Continuous industrial production method of high-purity bisphenol A-bis (diphenyl phosphate)

A technology of diphenyl phosphate ester and production method, which is applied in the fields of chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problem of low production yield, harm to human health, and chemical plant bubbles. Problems such as dripping and leaking can be avoided, and the effect of reducing production costs, improving labor efficiency, and reducing labor intensity can be achieved.

Active Publication Date: 2021-02-26
ZHEJIANG WANSHENG
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  • Application Information

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Problems solved by technology

Usually, BDP produced by this industrial method usually contains about 1-3% of triphenyl phosphate TPP and about 1% of isopropenylbenzenediphenyl ester. These two substances are harmful substances, and isopropyl is unstable. Phenomenon, the existence of isopropenyl group makes the color of the product darken when it is exposed to light, and the existence of TPP will cause defects, pollution and corrosion of the molded product. After entering the material, it is prone to volatilization, seepage and other problems, which will ...

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  • Continuous industrial production method of high-purity bisphenol A-bis (diphenyl phosphate)

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Embodiment 1

[0030] A continuous industrial production method of high-purity bisphenol A-bis(diphenyl phosphate), specifically comprising the following steps:

[0031] 1. Multi-level cross-linking reaction:

[0032] Phosphorus oxychloride 4500Kg / h, magnesium chloride 20Kg / h, bisphenol A 1200kg / h are continuously fed into the pre-mixing tank in proportion, and after heating and pre-mixing in the pre-mixing tank, the reaction liquid in the pre-mixing tank is continuously The feeding method flows from the first-stage reactor to the fourth-stage reactor, the reaction temperature of the first-stage reactor is 80-85°C, the reaction temperature of the second-stage reactor is 90-100°C, and the reaction temperature of the third-stage reactor The reaction temperature is 100-110°C, the reaction temperature of the fourth-stage reactor is 110-120°C, the residence time of materials in each reactor is 2 hours, and the reaction pressure is controlled at -0.015mpa~-0.02mpa.

[0033]The reaction liquid flo...

Embodiment 2

[0060] Substantially the same as Example 1, the phosphorus oxychloride amount is changed into 5500kg / h, and other reaction conditions are constant.

Embodiment 3

[0062] Basically the same as in Example 1, the ratio of the two feeds of bisphenol A is changed to 70% of the total amount of bisphenol A added for the first time (that is, the flow rate of the first part of bisphenol A that first participates in the reaction is 1050kg / h), Add the remaining 30% for the second time (that is, the flow rate of bisphenol A participating in the reaction in the second part of the later stage is 450kg / h), and the other reaction conditions remain unchanged, and the test is carried out.

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Abstract

The invention discloses a continuous industrial production method of high-purity bisphenol A bis (diphenyl phosphate). The method comprises the following steps: dividing bisphenol A into two parts, mixing part of bisphenol A with phosphorus oxychloride and a Lewis acid catalyst, adding the mixture into a continuous multistage crosslinking reactor, reacting, and evaporating to remove excessive phosphorus oxychloride after the reaction is ended, adding an organic alkali acid-binding agent into the distillation residual liquid to react with the residual bisphenol A for 1.5-3 hours at the temperature of 115-120 DEG C to obtain an intermediate product reaction liquid, mixing the intermediate product reaction liquid with phenol, feeding the mixture into a multi-stage esterification reactor for esterification reaction, continuously supplying consumed phenol in the esterification process, and obtaining a crude product after the reaction is finished; and sequentially carrying out continuous acid washing, continuous alkali washing, continuous water washing, continuous solvent recovery and filtration to obtain the bisphenol A-bis (diphenyl phosphate) finished product. According to the method,the production cost is reduced, the product yield is increased to 97% or above, the product color number is increased to 50 or below, TPP is controlled to be 0.1%, isopropenyl phenyl diphenyl phosphate is smaller than 50 ppm, and fluctuation of quality indexes of all products is small.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a continuous industrial production method of high-purity bisphenol A-bis(diphenyl phosphate). Background technique [0002] The molecular formula of bisphenol A-bis(diphenyl phosphate) (BDP for short) is C 39 h 34 o 8 P 2 , the molecular weight is 692, and its structural formula is as follows: [0003] , [0004] Bisphenol A-bis(diphenyl phosphate) is an oligomeric non-halogenated flame retardant and also a good plasticizer, mainly used in thermoplastic engineering plastics such as PC, ABS, PC / ABS, PPO / Epoxy resin and its polymers for HIPS rigid circuit board, its flame retardant performance is much better than traditional flame retardants such as alkyl phenyl phosphate. With the widespread popularization of new energy vehicles in recent years, the demand for bisphenol A-bis(diphenyl phosphate) has increased significantly, and the market is in shor...

Claims

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Application Information

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IPC IPC(8): C07F9/12
CPCC07F9/12
Inventor 李旭锋吕云兴王秋伟吴宪水
Owner ZHEJIANG WANSHENG
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