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Metacelsus
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You mean brown solutions of pure compounds? In organic chemistry, brown solutions are commonplace, but generally a sign of impurities.
It's probably because brown is composed of many other colors, so it requires lots of different absorption frequencies.
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xfusion44
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Quote: Originally posted by greenlight  | On looking at the patent a second time it does appear to be a bit more complicated than the backyard lab unless you have a heating source to heat a
vessel to 250 Degrees Celcius and a vessel or stainless steel "bomb" capable of handling 1000 psi pressure as it says here:
"The acetonitrile, water and zinc acetate are mixed in ice a closed vessel and heated to a temperature of 250 C., preferably 240 C. As the heating
proceeds, the pressure rises. During the initial stages of the reaction, the pressure may reach as high as 1,000 p.s.i.g., preferably about 700
p.s.i.g. Thereafter, as the reaction proceeds, the pressure falls due to the formation of acetamide which has a lower vapor pressure than acetonitrile
and hence as acetamide is formed, the pressure drops. The pressure at the conclusion of the reaction is usually from 40 to 50 p.s.i.g. "
I think the best way to go would be to obtain some Ethyl acetate and use the method posted in the thread link by Polesch which uses 9% Ammonia as it
looks like less of a headache. The Ethyl acetate can be synthesized and the 9% Ammonia should be easy to get.
I have read that ethyl acetate is the primary solvent in non-acetone nail-polish remover but a distillation would be necessary.
Otherwise, here is a two links to a method of making Ethyl acetate from concentrated Sulphuric acid, ethanol and glacial Acetic acid:
https://www.erowid.org/archive/rhodium/chemistry/ethyl.aceta...
https://sites.google.com/site/mutludemirel/organic-chemistry...
There is also a video on youtube here:
http://www.youtube.com/watch?v=cFxZ0NircIk
Hope that helps.
[Edited on 22-11-2014 by greenlight] |
Thanks, sure it helps 
I have no "bomb", that would hold 1000psi/70bar  But maybe I could try the way
you've mentioned, I have very small amounts of conc. H2SO4 (only few milliliters), so making it wouldn't be an option, but I could try finding
non-acetone nail polish remover, but how do I know that it has only ethyl acetate and not acetone or other solvents? Do you think it should be written
on the bottle - I have small bottle of nail polish remover, but it says it does contain acetone, ethanol and a load of other solvents (this seems to
be a problem)
Here is a picture of the bottle:
PS: even if I find NPR with ethyl acetate - there may be other additional solvents with lower BP than ethyl acetate, so there could be distillation
problems, or not?
Thanks 
[Edited on 22-11-2014 by xfusion44]
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greenlight
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You need the Acetone free nail polish remover,it should say it on the bottle. It should have the ingredients written on the bottle, or look up the
product name's Material Safety Data Sheet.
I believe the Acetone free brands should have Ethyl acetate, Ethanol and fragrance in them. Here is an old thread about extracting Ethyl acetate from
non Acetone nail polish remover by distillation:
http://www.sciencemadness.org/talk/viewthread.php?tid=17401
Ethyl acetate (77.1.C) is very close boiling point wise to Ethanol (78.37 .C) which makes this difficult. You could use a fractioning (vigreux)
column if you have one otherwise just go for it and see what you get.
If this fails, hunt down some Sulphuric acid, hardware store drain cleaners, battery top-up solution (read labels), and boil this down to
concentration and try the actual synthesis
[Edited on 23-11-2014 by greenlight]
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xfusion44
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Thanks very much
Unfortunately I don't have fractionating column :-/
I will try to get non-acetone polish remover ASAP and will distill it and see what happens. Hopefully I'll be able to maintain the temperature under
78°C, althouhg some of ethanol may come with EtOAc too, I think it's worth a try. Do you think that ethanol would be a problem in this reaction? I
looked up on internet and found out that ethylamine could form when ammonia is mixed with ethanol, but only at high temperatures (200°C) and with
catalyst, so maybe it won't be a problem?
