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Method and reaction device for synthesizing oligomeric alkyl phosphate by one-pot method

An oligomeric alkyl phosphate ester and a technology for a reaction device, which are applied in chemical instruments and methods, chemical/physical/physical-chemical stationary reactors, chemical/physical/physical-chemical nozzle reactors, etc., can solve the problem of high production costs. , long production cycle, low reaction efficiency and other problems, to achieve the effect of improving device production capacity, high volume utilization rate, and improving reaction efficiency

Active Publication Date: 2022-07-22
YUNNAN YUNTIANHUA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method and a reaction device for synthesizing oligomeric alkyl phosphates in one pot, so as to solve the problems of low reaction efficiency, long production cycle and high production cost in the existing traditional kettle production process

Method used

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  • Method and reaction device for synthesizing oligomeric alkyl phosphate by one-pot method
  • Method and reaction device for synthesizing oligomeric alkyl phosphate by one-pot method
  • Method and reaction device for synthesizing oligomeric alkyl phosphate by one-pot method

Examples

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Effect test

example 1

[0077] Adopt single-tank reactor, add phosphorus pentoxide automatic feeding purging unit and circulating flow jet reaction system, namely reaction device 100, and then adopt the following steps to carry out production operation:

[0078] (1) The triethyl phosphate of 6kg is added to the stirring reactor, that is, the container body 10, in, and then the phosphorus pentoxide of 3kg is slowly added. The material filling factor is controlled to be 0.7. During the addition, vigorous stirring was performed to prevent agglomeration, maintained for 1 hour, and the temperature was controlled at about 60°C to complete the first-step reaction.

[0079] (2) 25g of titanium oxide acetylacetone was added to the reaction system, and then slowly 3.24kg of ethylene oxide was introduced into the stirring reactor to react. After starting to feed ethylene oxide, control the temperature of the reaction system to gradually increase with the increase of the ethylene oxide feeding amount, and the r...

example 2

[0082]Using the optimized new high-efficiency reaction process and reaction device 100 of the oligomeric alkyl phosphate flame retardant, 4.5 kg of triethyl phosphate was added to the container body 10, and then 2.5 kg of phosphorus pentoxide was slowly added. During the addition process, vigorous stirring was performed to prevent agglomeration, maintained for 3 hours, and the temperature was controlled at about 60°C to generate the intermediate pyrophosphate. 20 g of α-stannous was added to the reaction system, and then a total amount of 2.4 kg of ethylene oxide was slowly introduced into the container body 10 to conduct the reaction. After starting to feed ethylene oxide, the temperature of the reaction system was controlled, the reaction temperature was maintained at 100°C, the ratio of the air flow rate to the liquid flow rate of the jet reactor 23 was 1:3, and after 42 hours, the acid value of the product was less than 1.5mg .KOH / g, stop the reaction, remove the residual ...

example 3

[0084] Using the optimized new high-efficiency reaction process and reaction device 100 of oligomeric alkyl phosphate flame retardant, 7.5 kg of trimethyl phosphate was added to the container body 10, and then 3.6 kg of phosphorus pentoxide was slowly added. During the addition, vigorous stirring was performed to prevent agglomeration, maintained for 4 hours, and the temperature was controlled at about 85°C to generate an intermediate pyrophosphate. 38 g of stannous octoate was added to the reaction system, and then 3.9 kg of ethylene oxide in total was slowly introduced into the container body 10 to carry out the reaction. After starting to feed ethylene oxide, the temperature of the reaction system was controlled, the reaction temperature was maintained at 135°C, the ratio of the air flow rate to the liquid flow rate of the jet reactor 23 was 1:4, and the acid value of the product was less than 1.5 after 36 hours of reaction. mg.KOH / g, stop the reaction to obtain the oligome...

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Abstract

The invention discloses a method for synthesizing oligomeric alkyl phosphate by a one-pot method and a reaction device, and relates to the field of flame retardant manufacturing. On the basis of a traditional alkyl phosphate synthesis production process, one-pot synthesis is adopted, the safety risk in the intermediate product transfer process is avoided, meanwhile, the continuous adding mode of solid materials is optimized, a circulating flow jet reaction system is added, and by controlling the temperature, pressure and other conditions of the reaction system, the alkyl phosphate is obtained. Finally, the synthesis process of the oligomeric alkyl phosphate is optimized, the safety risk is reduced, the reaction time is shortened, and the reaction efficiency is improved. The alkyl phosphate oligomer jet circulation flow reaction system can carry out gas and liquid mass transfer reinforced flow circulation in the reaction system, so that the reaction efficiency is greatly improved, and the production period is shortened. When the reaction system is used for synthesizing the alkyl phosphate oligomer, the time for obtaining the product with the same quality is only about 1 / 5-1 / 3 of that of a traditional method.

Description

technical field [0001] The invention relates to the field of flame retardant manufacturing, in particular to a one-pot method for synthesizing oligomeric alkyl phosphate and a reaction device. Background technique [0002] The traditional production of alkyl phosphate oligomers uses a tank reactor, which has mature technology, complex equipment, long production cycle and low production efficiency. The traditional kettle-type production process has extremely low gas-liquid reaction efficiency in the synthesis process. It takes at least 150 hours from the start of feeding materials to obtain qualified products, and the production cycle is long. The long production cycle makes the production cost of finished products high, which is not conducive to the stable control of product quality. During the reaction process, a large amount of unreacted ethylene oxide is enriched in the upper part of the reactor for a long time, which can easily cause the occurrence of ethylene oxide exp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/26B01J19/18B01F25/312B01F33/82
CPCB01J19/26B01J19/18
Inventor 马航李云东刘晨曦万邦隆梅连平朱境陆忠海张振环杨晓龙
Owner YUNNAN YUNTIANHUA
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