Sciencemadness Discussion Board

Asbestos catalyzed nitroethane synthesis design

PonderosaP - 12-8-2024 at 23:43

This is my first post, sorry if it belongs somewhere else. I want to remind anyone reading this that they're involved in such a cool online community. This extends to the 10 community members lurking around every single active poster. There aren't many gems like this one around anymore. Thank you.

Does anyone have any details about this process or what the construction of the apparatus entails? A blip exists about it in the wiki but I couldn't follow the information trail successfully.

I've had success with converting ethyl iodide to nitroethane using silver filings and sodium nitrite. I really appreciate the aroma of this compound and would like to perform this synthesis. My grandfather passed away from lung cancer a long time ago, probably in part because of his extremely large exposure profile to the wolly rock. He served years in the Navy during WWII on a ship, likely happily chiseling old boilers out or whatever. He regularly sanded his asbestos clad house in preparation for paint. (Don't worry he smoked like a chimney)

When it was finally my turn to rummage his old repair shop, I found some exiting treasures from the 50s. He left me a nearly brand new spool of "the finest PTFE coated asbestos rope produced, of exceptional purity"

Wil the catalyst be consumed during this reaction?

Thanks for coming to my TED TALK fellow madlads/lasses.

PonderosaP - 2-9-2024 at 17:10

At the risk of starting a thread doomed to obscurity due to overdiscussion and eye rolling specificity I offer an update;

Ive decided to fray/unwind a section of the packing rope to an extent sufficient to bypass removing the ptfe coating.

Ill fish this through a 10' stick of 1/2" EMT.
Ill then bend a bunch of U's into it to reduce how cumbersome it is.
Then ill add a 1/2" compression coupling and another 10' stick. Ill place a lawn sprinkler under this section. Finally ill terminate this section with an upward bend of about 30-50* with a drip loop of tie wire attached a few feet before the end of the pipe. The aim is to have a final "flat" leg of pipe which drips product into a steel or iron vessel on an icebath, free of cooling water contaminant but still in open air.

On the other end ill fit a male end via compression connector threaded onto a black iron tee. One side will be fitted with a silicone tube attached to a pressure cooker charged with ethyl alcohol. The other end will be fitted with a (pvc ?) check valve. On the inlet side of the check valve ill adapt a silicon tube to an empty 2 neck flask. The other neck will be adapted to a distillation setup or almbeic charged with copper sulfate/conc. Sulphuric acid ready to accept a nitrate salt and feed the requisite gas slowly.

Comments or suggestions are appteciated. Will update with results.

[Edited on 3-9-2024 by PonderosaP]

Rainwater - 2-9-2024 at 17:38

I suggest having the asbestos materials properly disposed of or if qualified, destroy it yourself.
Using a flux if 3 parts NaOH, 1 part Boric acid, you should be able to melt the material at about 750c. Once fully melted, it is not asbestos anymore.

I hate to recommend this but if you are exposed, or expose some one else, it can take days or 20 years for symptoms to start showing.

PonderosaP - 2-9-2024 at 18:27

Quote: Originally posted by Rainwater  
I suggest having the asbestos materials properly disposed of or if qualified, destroy it yourself.
Using a flux if 3 parts NaOH, 1 part Boric acid, you should be able to melt the material at about 750c. Once fully melted, it is not asbestos anymore.

I hate to recommend this but if you are exposed, or expose some one else, it can take days or 20 years for symptoms to start showing.


Thanks for your response! I didnt know that asbestos could be rended harmless this relatively easily. I wish the navy had bothered to do that with the stuff before they had gramps demo it on their ship as a teenager.

I could destroy this processed mineral wool. Then how could I achieve an alternative procedure to produce nitroalkanes using a modular apparatus in batch production without stinky halogens in a clean cheap and efficient manner without requiring gnarly carcinogenic solvents and painstaking liquid separations or extractions and such?

[Edited on 3-9-2024 by PonderosaP]

Rainwater - 3-9-2024 at 17:31

Quote: Originally posted by PonderosaP  
I didnt know that asbestos could be rended harmless this relatively easily.

Ya its just a mineral with a hair like crystal structure, lots of oxygen, silicon and some magnesium. The lye and boric acid drop the melting point and change the toxic hair like crystals into sodium silicate.
Quote:
how could I achieve an alternative procedure to produce nitroalkanes

Not sure, can you post some references your reading.

The only thing I was able to find on goodle was this paper about nitroalkanes being at higher consentrations in asbestos exposed lungs mater
https://www.jci.org/articles/view/3169/pdf

PonderosaP - 3-9-2024 at 18:49

Excuse me I shoild have posted the link in the OP
[Can a janitor reading this please edit my OP to include the obscure paywalled indian research paper from 1916 linked below? This is what Ive based my assumptions on and foolishly omitted.]

https://pubs.rsc.org/en/Content/ArticleLanding/1916/CT/CT916...

