Method for producing high quality triarylphosphate

A technology of a triaryl phosphate ester and a production method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Effect

Active Publication Date: 2011-07-13
泰州市永昌化工有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

In the existing method, only the front fraction is collected for re-esterification during distillation, resulting in the unqualified acid value of the finished product. A post-treatment process is often added, that is, re-washing and dehydration of the unqualified product, thereby increasing production. time and production equipment, while a certain amount of waste water
In addition, the reaction is not complete enough, it is difficult to obtain high yield, high purity, high quality triaryl phosphate products

Method used

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Experimental program
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Effect test

Embodiment Construction

[0016] Concrete steps of the present invention are as follows:

[0017] a. Alkylation reaction, put 600Kg of melted phenol into a 1000-liter reactor, start stirring, and inject steam into the jacket of the reactor to raise the temperature in the reactor to 115°C, then start to feed propylene Until the mass ratio of phenol to propylene is 1:0.16, the reaction temperature is controlled by the amount of feed in the whole feeding process, the reaction temperature is kept at 115-125 ° C, and the reaction time is 9-10 hours; after that, the deepening reaction is carried out, and the time is 0.5 -1 hour, flush with nitrogen to cool, and keep the temperature at 50-55°C.

[0018] b. Esterification reaction. Inhale the finished material of the alkylation reaction into the esterification reaction kettle, turn on the stirring, turn on the electric heating switch, raise the reaction temperature to 60°C, and start to add phosphorus oxychloride dropwise. The whole dropping process starts wit...

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Abstract

The invention discloses a producing method of tri(4-isopropylphenyl)phosphate. In the exisint method, the acid value of the finished product is not qualified, an extra post treatment procedure is often needed, and the tri(4-isopropylphenyl)phosphate products with high yield, high purity and high quality are hard to be obtained. The producing method comprises the following steps in sequence: melt phenol is put into a reaction kettle; propylene is pumped into the reaction kettle and the reaction temperature is kept between 115 DEG C to 125 DEG C; the materials treated with the action are put into an esterification kettle, the temperature is kept between 60 DEG C to 80 DEG C and phosphorus oxychloride is dripped in; the materials after being esterified is pumped into a distillation kettle for distillation; the front cut fraction and the after cut fraction obtained from the distillation are returned to the esterification kettle for esterification reaction, and the middle fraction is the finished tri(4-isopropylphenyl)phosphate product.

Description

technical field [0001] The invention discloses a production method of high-quality triaryl phosphate. Background technique [0002] High-quality triaryl phosphate is mainly used as a flame-retardant plasticizer for synthetic rubber such as rubber products, PVC plastic flame-retardant conveyor belts, leather, tarpaulins, agricultural mulch, floor materials, wires, cables, neoprene rubber, and NBR. , flame retardant of epoxy resin, can also be used as anti-pressure additive of cutting oil, gear oil, calendering oil, etc. In the existing method, only the front fraction is collected for re-esterification during distillation, resulting in the unqualified acid value of the finished product. A post-treatment process is often added, that is, re-washing and dehydration of the unqualified product, thereby increasing production. Time and production equipment, while there is a certain amount of waste water. In addition, the reaction is not complete enough, and it is difficult to obta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/12
Inventor 陈冬根
Owner 泰州市永昌化工有限公司
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