Abdalrahman
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Whats the right method to make reaction between ethanol and phosphoric acid
How ethanol react with phosphoric acid to form 0,0diethyl phosphat
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j_sum1
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Thread Moved
9-12-2018 at 04:15 |
j_sum1
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Please do not double-post.
I have retained the clearer of your two threads and moved it to Beginnings where it belongs. However, it is still unclear what you intend to
accomplish. How much do you intend to produce? What purity is required? For what purpose? What equipment do you have access to?
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AJKOER
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Patent US 6673955B2
Preparation of triethyl phosphate
"Abstract
The invention relates to a process for preparing triethyl phosphate by reacting phosphorus oxychloride with a greater than stoichiometric quantity of
ethanol under reduced pressure at temperatures of from 0 to 50° C. in a reaction vessel, wherein
a) the volatile components resulting from the reaction are predominantly condensed by means of a reflux condenser and the remaining volatile
components are passed into a scrubber filled with water,..."
Link: https://patents.google.com/patent/US6673955B2/en
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Patent US 2712494A
"Phosphorus oxychloride, POC13, has been made by the oxidation of phosphorus trichloride, a slow process requiring the use of oxygen if any speed of
reaction is to be obtained. The phosphorus trichloride and oxygen are not common or easy to use and are suificiently expensive. Phosphorus oxychloride
has also been made by chlorinating tricalcium phosphate at high temperature, but in that process much of the chlorine is lost in forming by-product
calcium chloride, which has no value, and the process is wasteful.
It is an object of the invention to make POCls economically and speedily, in distinction to the phosphorus trichloride method, and with economy of
reagents and without inefficient side reactions, in distinction to the meal cium phosphate method.
The objects of the invention are accomplished, generally speaking, by reacting chlorine with a member of the group of the phosphorus acids and their
anhydrides, under reducing conditions, for instance in a reducing reaction medium, in he presence of a chlorination catalyst, for instance carbon, at
a temperature on the order of 300 to 700 C. Carbon is very satisfactory because it acts both as acatalyst and as a reducing agent, the reaction of
chlorine and P205 proceeding in its presence in accordance-with the equation a The reaction or" pyrophosphoric acid and chlorine is represented by the
equation,..."
Link: https://patents.google.com/patent/US2712494A/en
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Personally, in my opinion, I suspect there are much easier paths to the Ethyl radical and the Phosphate radical, and then, just let them interact.
Likely lower yield, harder to scale up for larger quantities, and associated impurities. However, also much more reagent accessible, less costly, less
dangerous prep, faster, and drawing less attention (actually, more like the extreme opposite, like approaching invisible).
[Edited on 9-12-2018 by AJKOER]
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Tsjerk
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Shitty question, Shitty answer
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unionised
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Not, I think, as bad a question as you think.
I'm fairly sure that the simple "boil the alcohol with the acid" approach doesn't work here.
If anyone knows a way to make diethyl phosphate using phosphoric acid as the reactant, I'd be interested to know about it.
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Tsjerk
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Is it really necessary for it to be the di-ethyl ester? It seems to be not too hard to make but harder to get a pure mono, di or tri ester.
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morganbw
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I truly believe that you will be more comfortable here if you show that you have actually studied/at least googled your questions before posting.
Just that you are asking the questions you are asking speaks loudly. Just explain that you have looked and cannot find what you are looking for.
A real trouble with a synth will probably be responded to. Asking how to do a particular synth with no background of trying will probably be ignored
or tossed.
Just my opinion and that is usually zero-sum.
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Loptr
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I dont think phosphate esters can be made with the acid, but instead require a phosphorus halide. I seem to recall one being phosphorus oxychloride,
which will react with an alcohol to form the trialkyl ester.
I recently looked into this, but cant recall the reason why it doesnt work right now. It's all about the mechanisms.
"Question everything generally thought to be obvious." - Dieter Rams
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