dormouse (Member)
04-25-00 01:07
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Author  Topic:   Nitro toluene reduction 
Sky
Hive Bee   posted 01-31-2000 06:45 AM           
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Cheapskate Try the catalytic hydronation of nitro toluene its clean you can make your H2 in a simple H2 generator. just flush out air with H2 and seal container use Nickle as catylst heat up a little to product pressure then shake it up for a few minutes. removing the nickel is easier than that damn iron.All you have to do is seperate the isomers!
 
Cheapskate
Hive Bee   posted 02-02-2000 01:48 AM           
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SKY you tried this??
Cool, now more details, which kind of H2 generator did you use? What proportions? How did you connect it and what kind of pressure vessel did you have. How much pressure are we talking about here a couple of pounds or a whole bunch. Which nickel catalyst did you use and about what did it cost? What color is your hair and how tall are you. Is there anything good on TV tonight?

By the way, I managed to separate the isomers in the nitrotoluene stage yesterday while waiting for something else to cool

I put the nitrotoluene in the freezer and let it set for about an hour and damned if some of the stuff didn't freeze!! Let it set longer and no more froze. Filtered and tried it again and nothing froze. I had the frezer set to -5C to do this. Yes, I actually messed around with the temperature of the freezer. This stuff reduced just fine with the iron reduction (see the anthranilic thread for more details). Still had to steam distill though.


Sky
Hive Bee   posted 02-02-2000 05:03 PM           
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I used 2- 500 ml containers in one I place 100 ml of nitro toluene and and 10g of raney nickle , in the other container I put Zinc powder I ran a tube from one container too the other in the container with the nitro I placed another tube too release all of the air from the container in the other container I poured sulfuric acid on the Zinc and a lot of H2 started to bubble out I quickly sealed the container and allowed the H2 too fill the Container and flush out the air. After the container was flushed with H2 I removed the H2 generater and sealed the container. I swirled it around for a few minutes with no pressure then I shook it up vigerously mixing everything up covering the sides of the container with Nickle and nitro toluene. I placed the container in a oil bath but thought it might bust so I removed it was warm to the touch shook some more. by this time it was late so I left to go to bed the next after noon I went to check on it shook some more this shit was all over the sides. at this point I thought I was wasting my time and filled the container with DH2O and swirled around I did not see a seperation so I thought something must have Happened poured the liquid through 4 filteration and had distilled water with a yellow tint this has too be product . I had to leave project for a while so I don't know exact yeild but this as to be the stuff>
 
Sky
Hive Bee   posted 02-02-2000 10:43 PM           
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I wonder if the Nickel is nessesary it seems to me the H2 would take off the O to form water on its own and automatically take H2 in its place? I'm going to do more work on this
. the nitro molecule is easily aminated! If this step could be simplified it would make ludes alot easier too make.
 
KrZ
Hive Bee   posted 02-03-2000 12:00 AM           
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No you definitely need the nickel.
 
Cheapskate
Hive Bee   posted 02-03-2000 11:00 AM           
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o-toluidine is only barely soluable in water, but o-nitrotoluene is the same way. I wonder why you wound up with a mix that didn't separate.
I'm impressed that you didn't need any pressure!!! This could make the reaction really practical. I can't try this right now I have to leave town for work, but let me know what you see. I can help with it next week.

CS


Sky
Hive Bee   posted 02-09-2000 09:09 PM           
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The Nitro toluene did not reduce. I got a tank of H2 I'm going to put psi to the reaction this time. Can raney Ni be used over and over ? If so how many Times before its spent?
 
Sky
Hive Bee   posted 02-09-2000 09:15 PM           
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Cheapskate I was wondering if you tried freezing the Iron cl-Toluidine mix this might be a way to seperate?? Freeze pour off liquid like you did with the isomers?
 
Cheapskate
Hive Bee   posted 02-11-2000 06:58 PM           
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I don't think freezing would work. One of the problems is that the damn iron chloride mush holds too much of the target compound. If one can get the stuff out of the flask and into a vacuum filter and then rinse it with hot water to get the toluidine out, then freezing may separate it the rest of the way. This would really stink up the house though.
 
Sky
Hive Bee   posted 02-11-2000 08:02 PM           
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Thanks Cheapskate I'm still working on ways to simplify that reduction it is a pain. O-Toluidine is easy to purchase but it cost me 50$ plus 20$ shipping . I,m sure it could be made cheaper then this in bulk. I'm also a little paranoid about ordering it they mark the Damn box with DANGER and WARNING and shit like this.
 
Cheapskate
Hive Bee   posted 02-14-2000 06:58 PM           
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Yep, I encountered the same thing. Too much traffic in this will get you watched like a hawk, not as bad as acetic anhydride or red phosphorus though. As my name states, cheaper is better, but the reduction has to be made better somehow.
 
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