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Purification method of 2-chloro-2-oxo-1, 3, 2-dioxaphospholane

A dioxaphospholane and purification method technology, which is applied in the direction of separation methods, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc., can solve the problems of large COP loss, easy decomposition, and high boiling point , to achieve the effect of improving equipment life, avoiding pyrolysis, and high safety factor

Active Publication Date: 2022-03-25
陆宽
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It can be seen that the boiling point of the raw material and various impurities in the crude COP product is relatively high and the melting point is quite different, and COP is heat-sensitive and easily decomposed by heat, so the purification method of traditional synthetic COP causes a large loss of COP
[0006] CN201910399054.2 discloses a method for preparing 2-chloro-2-oxo-1,3,2-dioxaphospholane, and prepares 2-chloro-2-oxo-1,3,2- The crude product of dioxaphospholane is based on the addition of fluorine-containing reagents in the synthesis reaction system, and the post-treatment can be obtained only through simple liquid separation and distillation. However, this COP purification method has two major drawbacks. The price of fluorine-containing reagents is extremely high, all rely on imports, and cannot be applied industrially; second, this purification method cannot completely remove the reaction solvent, and the residual solvent will affect the quality of subsequent products

Method used

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Embodiment 1

[0039] Get crude product COP altogether 100g, wherein impurity content is 10g, crude COP is purified, and purification process comprises the following steps:

[0040] (1) Under the protection of nitrogen, pass the crude product COP into the melting crystallizer, pass into the cooling water in the hollow fin type stirring, pass into the cooling water in the jacket of the melting crystallizer, control the temperature of the cooling water at 5 °C per hour Cool down to -25°C at a speed of 30 r / min while stirring slowly for 4 hours;

[0041] (2) After the crystallization of the crude COP is complete, open the discharge valve with the tetrafluoro filter plate at the bottom, let off the uncrystallized toluene, then close the bottom valve, and set the temperature of the cooling water in the jacket of the melting crystallizer and the hollow stirring at a rate of each Slowly heat up to 0°C at a speed of 0.5°C per hour, at this time, the crystallized crude COP begins to sweat once, and t...

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Abstract

The invention belongs to the technical field of a purification method of a phosphorus-containing organic compound intermediate 2-chloro-2-oxo-1, 3, 2-dioxaphospholane, and particularly relates to a purification method of 2-chloro-2-oxo-1, 3, 2-dioxaphospholane, in particular to a purification method of 2-chloro-2-oxo-1, 3, 2-dioxaphospholane. The purification method of the 2-chloro-2-oxo-1, 3, 2-dioxaphospholane comprises the following steps: introducing a crude product COP into a melt crystallizer, cooling to-25 DEG C at a speed of 5 DEG C / h, stirring, and crystallizing the COP; after COP crystallization is completed, the temperature of the melt crystallizer is increased to 0 DEG C at the speed of 0.5 DEG C / h, and primary sweating and secondary sweating are conducted; after sweating, raising the temperature to 25 DEG C at the speed of 5 DEG C / h; and continuously repeating the steps to obtain the high-purity COP. The purification method of 2-chloro-2-oxo-1, 3, 2-dioxaphospholane provided by the invention improves the COP yield and purity, prolongs the service life of equipment, saves energy, reduces emission, and is high in safety.

Description

technical field [0001] The invention belongs to the technical field of purification methods of phosphorus-containing organic compound intermediate 2-chloro-2-oxo-1,3,2-dioxaphospholane, and specifically relates to a 2-chloro-2-oxo-1, A method for purifying 3,2-dioxaphospholane. [0002] technical background [0003] 2-Chloro-2-oxo-1,3,2-dioxaphospholane (COP) is an important intermediate in the field of fine chemicals, mainly used for the synthesis of phospholipid amphiphiles with good biocompatibility compounds with broad application prospects. [0004] COP has a normal pressure boiling point of 270°C and a melting point of 12°C. It decomposes when it exceeds 120°C. It has the characteristics of high boiling point, easy to decompose when heated, and the chlorine content is corrosive. The traditional purification method is to use high vacuum vacuum distillation, but this The purification method has extremely high requirements on vacuum equipment, and high-vacuum vacuum dist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574B01D9/00B01D29/03
CPCC07F9/65742B01D9/0013B01D9/0031B01D29/03Y02P20/10
Inventor 陆宽
Owner 陆宽
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