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: <biofuel@sustainablelists.org>
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 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 <mailto:[EMAIL PROTECTED]>
> *To:* biofuel <mailto:Biofuel@sustainablelists.org>
> *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, to wash/distill. There's time for suggestions.
> Tom
>
>
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