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A kind of preparation method of diphenyl phosphite

A technology of diphenyl phosphite and diphenyl phosphate, which is applied in the field of preparation of diphenyl phosphite, can solve problems such as reducing production efficiency, increasing environmental costs, and loss of raw materials, so as to improve production efficiency, solve cost increases, The effect of reducing production and environmental costs

Active Publication Date: 2022-06-03
JIANGSU EVERGREEN NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the phenol produced is often recovered and regenerated with phosphorus trichloride to produce triphenyl phosphite. Repeated recovery not only wastes energy and reduces production efficiency, but also the phenol recovered many times will gradually affect the product. Therefore, usually after recycling twice, phenol needs to be refined before it can be used continuously, and unusable residual waste liquid will inevitably be produced during this period, resulting in loss of raw materials and increased environmental costs

Method used

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  • A kind of preparation method of diphenyl phosphite
  • A kind of preparation method of diphenyl phosphite
  • A kind of preparation method of diphenyl phosphite

Examples

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Effect test

Embodiment 1

[0029] A preparation method of diphenyl phosphite, the preparation method comprises the following steps:

[0030] A. First use nitrogen to fully replace the air inside the reaction device, so that all the gases in the device are replaced with nitrogen, and the nitrogen concentration is more than 99%;

[0031] B. Add phenol and water to the reaction device, heat up to 80 °C, and stir for 0.1 hour to make the material uniform;

[0032] C, dropwise add phosphorus trichloride to the mixture of phenol and water stirred in the step B to form a material, and the dropwise addition duration of phosphorus trichloride is 3 hours. In this embodiment, the molar ratio of phosphorus trichloride to phenol and water is 1:1.5:1.5;

[0033] D, in step C, material is warming up to 105 ± 5 ℃, and keep stirring in this temperature interval, and stirring time is 8 hours;

[0034] E. The hydrogen chloride gas generated in the material is discharged through the method of vacuum distillation and nitr...

Embodiment 2

[0037] A preparation method of diphenyl phosphite, the preparation method comprises the following steps:

[0038] A. First use nitrogen to fully replace the air inside the reaction device, so that all the gases in the device are replaced with nitrogen, and the nitrogen concentration is more than 99%;

[0039] B. Add phenol and water into the reaction device, heat up to 35 °C, and stir for 1 hour to make the material uniform;

[0040] C. Phosphorus trichloride is added dropwise to the mixture of phenol and water stirred in step B, and the dropwise addition duration of phosphorus trichloride is 12 hours. In this embodiment, the molar ratio of phosphorus trichloride to phenol and water is 1:2.3:0.7;

[0041] D, the material in step C is warmed up to 135 ± 5 ℃, and keep stirring in this temperature interval, and the stirring time is 0.5 hour;

[0042] E. The hydrogen chloride gas produced in the material is discharged through the method of vacuum distillation and nitrogen introd...

Embodiment 3

[0045] A preparation method of diphenyl phosphite, the preparation method comprises the following steps:

[0046] A. First use nitrogen to fully replace the air inside the reaction device, so that all the gas in the device is replaced with nitrogen, and the nitrogen concentration is more than 99%.

[0047] B, then add phenol and water in the reaction unit, be warming up to 65 ℃, stir for 0.5 hour to make the material uniform;

[0048] C, drip phosphorus trichloride in the phenol and water mixture after described step B stirring, and phosphorus trichloride dripping duration is 8 hours. In this embodiment, the molar ratio of phosphorus trichloride to phenol and water is 1:1.9:1.1;

[0049] D. Heat the material in step C to 120±5°C, and keep stirring at this temperature interval, and the stirring time is 4 hours.

[0050] , and then discharge the hydrogen chloride gas generated in the material by vacuum distillation and introducing nitrogen gas, and control the vacuum degree to...

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Abstract

The invention discloses a preparation method of diphenyl phosphite. In the method, phosphorus trichloride, phenol and water are used as raw materials. After the reaction is completed, the diphenyl phosphite is obtained by depressurizing and introducing nitrogen gas to eliminate by-product hydrogen chloride. The method does not produce phenol as a by-product, solves the problems of increased cost and waste liquid treatment caused by repeated recovery of phenol, simplifies the production process, improves production efficiency, and does not need to use a large amount of phosphorous acid in the production process, greatly reducing production Risk, reduced production cost and environmental cost, suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of diphenyl phosphite. Background technique [0002] Diphenyl phosphite is a commonly used additive in PVC. The method for preparing diphenyl phosphite reported in the literature mainly includes the following: [0003] 1. It is prepared by acid hydrolysis of diphenylalkyl (ethyl or propyl) phosphite, the reaction equation is as follows: [0004] [0005] Diphenyl alkyl phosphite and anhydrous hydrogen chloride undergo an acid hydrolysis reaction to obtain the main product diphenyl phosphite after removing the by-product chlorinated alkyl. The starting material of this method, diphenylalkyl phosphite, is relatively expensive and not economical in production. [0006] Prepared by the reaction of triphenyl phosphite and phosphorous acid, the reaction equation is as follows: [0007] [0008] E. N. Walsh mixes 1 mol of triphenyl phosphite and 0.5 mol of phosphorous acid at 25 °C, and protects the reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/145
CPCC07F9/145Y02P20/10
Inventor 曾繁馨雷树敏缪栋
Owner JIANGSU EVERGREEN NEW MATERIAL TECH
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