Phosphate ester preparation method

A phosphoric acid ester, esterification technology, applied in chemical instruments and methods, phosphorus organic compounds, compounds of elements of Group 5/15 of the periodic table, etc., can solve the difficulty of separation and recycling of alcohol, increase production cost and energy consumption, Long reaction time and other problems, to achieve the effect of stable product quality, high production efficiency and low production energy consumption

Active Publication Date: 2015-07-29
北京化工大学苏州(相城)研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the industry, phosphorus oxychloride is mostly added dropwise to a stirred tank, and it is prepared by direct esterification of alcohol and phosphorus oxychloride, which has the disadvantages of long reaction time, low production efficiency, and high alcohol unit consumption.
CN85104673A discloses a kind of production process of phosphoric acid ester, wherein the molar ratio of butanol and phosphorus oxychloride is as high as 7~12:1, and alcohol is excessive in a large number, makes the separation and recycle of alcohol in post-processing difficult, increases production cost and energy consumption
CN102040622A discloses a synthesis method of phosphoric acid ester. The esterification reaction process is to add phosphorus oxychloride dropwise to a butanol reactor with stirring. In the process of large-scale industrial production, the dropwise addition time is longer and the production efficiency is higher. Low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1 The preparation method of this phosphoric acid ester comprises:

[0049] (1) Put phosphorus oxychloride and ethanol into a high-gravity rotating packed bed reactor to mix and carry out esterification reaction to generate esterified products, wherein the molar ratio of phosphorus oxychloride to ethanol is about 1:3.3, super The rotating speed of the gravity rotating packed bed reactor is 100rpm, and the esterification reaction is carried out under reduced pressure, and the vacuum degree during the reduced pressure is selected at about 0.04MPa;

[0050] (2) React the product obtained in step (1) with sodium hydroxide solution to obtain phosphoric acid ester, and the yield of phosphoric acid ester is 93.1%.

Embodiment 2

[0051] Example 2 The preparation method of this phosphoric acid ester comprises:

[0052] (1) Input the mixture of phosphorus oxychloride, phenol and isooctyl alcohol into a high-gravity rotating packed bed reactor for mixing and carry out esterification reaction to generate esterified products, wherein the molar ratio of phenol to isooctyl alcohol is 1: 1. The molar ratio of phosphorus oxychloride to isooctyl alcohol is about 1:1, the rotation speed of the supergravity rotating packed bed reactor is 1500rpm, and the esterification reaction is carried out under reduced pressure. At about 0.098MPa;

[0053] (2) React the product obtained in step (1) with sodium carbonate solution to obtain phosphoric acid ester, and the yield of phosphoric acid ester is 92.5%.

Embodiment 3

[0054] Example 3 The preparation method of this phosphoric acid ester comprises:

[0055] (1) Put the mixture of phosphorus oxychloride, phenol and cyclohexanol into a supergravity fixed-rotor reactor to mix and carry out esterification reaction to generate esterified products, wherein the molar ratio of phenol to cyclohexanol is 1 : 1, the mol ratio of phosphorus oxychloride and phenol is about 1:1.5, and the rotating speed of supergravity fixed-rotor type reactor is 500rpm, and esterification is carried out under normal pressure;

[0056] (2) React the product obtained in step (1) with sodium carbonate solution to obtain phosphoric acid ester, and the yield of phosphoric acid ester is 90.7%.

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Abstract

The present invention discloses a phosphate ester preparation method, which comprises: (1) at least inputting phosphorus oxychloride and an organic hydroxy compound with a general formula of ROH into a super gravity rotating bed reactor, mixing, and carrying out an esterification reaction to generate an esterification product with a general formula of OP(Cl)m(OR1)x(OR2)y(OR3)z; and (2) carrying out a post-treatment on the esterification product obtained in the step (1) to obtain the phosphate ester with a general formula of OP(OH)m(OR1)x(OR2)y(OR3)z, wherein R, R1, R2 and R3 are organic groups, the organic groups comprise aliphatic groups, alicyclic groups or aromatic hydrocarbon groups, m is an integer of 0-2, m+x+y+z is 3, and x, y and z are selected from any one integer of 0-3. The preparation method of the present invention has advantages of simple process, high production efficiency, low production energy consumption, low production cost, and the like.

Description

technical field [0001] The invention relates to a method for preparing phosphoric acid esters, in particular to a method for preparing phosphoric acid esters using high-efficiency microscopic mixing technology-high gravity technology, and belongs to the technical field of organic synthesis. technical background [0002] Phosphate ester is an important chemical product, which is widely used in coatings, printing and dyeing, construction, oil exploration and other fields. It can be added to coatings and adhesives as a solvent, defoamer, plasticizer, etc., and can also be used as an extraction agent for rare metals. [0003] In the industry, phosphorus oxychloride is mostly added dropwise into a stirred tank, and it is prepared by direct esterification of alcohol and phosphorus oxychloride, which has disadvantages such as long reaction time, low production efficiency, and high alcohol unit consumption. CN85104673A discloses a kind of production process of phosphoric acid ester...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07F9/09C07F9/11C07F9/12
Inventor赵宏陈建峰刘海涛初广文周勃
Owner北京化工大学苏州(相城)研究院