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Preparation method of bisphenol A-bis(diphenyl phosphate)

A technology of diphenyl phosphate and phenol, which is applied in the field of bisphenol A-bis preparation, can solve problems affecting human health and life, and achieve the effects of reduced impurity content, stable method, and increased purity

Inactive Publication Date: 2019-10-11
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The products of the above two reactions are harmful substances, which will affect human health and life in the process of adding flame retardants to prepare PC / ABS, PPO / HIPS engineering materials

Method used

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  • Preparation method of bisphenol A-bis(diphenyl phosphate)
  • Preparation method of bisphenol A-bis(diphenyl phosphate)
  • Preparation method of bisphenol A-bis(diphenyl phosphate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1. Esterification reaction: add 150g (0.66 moles) of bisphenol A, 15g catalyst magnesium chloride, and 200g xylene into a four-neck flask, raise the temperature to 90-100°C, and slowly add 335g (2.18 moles, bisphenol The molar ratio of A to phosphorus oxychloride is 1: 3.3), and the dropwise addition is completed in 2 hours. After the addition, it is kept at 105-110°C for 2.5 hours. Distill at 2-3KPa until the temperature is 130-140°C, stop the distillation, and obtain the polycondensed phosphorus oxychloride intermediate;

[0049] 2. Capping reaction: Control the temperature at 130-140°C and add 230g of phenol dropwise (2.4 moles, the molar ratio of bisphenol A to phenol is 1:3.6), add it in about 3 hours, keep it warm for 2 hours, and recover the phenol under vacuum Temperature is 2~3KPa, temperature is 130~140 ℃, obtain bisphenol A-bis(diphenyl phosphate) crude product;

[0050] 3. Crude product refinement: Alkaline washing of bisphenol (diphenyl phosphate) and water ...

Embodiment 2

[0059] It is basically the same as Example 1, but toluene is used as the solvent instead, and the others remain unchanged, and the yield is 96.8%.

Embodiment 3

[0061] Basically the same as Example 1, the vacuum of phosphorus oxychloride distilled under reduced pressure is 2.8~3KPa, and the others are unchanged, and the yield is 96.4%.

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Abstract

The invention relates to a preparation method of bisphenol A-bis(diphenyl phosphate). The preparation method comprises the following steps of 1, an esterification reaction, wherein phosphorus oxychloride is dropwise added into a bisphenol A solution containing a solvent, the esterification reaction is conducted in the presence of a Lewis catalyst, and reduced pressure distillation is conducted onthe phosphorus oxychloride after the reaction is completed; 2, an end-capping reaction, wherein end capping is conducted by using phenol, the phenol is recycled under reduced pressure to obtain a bisphenol A-bis(diphenyl phosphate) crude product; 3, refining of the crude product, wherein the crude product is washed with alkali and water, and then reduced pressure distillation is conducted to obtain the product. According to the method, the phosphorus oxychloride is dropwise added into the solution of bisphenol A and xylene or toluene, the method is convenient and reliable to use and easy to operate and does not need special equipment, the solvent can be recycled, the consumption is reduced, the quality of products in a batch production process is ensured, the yield is stable, and high-endproducts can be stably generated.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, and relates to a preparation method of bisphenol A-bis(diphenyl phosphate). Background technique [0002] Bisphenol A Bis (Diphenyl Phosphate) (Bisphenol-A Bis (Diphenyl Phosphate), referred to as BDP) molecular formula is C 39 h 34 o 8 P 2 , the molecular weight is 692.63, and its structural formula is as follows: [0003] [0004] Bisphenol A-bis(diphenyl phosphate) is a colorless or light yellow liquid, insoluble in water, and miscible with dichloromethane, toluene, methanol and methyl ethyl ketone. Density (25°C) 1.26g / ㎝ 3 , the viscosity (40°C) is about 2200mpa.s, and the temperatures for TGA weight loss of 5%, 10% and 50% are 371°C, 397°C and 444°C, respectively. [0005] At present, about the preparation method: mainly adopt phosphorus oxychloride to react with bisphenol A, distill phosphorus oxychloride under reduced pressure, and then carry out end-capping treatment wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12
CPCC07F9/12
Inventor 冯舜牛丽丹金译平
Owner ZHEJIANG WANSHENG
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