solvent drying (zeolites and zeolite synthises)

Ephoton · Fri Aug 05, 2005 6:19 pm

many times I have used metals or salts to dry organic solvents.
but the other day I cryed enough of this often waistfull and tedios
necessity.

Zeolites I thought we need OTC home synthed zeolites.

after looking for a while I found that we needed 0.3 and 0.4 nano meter
cavity to absorbe water from most organic solvents.

so I started to search for there synthesis.
I was only able to realy find one place on the interenet that had more
than a zsm-5 synth

www.iza-synthesis.org

I know zk-5 has a cavity of 0.4 nm but it needs stronium so thats
no go. (otc stronium anyone)

my next goal is to find an easy to make zeolite of the right size.

any past experiance or advice would be great.

bio · Working Bee

This would be interesting to know for sure, however zeolite or silica gel dessicant grade (even RA) is quite inexpensive and if properly cleaned can be regenerated indefinetly.

With repeated use there is gradual breakdown of the particle size but a kilo of the 3-5mm silica beads RA grade has lasted me now for 3years and the jar is still 3/4 full.
IIRC was $80 but the cheap stuff (say $20) works OK if cleaned with HCl and is a fraction of that price. Doubt that you could make it for that!

Maybe try a patent search for the zeolite synth. Can't find it right now but I have a copy of a patent that has many examples of different zeolite preps. Thing is the ingredients needed, all put together, would probably cost more than the 3A sieves.

Ephoton · Mon Aug 08, 2005 6:06 pm

whats stopping us making some of the gels
is it getting the purity needed or experimental conditions.

posted from iza
MFI
[Fe]-ZSM-5
Si(96), Fe(4)

Contributed by Angelika Brückner

Verified by Y. Kiyozumi and by P. Fejes

Type Material Na0.3(TPA)3.7[Fe4Si92O192] wH2O (TPA = tetra-n-propylammonium)

Method A. Brückner, R. Lück, W. Wieker, B. Fahlke [1]

Batch Composition 30 Na2O : Fe2O3 : 30 SiO2 : 1040 H2O : 5 (TPA)Br : 25 H2SO4

Source Materials

distilled water
sulfuric acid (reagent grade, 98% H2SO4)
iron(III) sulfate (reagent grade, Fe2(S04)3. 9 H2O)
sodium metasiicate (reagent grade, Na2SiO3. 9 H2O) a
tetrapropylammonium bromide (TPABr) (Fluka, CH-9470 Buchs)

Batch Preparation (for ~20 g volatile-free product)

(1) [100 g water + 22 g sulfuric acid + 5.62 g iron(III) sulfate], stir until dissolved
(2) [163.4 g water + 85.26 g sodium metasiicate], stir until dissolved
(3) [(1) + (2)], add silicate slowly to iron(III) sulfate solution with good mixing
(4) [(3) + 13.31 g TPABr], mix vigorously until uniform (~ 400 rpm)

Crystallization

Vessel: stainless steel autoclaves
Temperature: 1700C
Time: 72 hours
Agitation: autoclaves are rotated axially

Product Recovery

(1) After cooling, filter and wash with water several times
(2) Dry over P4010
(3) Calcine at 5500C for 4 hours to remove template

Product Characterization

XRD: ZSM-5 (only phase)
Elemental Analysis: 0.07 Na2O : Fe2O3 : 48 SiO2 : wH2O
Crystal Size and Habit: 1-6 um, snowball-like
Click here to view XRD pattern

Reference

[1] A. Brückner, R. Lück, W. Wieker, B. Fahlke, Zeolites 12 (1992) 380

Note

a. Al(III), a common impurity in silica sources, displaces Fe(III) from T-atom positions in MFI. [1]

these reagent dont seem impossible
i havent looked into the metasilcate yet maby this is what you mean.

bio · Working Bee

.........whats stopping us making some of the gels
is it getting the purity needed or experimental conditions.................

Ahem...Well let's see now this rotating autoclave should be readily available in 6months for $20K.

.............Crystallization
Vessel: stainless steel autoclaves
Temperature: 1700C
Time: 72 hours
Agitation: autoclaves are rotated axially .......................

And this drying step could be a little hotter maybe but the oxy-acetylene torch make it anyway. Ah WTF just put it in the micro.

.........Product Recovery
(1) After cooling, filter and wash with water several times
(2) Dry over P4010
(3) Calcine at 5500C for 4 hours to remove template....................

Otherwise a piece of cake. There are really simple easy ways to do this.

Maybe calcined Kitty Litter??