Preparation process of triethylphosphite

A technology of triethyl phosphite and preparation process, applied in the field of chemical production, can solve the problems of small production capacity, long production cycle, large material consumption, etc., and achieve the effects of strong production capacity, stable product quality, and simple control links

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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The N,N-dimethylaniline method is a batch production method; this method has small production capacity, long production cycle per unit product, large material consumption, unstable product quality, high cost, all by-products are discharged, and "three wastes" are discharged The amount is large, the waste water contains carcinogens, and it is difficult to treat, and the quality and yield of the product cannot be guaranteed
[0004] Another production method is called the triethylamine method, which is a continuous production method; this method has large production capacity, stable product quality, and relatively low cost, but all by-products are discharged. Sodium, resulting in high wastewater treatment costs, greatly increased production costs, generally unaffordable for enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add absolute ethanol, phosphorus pentachloride, dimethylaniline, and triethylamine to the esterification kettle for esterification reaction at normal temperature and pressure; among them, control the content of dimethylaniline to 45%, and the content of triethylamine to 8%. , the content of absolute ethanol is 30%; the reaction temperature is 10°C, and the time is 1 hour. After the esterification reaction is completed, the material is filtered, and then it is put into the neutralization tank, and soda ash is added under the condition of stirring. And react, adjust to the pH value of material at 6.

[0018] After the neutralization reaction is completed, the material is subjected to initial distillation. During the initial distillation, the temperature in the crude distillation tower is controlled. When the temperature in the distillation tower is 85°C, low-boiling components are distilled from the top of the distillation tower, i.e. dimethylaniline, The mixture of triet...

Embodiment 2

[0021] Add absolute ethanol, phosphorus pentachloride, dimethylaniline, and triethylamine to the esterification kettle for esterification reaction at normal temperature and pressure; among them, control the content of dimethylaniline to 55%, and the content of triethylamine to 10%. , the content of absolute ethanol is 40%; the reaction temperature is 25°C, and the time is 2.5 hours. After the esterification reaction is completed, the material is filtered, and then it is put into the neutralization tank, and soda ash is added under the condition of stirring. And react, adjust to the pH value of material at 7.

[0022] After the neutralization reaction is completed, the material is subjected to initial distillation. During the initial distillation, the temperature in the crude distillation tower is controlled. When the temperature in the distillation tower is 100°C, low boiling point components are distilled from the top of the distillation tower, namely dimethylaniline, The mix...

Embodiment 3

[0025] Add absolute ethanol, phosphorus pentachloride, dimethylaniline, and triethylamine to the esterification kettle for esterification reaction at normal temperature and pressure; the content of dimethylaniline is controlled at 50%, and the content of triethylamine is 9%. , the content of absolute ethanol is 35%; the reaction temperature is 20°C, and the time is 2 hours. After the esterification reaction is completed, the material is filtered, and then it is put into the neutralization tank, and soda ash is added under the condition of stirring. And react, adjust to the pH value of material at 6.5.

[0026] After the neutralization reaction is completed, the material is subjected to initial distillation. During the initial distillation, the temperature in the crude distillation tower is controlled. When the temperature in the distillation tower is 95°C, low boiling point components are distilled from the top of the distillation tower, i.e. dimethylaniline, The mixture of tr...

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Abstract

The invention relates to a preparation process of triethylphosphite, belonging to the technical field of chemical production. Absolute alcohol and phosphorus pentachloride are adopted as main raw materials, and dimethylaniline and triethylamine are adopted as solvents. Production capacity is high and product quality is stable. When the entire operating system reaches equilibrium, control links arevery simple, and process indicators of the product are basically balanced.

Description

technical field [0001] The invention relates to a preparation process of triethyl phosphite, which belongs to the technical field of chemical production. Background technique [0002] Triethyl phosphite is an important pharmaceutical and pesticide intermediate, and also a main raw material for the production of plasticizers, stabilizers, brighteners, and additives in plastics, dyes, and lubricating oils. In recent years, as the global requirements for safety and environmental protection have become higher and higher, phosphorus-based non-toxic flame retardant products with triethyl phosphite as the main raw material have also received widespread attention and development. At present, there are two main production methods for the production of triethyl phosphite using phosphorus trichloride and absolute ethanol as raw materials in China; one is called N,N-dimethylaniline method, that is, xylene (or mixed benzene) is used as Solvent, using N,N-xylidine as an acid-binding agen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
CPCC07F9/142
Inventor 黄祥安鄢丙东罗方明易继舫李杰代小堂
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