Preparation method of 2-chloroethyl phosphate 2-(2-chloroethyl) ester by rearrangement reaction

Abstract

The invention discloses a preparation method of 2-chloroethyl phosphate 2-(2-chloroethyl) ester by rearrangement reaction. The method adopts an n-stage stepped tank continuous reaction. The 3-(2-chloroethyl) sub phosphate ester first enters the first-stage rearrangement kettle at a flow rate of 0.5 to 0.9 m3 / h. The 3-(2-chloroethyl) sub phosphate ester is heated to 140-150 DEG C under normal pressure in a class 1 rearrangement kettle. Then, the material is taken out from the outlet of the first-stage rearrangement circulator pump into the second-stage rearrangement kettle. The temperature of the material is increased by 5 to 10 DEG C under normal pressure. Then the material is taken out from the 2-stage rearrangement kettle and the operation is repeated until entering the n stage rearrangement kettle, and n is an integer from 3 to 6. The invention also discloses an ethephon preparation method. The method comprises the above process for 2-chloroethyl phosphate 2-(2-chloroethyl) ester by rearrangement reaction. The method makes the rearrangement reaction temperature easier to control, with more complete and thorough rearrangement reaction. The conversion of 3-(2-chloroethyl) subphosphate ester and the yield of 2-chloroethyl phosphate 2-(2-chloroethyl) ester can be increased.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a method for preparing 2-chloroethyl phosphate bis(2-chloroethyl) through rearrangement reaction of tris(2-chloroethyl)phosphite. Background technique [0002] The preparation of 2-chloroethyl phosphate bis(2-chloroethyl) by rearrangement reaction of tris(2-chloroethyl)phosphite is a key step in the production of ethephon. Practice has proved that the content of 2-chloroethyl phosphate bis(2-chloroethyl) ester plays an important role in the content and consumption of ethephon original drug, and the 2-chloroethyl phosphate bis(2-chloroethyl) in the rearrangement product ) The higher the ester content, the higher the ethephon content can be obtained, and the consumption of raw and auxiliary materials and by-products in the ethephon production process can be reduced. Most of the rearrangement processes in traditional ethephon production are produced by vertica...

AI Technical Summary

Problems solved by technology

However, because the rearrangement reaction is simply decoupled into two stages of preheating and rearrangement reactions, the requirements for controlling the reaction temperature are still very high. When the inlet temperature of the heat transfer oil is reduced from 160 °C to 155 °C, three (2 -Chloroethyl) phosphite conversion rate is greatly reduced