Also, do you think, that it would work fine if I'd use pure NH3 instead of solution? I could make it with NH4Cl + NaOH + H2O, although I don't know if
that is effective way, to produce enough ammonia gas?
Thanks again
[Edited on 23-11-2014 by xfusion44]
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greenlight
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It could lower the final yield of the Acetamide but I don't think it would cause too much of a problem. I would just take the distillation slow as I
could and not let the temp go above 78.C.
On the Acetamide synthesis thread from this site I linked before, Polesch uses 9% Ammonia but says two posts down that he uses a saturated solution of
ammonia in ice cold water and gets much better yields.
I would either use Ammonia solution from the shop or dissolve the ammonia gas into water until saturated and use that instead of just pumping the gas
straight in on its own.
The better you run the distillation the more pure your distillate should be. I would definitely suggest buying a fractioning column if you can't get
it right though.
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xfusion44
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I would need a quick answer - can butyl acetate be used instead of ethyl acetate? Im in supermarket...
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greenlight
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I don't think you can substitute it, you need the Ethyl acetate.
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xfusion44
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Anyway, I bought the one with butyl acetate, they didn't have anything other and drugstore was closed, hopefully butyl a. can be used, otherwise I'm
going tomorrow again to see, if the drugstore has it...
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xfusion44
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Ok, then I will go tomorrow again. I'll read your previous answer as soon as I get home.
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greenlight
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Yeah you can give it a go. What did you buy the Butyl acetate as, was it nail polish remover?
I think you will need the Ethyl acetate non acetone nail polish remover though.
[Edited on 23-11-2014 by greenlight]
[Edited on 23-11-2014 by greenlight]
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arkoma
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Here in the states "MEK substitute" at home depot=ethyl acetate. Five bucks a quart.
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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xfusion44
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@greenlight
Damn :-/ I probably bought useless nail polish remover... At first I saw that it said on the bottle butyl acetate and thought "that's it!" Then I
noticed, when I checked again that I was thinking wrong, because I thought it was ethyl acetate... Then I bought it and you said I could give it a
try, and now, when I'm at home I noticed that on the end of text it says acetone too  Maybe I can still get only butyl acetate from it by careful distillation, but even then, the question remains: will it work with butyl a.?...
Thanks for previous question, I'll see, what I can do...
When you say non acetone NPR, do you mean that acetone would react with ammonia to form other byproduct?
It's funny that all of the time, when we were mentioning not to go above 78°C, I thought that's for preventing ethanol from distilling, but I
remembered that it's the acetone that has 78°C boiling point - so if I'd have non acetone NPR I wouldn't need to worry about going above 78°C, I
think? Were we both confused?
Thanks
[Edited on 23-11-2014 by xfusion44]
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xfusion44
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I found (it doesn't even say how much), but I think it's 1 liter ethyl acetate for 8EUR - about 10USD on one of our online shops, I think that isn't
cheap for 1l EA, but if I don't find anything other, I may order it from there...
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greenlight
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I said to distill non-Acetone nail polish remover because they substitute the acetone with Ethyl acetate, the product you need to make Acetamide. It
may be harder to find the acetone free polish than the normal acetone brand.
I did mean not to go over 78.C because the non Acetone nail polish remover also has Ethanol in it which has a boiling point close to Ethyl acetate and
you want to try and distill Ethyl actetate only.
Acetone has a boiling point of 56.C. Sorry if i caused confusion.
I will see if I can find any literature about whether Butyl acetate can be substituted.
If you can't find it as the MEK substitute, Ethyl acetate is on ebay as "insect collecting fluid" and also from standard chem suppliers on there.
[Edited on 23-11-2014 by greenlight]
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xfusion44
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| Quote: Originally posted by greenlight | I said to distill non-Acetone nail polish remover because they substitute the acetone with Ethyl acetate, the product you need to make Acetamide. It
may be harder to find the acetone free polish than the normal acetone brand.
I did mean not to go over 78.C because the non Acetone nail polish remover also has Ethanol in it which has a boiling point close to Ethyl acetate and
you want to try and distill Ethyl actetate only.
