Preparation of bisphenol A bis(diphenyl phosphoester )

A technology of diphenyl phosphate and phenol is applied in the field of preparation of bisphenol A, which can solve the problems of unstable purity of target product, impact on production environment, and difficulty in complete reaction, achieve good economic and social benefits, and reduce labor. Strength, the effect of avoiding corrosion

Active Publication Date: 2009-01-21
山东旭锐新材股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods all are to adopt the mode of solid bisphenol A to add material to carry out, difficult reaction is complete; Reaction is carried out under non-vacuum state, because the influence of air easily

Method used

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  • Preparation of bisphenol A bis(diphenyl phosphoester )

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1, 80g (0.351mol) bisphenol A and 245g (1.596mol) phosphorus oxychloride are added to the four ports of dry, replaced with nitrogen and equipped with stirrer, thermometer, nitrogen inlet pipe, oil heating device In the flask, raise the temperature to 60°C and stir slowly until the bisphenol A is completely dissolved, as the dissolved material, keep warm for later use; weigh 1.5g of anhydrous aluminum trichloride and 100g (0.651mol) of phosphorus oxychloride In a four-necked flask equipped with a stirrer, reflux pipe, thermometer, nitrogen gas introduction pipe, heating device and hydrogen chloride absorption device, the temperature was raised rapidly to 90 °C, and then the above dissolved materials were slowly added dropwise, and added dropwise over 3 hours. Completed, then reacted for 2 hours under the condition of gradient temperature increase from 110°C to 130°C, then cooled the material to below 60°C under the condition of feeding a small amount of nitroge...

Embodiment 2

[0019] Embodiment 2, 80g (0.351mol) bisphenol A and 230g (1.503mol) phosphorus oxychloride are made into dissolved material; Weigh 1g anhydrous aluminum trichloride and 90g (0.586mol) phosphorus oxychloride in four ports Rapidly heat up to 70°C in the flask, then add the above-mentioned dissolved materials dropwise in the time of 2 hours, distill out excessive phosphorus oxychloride after the completion of the reaction, add 127g (1.351mol) phenol in the material that has been distilled. React for 8 hours under the condition of gradient temperature rise from 70°C to 150°C, and finally wash to obtain the target product. Other technical characteristics are the same as embodiment 1.

Embodiment 3

[0020] Embodiment 3, 80g (0.351mol) bisphenol A and 280g (1.824mol) phosphorus oxychloride are made into dissolved material; Weigh 2g anhydrous aluminum chloride and 150g (0.977mol) phosphorus oxychloride in four ports Rapidly heat up to 80°C in the flask, then add the above-mentioned dissolved materials dropwise in the time of 2 hours, distill out excessive phosphorus oxychloride after the completion of the reaction, add 136g (1.446mol) phenol in the material that has been distilled. React for 10 hours under the condition of gradient temperature rise from 70°C to 150°C, and finally wash to obtain the target product. Other technical characteristics are the same as embodiment 1.

[0021] It is found through testing that the product prepared by using the preparation method of the present invention has stable quality and superior performance, and its normalized area is 4% higher than that of the product prepared by the existing method on average. The following table is the HPLC ...

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Abstract

The invention provides a method for preparing bisphenol A bi-(diphenyl phosphate). The method is characterized in that the proper amount of bisphenol A and phosphorus oxychloride is added in a reactor, and subjected to heating and stirring until bisphenol A is completely dissolved, and dissolved materials are obtained; the proper amount of Lewis acid and phosphorus oxychloride is added in a reactor provided with a chlorine hydride absorption device and subjected to quick heating, the dissolved materials are added in the reactor, the excessive phosphorus oxychloride is distilled off after the reaction finishes, and the proper amount of phenol is added, the temperature is adjusted until the reaction finishes, and the finished product is obtained after washing and debenzolization. The product prepared by the process of the invention has the advantages of having good product quality, lowering labor intensity, improving working environment and having better economic and social benefits.

Description

Technical field [0001] The invention belongs to a preparation method of bisphenol A bis(diphenyl phosphate). Background technique [0002] Bisphenol A bis(diphenyl phosphate) belongs to a new generation of condensed non-halogenated organophosphorus flame retardants. It has excellent thermal stability and low volatility, and is widely used in flame retardant PVC, cellulose resin, synthetic Rubber, phenolic resin, epoxy resin, polyester fiber, etc. are also flame retardants and extreme pressure wear-resistant agents for lubricating oil esters. At present, there are three main synthetic methods of bisphenol A bis(diphenyl phosphate): one is to react bisphenol A with phosphorus oxychloride to obtain bisphenol A (bis-dichlorophosphate), and then use phenol to block , Obtain target product; The 2nd, obtain diphenylphosphoryl chloride with phenol reaction earlier with phosphorus oxychloride, then obtain target product with bisphenol A reaction; Dichlorophosphate) to obtain the ta...

Claims

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Application Information

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IPC IPC(8): C07F9/32C09K21/12
Inventor 杨树仁郝建港王志强张荣华段俊彪于文智王洪刚
Owner 山东旭锐新材股份有限公司
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