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Continuous preparation method of diphenyl isooctyl phosphate

A technology of diphenyl phosphate and isooctyl ester, which is applied in the fields of chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problem of difficult preparation of isooctyl alcohol and phosphorus oxychloride products, etc. problem, to achieve complete reaction, improve reaction efficiency, and reduce the effect of by-product formation

Active Publication Date: 2015-09-09
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method is to react phosphorus oxychloride and isooctyl alcohol at low temperature, and then react with phenol. This reaction requires low temperature, because phosphorus oxychloride and isooctyl alcohol are very easy, and it is difficult to prepare A single product of phosphorus, the reaction is very active

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] Example 1: The continuous preparation method of diphenyl-isooctyl phosphate

[0023] Put 76.5g (0.5mol) of phosphorus oxychloride (first, phosphorus oxychloride) into the preheater for preheating, the preheating temperature is 50-60°C, and add 0.75 g of Lewis acid (weight of phosphorus oxychloride) while preheating 1% of phenol), 94g (1mol) of phenol, are fed into the reaction tower through the transfer pump for reaction, the temperature of the reaction tower is 118-120°C, and the vacuum degree is 70-75KPa. In the reaction kettle, the top of the tower reaches 120°C, the bottom of the tower reaches 150°C, and the vacuum degree is 30 KPa. The intermediate of phenylphosphoryl chloride and part of phosphorus oxychloride evaporated by vacuum distillation are recovered and reused, and the remaining The intermediate diphenylphosphoryl chloride 183g (1mol) and isooctyl alcohol 195 (1.5mol) are pumped into the reaction tower for reaction. The temperature of the reaction tower is...

example 2

[0025] Example 2: The continuous preparation method of diphenyl-isooctyl phosphate

[0026] 153g (1.0mol) of phosphorus oxychloride (put phosphorus oxychloride in the preheater to preheat, the preheating temperature is 50-60°C, add 1.53g of magnesium chloride while preheating), 184g (1mol) of phenol , the phenylphosphoryl chloride 180g (0.55mol) that embodiment 1 reclaims reacts in the reaction tower input reaction tower through delivery pump, and the temperature of reaction tower is 115~120 ℃, and vacuum tightness 70~75KPa, after material reacts in reaction tower for 50 minutes, Put into the vacuum distillation tower, reach 125 DEG C at the top of the tower, reach 155 DEG C at the bottom of the tower, vacuum degree 30 KPa, obtain monochlorophosphate intermediate after vacuum distillation, intermediate 366g (2mol) and isooctyl alcohol 280 (2.2 mol) is pumped into the reaction tower for reaction. The temperature of the reaction tower is 65-70°C, the vacuum degree is 70-75KP...

example 3

[0027] Example 3: The continuous preparation method of diphenyl-isooctyl phosphate

[0028] Add 76.5g (0.5mol) of phosphorus oxychloride (first, put phosphorus oxychloride in the preheater to preheat, the preheating temperature is 50-60°C, add 0.8g of magnesium chloride while preheating), 94g (1mol) The phenylphosphoryl chloride 180g (0.5mol) that phenol, embodiment 1 reclaims carries out reaction in the input reaction tower through conveying pump, and the temperature of reaction tower is 118~120 ℃, and vacuum tightness is 70~75KPa, and material reacts in reaction tower after 30 minutes , into a vacuum distillation tower, reaching 120°C at the top of the tower, 150°C at the bottom of the tower, and a vacuum of 30 KPa. After vacuum distillation, the monochlorophosphate intermediate is obtained, the intermediate 183g (1mol) and isooctyl alcohol 141 ( 1.1mol) was pumped into the reaction tower for reaction. The temperature of the reaction tower was 68-70°C, the vacuum degree ...

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Abstract

The invention relates to a continuous preparation method of diphenyl isooctyl phosphate. The continuous preparation method of diphenyl isooctyl phosphate comprises the following steps: reacting phosphorus oxychloride with phenol under reduced pressure in a reactor; after the reaction is finished, performing reduced-pressure separation to obtain primary diphenylphosphinyl chloride; reacting diphenylphosphinyl chloride with isooctyl alcohol under reduced pressure; removing reacted hydrogen chloride gas and unreacted isooctyl alcohol to obtain a crude diphenyl isooctyl phosphate product; performing alkali washing and water scrubbing on the crude diphenyl isooctyl phosphate product; and performing reduced-pressure distillation for removing water, thus obtaining qualified diphenyl isooctyl phosphate. According to the continuous preparation method, since reactions are performed in a tower type reactor, the production cycle is greatly shortened to 3-4h and reduced by 50% as compared with the production cycle of discontinuous process reaction; therefore, the working efficiency is improved greatly and the production cost is lowered.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and specifically relates to a continuous preparation method of diphenyl-isooctyl phosphate which has a short production cycle, is economical, and is environmentally friendly and meets the requirements of industrial scale production. Background technique [0002] The continuous preparation method of diphenyl-isooctyl phosphate of the present invention adopts the reaction of phosphorus oxychloride and phenol with phenol, and then reacts with isooctyl alcohol to obtain the product. The traditional method is to react phosphorus oxychloride and isooctyl alcohol at low temperature, and then react with phenol. This reaction requires low temperature, because phosphorus oxychloride and isooctyl alcohol are easy to prepare, and it is difficult to prepare A single product of phosphorus, the reaction is very active. Contents of the invention [0003] The present invention overcomes the deficienc...

Claims

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Application Information

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IPC IPC(8): C07F9/12
Inventor 王秋伟王福兵金译平
Owner ZHEJIANG WANSHENG
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