Acetone has a boiling point of 56.C. Sorry if i caused confusion.
I will see if I can find any literature about whether Butyl acetate can be substituted.
If you can't find it as the MEK substitute, Ethyl acetate is on ebay as "insect collecting fluid" and also from standard chem suppliers on there.
[Edited on 23-11-2014 by greenlight] |
Yeah, only I was confused, not we I figured that out later...
However, distillation is done!
My nail polish remover contains: butyl acetate, ethanol, acetone, butyl stearate and ricinus communis oil (castor oil).
Here are all ingredients, sorted by boiling point:
Acetone: 56°C
Ethanol: 78°C
Butyl acetate: 126°C
Butyl stearate: 220°C
Castor oil: 313°C
First, I used water boiling bath to distill all of the acetone and ethanol. Then I cleaned condenser and put all of the acetone/ethanol mixture in the
bottle and cleaned the beaker. I repeated the process, but without water bath - just directly on hotplate. I left it distilling for up to 196°C and
it still boiled a little, but the boiling drastically slowed down at about 150 or 160°C. That way I've collected butyl acetate (I could tell by smell
that it wasn't acetone or ethanol). At the end, I was left with castor oil and butyl stearate, which is just a fragrance, so it's probably mainly just
castor oil, that was left and maybe a bit of butyl acetate.
On the picture below, there are products of distillation.
In the first bottle, there is acetone/ethanol mixture (about 40ml).
In the beaker, I don't know what it really is (10ml), but it was collected between 100°C and 124°C - probably there was still ethanol left, or
something, is it water? But I don't know why it didn't evaporate before at 100°C? (I started collecting butyl acetate at 124°C although BP is
126°C).
In the second bottle there's a final product, butyl acetate (about 35ml).
And in the erlenmeyer flask, there's the castor oil, butyl stearate and a little amount of butyl acetate (15ml). I used 100ml of nail polish remover.
The next thing to do is getting some ammonium hydroxide or making it and then hopefully after mixing it with butyl acetate, the reaction will take
place and make some acetamide But that's unfortunately maybe not gonna happen
:-/
Thanks for helping
[Edited on 23-11-2014 by xfusion44]
PS: castor oil has a nice smell of peanut or walnut
[Edited on 23-11-2014 by xfusion44]
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greenlight
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Well done.
I have been looking around and I'm pretty sure the Butyl acetate is a no-go in the production of Acetamide.
At least you have some experience distilling nail polish remover now for when you find an Acetone-free brand which contains Ethyl acetate.
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xfusion44
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Thanks for support
I agree that it probably won't work, so today I'll go to see if I can find ethyl acetate nail polish remover anywhere.
Thanks again, when I find something I'll be back
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xfusion44
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| Quote: Originally posted by greenlight | Well done.
I have been looking around and I'm pretty sure the Butyl acetate is a no-go in the production of Acetamide.
At least you have some experience distilling nail polish remover now for when you find an Acetone-free brand which contains Ethyl acetate.
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Finally I've got the right thing
I'll distill it when I'll have some time. Do you thing that the ethanol will be a problem?
However, here it is, acetone free NPR, with ethyl acetate:
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greenlight
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Put it in the distillation apparatus and collect the different fractions at different temperature ranges like you did the last bottle and take it
slow and see what you get. The boiling points are as follows:
Ethyl acetate = 77.1.C
Denatured alcohol = 78.3.C
Water = 100.C
The Ethyl acetate and Ethanol are very close together again so a fraction column would be recommended but you do not have one. If you have a spare
condenser you could attach it between the boiling flask and still head and pack it with broken glass to slow the vapors.
I think the Ethyl acetate may form and azeotrope with the Ethanol because of the very close boiling points and maybe even the water so they may come
over together regardless. 
