Rainwater
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DIY zeolite
I have been reading this paper "Zeolite synthesis from low-cost materials and environmental applicationscurrently free"
And am getting ready to attempt the hydrothermal synthesis outlined within this
paper. Well, outlined in papers, that are in papers. That this paper references,
My first target will be the P type Na6(AlO2)6(SiO2)6 •5H2O GIS (gismondine).
I picked this because of the reported 0.3nm size. My line of thinking is i can use a
simple hydrometer and some Ethanol to test and fine tune the selectivity.
The reactor will be one of these ptfe lined autoclave reactors courtesy of santa
Now the paper appears to simply be a review and summary of about 40+ other papers. https://doi.org/10.1016/j.fuel.2014.08.016
Anyone got any pointers, or experience with this type of appratus.
Heating of the sealed reactor will be done in a banger cage, inside my kiln, away from people, places, and things that are not explosion friendly.
And opening the reactor will be done with just as much paranoiya as cooking it.
Im really looking for suggestion on testing composition and products.
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Sulaiman
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Regarding the synthesis I know
nothing.
I have a little experience with 3a zeolites and a water:ethanol mixture:
The density test will be useful, but not enough,
you will also want to know how much water can be absorbed by the zeolite because if you need a lot of zeolite to absorb a little water
then your product losses by adhesion to the zeolite will be high.
(I believe that the losses can be recovered by distillation)
Try 100% ethanol with some zeolite and measure how much is lost by adsorbtion and absorbtion
CAUTION : Hobby Chemist, not Professional or even Amateur
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Rainwater
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I would like to write out the procedure to follow to test the products.
This helps me think amd figure out what I want to focus on.
So per exposure to a mixture. I would like to know
- How much mass is gained total (C - A)
- How much mass is coating the outside of the product (C - D)
- How much mass is absorbed into the product. (D - A)
- composition of absorbed mass
After synthesis, final workup, then activation of the sample.
Exposure procedure
- activation weight
- expose to solvent for fixed duration
- wet weight
- dry in dessicator until weight no longer changes
Number 4 is where the hydrometer comes into play.
Suppose a sample can absorb 10 grams, and I use 100 ml of 40% alcohol.
Crap, thats going to be a big sample.
Even if I find a container to minimize the amount of liquid required to use my
hydrometer. Its still going to be a lot,
Thats not practical at all for the scale of synthesis i will be doing.
Professional sieves only absorb 20~30% of their weight.
I can use density and a composition chart,
My most accurate scale is only +/- 1mg.
And possibly a boiling point chart.
My ability to measure temperature is within 1mK
All that said, its still not good enough for amateur work.
So scratch the hydrometer. I have some dry methanol.
Its about 0.38nm so with a perfect 3A zeolite, it will absorbe no methanol,
but 25% its wight in water
Ok i think i got the last steps figured out, at least enough to make a spreadsheet
So now just need to figure out a recipe and break out the old empirical methodology
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Sulaiman
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for quick determination of ethanol:water ratio you could use a refractometer,
but the correlation is non-linear.
I think I read somewhere (?) that the addition of crystal violet makes the relationship close to linear.
I will leave the research for you 
measuring the density of a solid object using Archimedes principle could be used for small samples of your mixture using a small solid mass of known
mass and density.to determine the liquid densiity?
CAUTION : Hobby Chemist, not Professional or even Amateur
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Rainwater
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Reagent A (Na2O)x(SiO3)y
(+/- 0.001g)
1000.002g of powdered rock. Mostly quartz.
1828.031g of NaOH*H2O
The mixture was covered, then heated in a stainless steel pot @ 345c for 48 hours.
Upon cooling 4L of di water was added and the mixture brought to 100c, then allowed to cool and decanted.
This leaching process was repeated twice until all the reaction mixture was collected.
Results were as thick as honey, clear as mud solution which solidified upon cooling. Product was dissolved and diluted again to ~15L.
Containers were left undisturbed for 14 days, resulting in brownish red, very clear solution sitting atop sludge.
It took that long to settle.
Solution was decanted and boiled to dryness 150c ( half now. Half next week)
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teodor
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I have an interst in zeolite synthesys too. How do you propose to test the result? For organic syntheses we have a melting point method. Do you know
methods to test the zeolite microstructure?
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Rainwater
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Im just going to use the fafo method and see if I can make some dust that can be compared to 3a
sieves. So far the first step is going great. Im up to almost ten ways not to clean up waterglass. The
best method so far(slowest) is to just leave it alone and let everything settle.
I would really like a yield so i can accurately calculate the consentration of the reagent a. Im sure i have
At least 50g of undisolved sludge, some of it is ferrous
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Rainwater
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Sodium silicate day 17
video link
Its saturated. Trying to to clean this up is a nightmare
[Edited on 19-1-2025 by Rainwater]
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Rainwater
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I went from mud to apple juice. The last 2 recrystallizations have done very little, so im
calling it as good as it's gonna get. I have about 2 gallons of saturated solution.
I want to titrate a sample to determine the sodium and silicon ratio, as well as
consentration. I was thinking about weighing 10mL(get the density), adding
methylene blue ph indicator, then adding diluted sulfuric acid until it goes from blue
to yellow(sodium consentration). Then filter dry and weigh the percipitate(Si conse tration)
Na2SiO3+H2SO4→Na2SO4+SiO2+H2O
I found this paper, explanes it all.
Attachment: is.14212.1995.pdf (1.6MB)
This file has been downloaded 62 times
[Edited on 21-1-2025 by Rainwater]
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Rainwater
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McDonald's sweet tea or liquid sand?
After over a dozen recrystallizations this is as clean as it gets.
My guess is the boiling pot contributed to the color.
Heres the data I have so far.
| Code: | volumetric flask
dry weight(g) h2o full(g) volume(mL)
25.001 51.287 26.286
HCl titration
hcl weight density(g/ml @ 20c)
30.394 1.15628091
Na2CO3 Start(g) end(g) mols used hcl concentration %/mass
29.936 16.361 0.1280805374 30.73%
Na2SiO3 test
weight(g) density(g/ml) HCl to neturalize(mols) Na by mass
33.253 1.265046032 0.19204074. 13.28%
weight boat dry(g) filtrate weigh(g) mol Si by mass
6.813 3.043 0.05064913449 9.15%
Na to Si Ratio:
3.79:1 by Stoichiometry
1.45:1 by weight
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And at 20c a consentration of 22.4%
[Edited on 24-1-2025 by Rainwater]
I have been doing a lot of back and forth but I think I have finally settled on an
experiment
DOI: 10.1016/j.matpr.2020.06.326
Comparative Study of Hydrothermal Synthesis Routes of Zeolite A
Low cost, low heat(60~100c), and atmospheric pressure.
This paper describes a simple process i think i will try to reproduce. All the
equipment and reagents are easily obtained. I wish they would have included more
information about their materials. For instant where it says "added NaOH.", is this
anhydrous, or the monohydrate. Taking the weights and measures literally would
mean all their reagents where dry before being added to water
I need more hours in a weekend
Attachment: 1-s2.0-S2214785320347994-main.pdf (1.2MB)
This file has been downloaded 42 times
Attachment: Na2sio3 study.xlsx (9kB)
This file has been downloaded 38 times
[Edited on 25-1-2025 by Rainwater]
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