Water phase high pressure method for preparing N,N'-di (m-tolyl) urea
A technology of tolyl and m-toluidine, applied in the N field, can solve the problems of troublesome recovery, high synthesis cost, expensive amyl alcohol, etc., and achieve the effect of simple reaction
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[0016] Example 1
[0017] 1) After mixing m-toluidine and water, add sulfuric acid dropwise to form a salt reaction. After dropping, add urea and stir; the equivalent ratio of m-toluidine to sulfuric acid is 1:0.95, and the molar ratio of m-toluidine to urea is 1: 0.5, the salt-forming reaction temperature is 0℃;
[0018] 2) Put the above reaction liquid into the autoclave, the autoclave pressure is 2atm, keep it for 5 hours, release the pressure, discharge, centrifuge and wash with hot water to obtain the finished product N,N'-bis(m-tolyl)urea The molar yield is 90%, based on m-toluidine.
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[0019] Example 2
[0020] 1) After mixing m-toluidine and water, add hydrochloric acid dropwise to form a salt reaction, add urea after dripping, and stir; the equivalent ratio of m-toluidine to hydrochloric acid is 1:1.05, and the molar ratio of m-toluidine to urea is 1: 1. The salt-forming reaction temperature is 80°C;
[0021] 2) Put the above reaction liquid into the autoclave, the autoclave pressure is 10atm, keep for 1 hour, then release the pressure, discharge, centrifuge, wash with hot water, get the finished product N,N'-bis(m-tolyl)urea The molar yield is 91%, calculated as m-toluidine.
Example Embodiment
[0022] Example 3
[0023] 1) After mixing m-toluidine and water, add phosphoric acid dropwise to form a salt reaction. After dropping, add urea and stir; the equivalent ratio of m-toluidine to phosphoric acid is 1:1, and the molar ratio of m-toluidine to urea is 1:1 0.5, the salt-forming reaction temperature is 0℃;
[0024] 2) Put the above reaction liquid into the high pressure reactor, the pressure of the high pressure reactor is 4atm, keep for 2 hours and then release the pressure, discharge, centrifuge, wash with hot water to obtain the finished product N,N'-bis(m-tolyl)urea The molar yield is 92%, calculated as m-toluidine.
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