If you get an azeotrope, they can be separated by extractive distillation with another solvent which doesn't look too difficult. I found this on a
patent:
"A method for recovering ethyl acetate from a mixture of ethyl acetate and ethanol which comprises distilling a mixture of ethyl acetate and ethanol
in the presence of an azeotrope forming agent, recovering the ethyl acetate and the azeotrope forming agent as overhead product and obtaining the
ethanol as bottoms product, wherein said azeotrope forming agent consists of one material selected from the group consisting of methyl formate,
2,2-dimethyl butane, hexane, cyclopentane, 2,2,4-trimethylpentane, t-butyl methyl ether, petroleum ether, dimethoxymethane and 4-methyl-2-pentanone."
And heres a link to another patent discussing the separation of Ethyl acetate and Ethanol by distillation with Methanol:
http://www.google.com/patents/US2649407
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DistractionGrating
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OK, this may not be a chemistry question, per se, but it does involve the physical properties of a substance, and so, please indulge me, if you will.
Some people assert that there are ways to somehow cut or grind holes in tempered glass without it shattering. Is this possible? If so, how?
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greenlight
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Distractiongrating, although not a chemistry question it can be cut and drilled if done the right way with a diamond bit and lubrication.
I attached a link below on how to drill a hole in tempered glass:
http://www.ehow.com/how_6813902_drill-hole-tempered-glass.ht...
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DistractionGrating
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Greenlight, The exact same source contains contradictory information that says glass must be drilled before tempering, and that it cannot be drilled
afterwards: http://www.ehow.com/facts_7714426_can-drill-hole-tempered-gl... I'm confused.
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DrMario
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| Quote: Originally posted by DistractionGrating | | OK, this may not be a chemistry question, per se, but it does involve the physical properties of a substance, and so, please indulge me, if you will.
Some people assert that there are ways to somehow cut or grind holes in tempered glass without it shattering. Is this possible? If so, how?
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We looked at this problem quite a bit, a couple of years ago, and the only safe way to "drill" holes in any sort of glass, is by sandblasting. The
sandblasting apparatus we're talking about is capable of making sub-mm diameter holes in glass plates, but we decided it's too expensive, and now
we're finally looking at a picosecond laser ablation system instead, which is more versatile.
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greenlight
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Yes, that is unusual how the same site contradicts itself.
The link says it is inadvisable because there is a high chance the glass will shatter and the diamond bit can get damaged, but if you have spare
sheets of glass you could give it a shot cause there is a small chance it may not shatter.
Otherwise, I think the only way to do it safely is what is suggested by DrMario, or maybe a water jet.
[Edited on 26-11-2014 by greenlight]
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xfusion44
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| Quote: Originally posted by greenlight | Put it in the distillation apparatus and collect the different fractions at different temperature ranges like you did the last bottle and take it
slow and see what you get. The boiling points are as follows:
Ethyl acetate = 77.1.C
Denatured alcohol = 78.3.C
Water = 100.C
The Ethyl acetate and Ethanol are very close together again so a fraction column would be recommended but you do not have one. If you have a spare
condenser you could attach it between the boiling flask and still head and pack it with broken glass to slow the vapors.
I think the Ethyl acetate may form and azeotrope with the Ethanol because of the very close boiling points and maybe even the water so they may come
over together regardless.
If you get an azeotrope, they can be separated by extractive distillation with another solvent which doesn't look too difficult. I found this on a
patent:
"A method for recovering ethyl acetate from a mixture of ethyl acetate and ethanol which comprises distilling a mixture of ethyl acetate and ethanol
in the presence of an azeotrope forming agent, recovering the ethyl acetate and the azeotrope forming agent as overhead product and obtaining the
ethanol as bottoms product, wherein said azeotrope forming agent consists of one material selected from the group consisting of methyl formate,
2,2-dimethyl butane, hexane, cyclopentane, 2,2,4-trimethylpentane, t-butyl methyl ether, petroleum ether, dimethoxymethane and 4-methyl-2-pentanone."
And heres a link to another patent discussing the separation of Ethyl acetate and Ethanol by distillation with Methanol:
http://www.google.com/patents/US2649407 |
Thanks for that
Hopefully I'll have some time today for this distillation, otherwise I'll do it ASAP.
I'll be back
Thanks
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