Adding:
I suspect the material you referenced actually gives a clue to the mechanism of this minerals peculiar [carcinogenic properties]. However i am certainly not an expert in these matters(or any other matters).

[Edited on 4-9-2024 by PonderosaP]

[Edited on 4-9-2024 by PonderosaP]

[Edited on 4-9-2024 by PonderosaP]

Rainwater - 4-9-2024 at 00:46

non paywall artical
It looks as if the asbestos was a substrate for the catalyst, and a catalytic converter would make a good replacment.

PonderosaP - 4-9-2024 at 09:46

Quote: Originally posted by Rainwater  
non paywall artical
It looks as if the asbestos was a substrate for the catalyst, and a catalytic converter would make a good replacment.


Thank you! That changes everything. Is the rearrangement of ethyl nitrite to nitroethane via Pt well known? I do think ive read that elsewhere.

Your link doesnt work for me.
Could you teach a man to fish? What did you use to cross reference search that article? Is there a unique ID to scholarly articles across different platforms?

Is there already a guide to this sort of question written somewhere?

I think i found the whole archive.

https://archive.org/details/journalchemical06britgoog/mode/1...

On the topic;

I'll cut out my catalytic converter soon and post updates as i build my setup. Thanks for the constructive redirection.

[Edited on 4-9-2024 by PonderosaP]

Rainwater - 4-9-2024 at 18:05

google link
Attached pdf

The catalyst is easy to make. But it's hard to make right.
I dont know the details of this reaction but pt partical size has a major effect of how it rearranges the bonds, if the crystals are to big you get slow reactions, to small and things go boom or woosh or just revert to carbon and diatomic nitrogen

Attachment: 10.1039_ct9160900701.pdf (463kB)
This file has been downloaded 67 times

Tips and tricks (youtube) for making a platnium on quartz wool catalyst
https://youtu.be/iaNSH89gpPk?si=5Ruyl-LdwVwULF23
The alcohol washing step is mostly optional unless sodium contamination with hurt your reaction

[Edited on 5-9-2024 by Rainwater]

j_sum1 - 4-9-2024 at 19:11

@PonderosaP
Welcome to the board.
Good discussion you opened up. I wish i had something constructive to contribute, but I have no experience of asbestos as a lab commodity and have not worked with nitroethane. You can be sure that there are others reading who will add something if they feel they have anything to say.

PonderosaP - 5-9-2024 at 06:56

Quote:

[Rainwater]
google link
Attached pdf

The catalyst is easy to make. But it's hard to make right.
I dont know the details of this reaction but pt partical size has a major effect of how it rearranges the bonds, if the crystals are to big you get slow reactions, to small and things go boom or woosh or just revert to carbon and diatomic nitrogen



Tips and tricks (youtube) for making a platnium on quartz wool catalyst
https://youtu.be/iaNSH89gpPk?si=5Ruyl-LdwVwULF23
The alcohol washing step is mostly optional unless sodium contamination with hurt your reaction

[Edited on 5-9-2024 by Rainwater]



Thank you, good video. Looks like very accessible chemistry.
If I understand what your implying(thanks for the clean dl link, I'm excited to finally read this in full) this is a repurposed ostwalt catalyst. A long and hot enough contact time may enable the feedstock of ethyl alcohol and ammonia? Or would the water generated bugger the reaction? From the first page they stipulate dry co2 to carry the dry ethyl nitrate, so probably not.
[Edit]some trace moisture is necessary, but not too much[/edit]
If I want to use my rope I'll definitely have to remove the ptfe coating, or I'll make some super toxic stinky fluorethylnitrite type garbage. That sounds gross. Might find another source of substrate or cut out my cat.

Is contact time important? A long unobstructed contact seems safer than a highly restrictive micropore ceramic.

[Edit]
4 to 5 hours at 120C
Looks like a long fractionation column would work better packed with catalyst under a heat lamp with reflux condenser back to the same flask.[/edit]

I only saw one reference to platinchloride, I don't understand where they actually say this is the catalyst on the asbestos substrate. Ostwalt patented his process 13 years earlier, wouldn't the Indian scientists need to reference this if they used his catalyst?

Do you know how important the purity of Pt is? I have a few (presumably more pure) Pt spark plugs I could carefully file for metal, or I could draw from the motherboard pile a board known to contain Pt. But separating this from other noble metals would be impossible.

I had assumed this metal mix would work well for something like this, as it would have a significant amount of silver admixture. I'll look in this direction for a reference as "my intuition" is garbage.
Quote:

[j_sum1]
Welcome to the board...


Thanks for dropping by, and for cleaning up the board.

[Edited on 5-9-2024 by PonderosaP]