occasionally swirl the contents of
the containers over the next 24 hrs.
I'll strain out the 3A
molecular sieve and re-weigh. If it works, I should be able to dry the methanol
and from the changes in mass of the molecular sieve, get a sense of the actual
volume of methanol I can reasonably hope to recover from a given volume of crude
glycerine. I also hope to get a sense of the temp cut-off point.
As I understand it, 3A
molecular Sieve will absorb about 25% of its weight in water. If, for
example the molecular sieve in container 1 (1st 2 gal distillate) increases by
5%, the next by 8%, the next by 15%, and the last by 25%, and additional Mol.
Sieve continues to gain mass, I would think that 6 or 7 gallons of methanol is a
reasonable
expectation for the volume of co-product I'm
distilling.
Suggestions ... including "Stop,
you have it all wrong!"
would be appreciated. It's tues. Friday looks like
a good day to brew; Saturday, to wash/distill. There's time for
suggestions.
Tom
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