Industrial preparation method of bisphenol A bis(diphenyl phosphate) with low triphenyl phosphate content

A technology of phenyl phosphate polycondensation and triphenyl phosphate, which is applied in the field of industrial preparation of bisphenol A phenyl phosphoric polycondensate, can solve the problem of physical properties affecting the flame retardancy of products, molded product defects, and easy occurrence Volatilization, seepage and other issues

Active Publication Date: 2015-11-11
ZHEJIANG WANSHENG
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AI Technical Summary

Problems solved by technology

However, engineering plastics are usually processed at a high temperature above 200°C, so the following problems will occur during the processing of flame-retardant engineering plastics: when using low-molecular-weight phosphate ester flame retardants such as triphenyl phosphate (TPP) When the low molecular weight phosphate flame retardant is decomposed due to its low thermal decomposition temperature during the molding process, the decomposition products will pollute the mold and produce poor molded products, and sometimes even decompose corrosive substances to cause the mold to break down. Corrosion damage, and because of its low molecular weight, it is prone to problems such as volatilization and exudation, which will affect the flame retardancy and other physical properties of the product
Usually, BDP produced on an industrial scale usually contains about 1-3% triphenyl phosphate TPP, and the existence of TPP will cause defects, pollution and corrosion of molds, and it is prone to volatilization and seepage after entering the material. Affect the flame retardancy and other physical properties of the product

Method used

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  • Industrial preparation method of bisphenol A bis(diphenyl phosphate) with low triphenyl phosphate content
  • Industrial preparation method of bisphenol A bis(diphenyl phosphate) with low triphenyl phosphate content
  • Industrial preparation method of bisphenol A bis(diphenyl phosphate) with low triphenyl phosphate content

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preparation example Construction

[0033] The industrialized preparation method of bisphenol A phenyl condensed phosphate with low triphenyl phosphate content of the present invention comprises the following steps:

[0034] 1) Put phosphorus oxychloride 4-10 times the molar amount of bisphenol A into the reaction kettle equipped with bisphenol A solid twin-screw feeder, phosphorus oxychloride reflux and vacuum distillation device, and hydrogen chloride gas absorption device, Add a catalyst with 0.2-1% of the weight of phosphorus oxychloride, raise the temperature to 90-100°C, use a twin-screw feeder to continuously add bisphenol A accounting for 90-99% of the total amount of bisphenol A, and after the addition is completed, the temperature is 100-110°C Insulation under heat until the reaction is complete; the catalyst is anhydrous magnesium chloride, anhydrous aluminum trichloride or anhydrous titanium tetrachloride;

[0035] 2) Switch the system to a phosphorus oxychloride distillation device equipped with a p...

Embodiment 1

[0045] 1) Put 6060 kg (39.48 kilomoles) of phosphorus oxychloride into a 6300L reaction kettle equipped with bisphenol A solid twin-screw feeder, phosphorus oxychloride reflux and vacuum distillation device, and hydrogen chloride gas absorption device, and add catalyst anhydrous Magnesium chloride 20 kg, heat up to 97°C, use a twin-screw feeder to continuously add 1425 kg (6.25 kilomoles) of bisphenol A, which accounts for 95% of the total bisphenol A, and add it in about 6 hours, then keep warm at 100-110°C for about 2 hours until the reaction is complete;

[0046] 2) Switch the system to a phosphorus oxychloride distillation device equipped with a phosphorus oxychloride distillation rate measuring device, and gradually increase the distillation temperature and vacuum degree. After about 5 hours, the temperature rises to about 135°C and the vacuum degree reaches 0.096Mpa. And when the phosphorus oxychloride distillation rate is less than 10ML / min, the phosphorus oxychloride d...

Embodiment 2

[0051] 1) Put 6060 kg (39.48 kilomoles) of phosphorus oxychloride into a 6300L reaction kettle equipped with bisphenol A solid twin-screw feeder, phosphorus oxychloride reflux and vacuum distillation device, and hydrogen chloride gas absorption device, and add catalyst anhydrous 20 kg of aluminum trichloride, heat up to 100°C, use a twin-screw feeder to continuously add 1350 kg (5.92 kilomoles) of bisphenol A, which accounts for 90% of the total bisphenol A feed, and add it in about 6 hours, and then add it at 100-110°C Keep warm for 2 hours until the reaction is complete;

[0052] 2) Switch the system to a phosphorus oxychloride distillation device equipped with a phosphorus oxychloride distillation rate measuring device, and gradually increase the distillation temperature and vacuum degree. After about 5 hours, the temperature rises to 140°C and the vacuum degree reaches 0.093Mpa, and When the phosphorus oxychloride distillation rate is less than 10ML / min, the phosphorus oxy...

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Abstract

The invention discloses an industrial preparation method of bisphenol A bis(diphenyl phosphate) with low triphenyl phosphate content. BDP is short for bisphenol A bis(diphenyl phosphate). The industrial preparation method comprises the following steps: firstly, reacting part of bisphenol A and excessive phosphoryl chloride in the existence of a catalyst to generate a bisphenol A phosphoryl chloride polycondensate containing excessive phosphoryl chloride; removing phosphoryl chloride through vacuum distillation; then, adding the left bisphenol A into the bisphenol A phosphoryl chloride polycondensate containing a small quantity of phosphoryl chloride; and reacting the obtained bisphenol A phosphoryl chloride polycondensate containing a trace amount of phosphoryl chloride and phenol to prepare a crude product of BDP, dissolving the crude product of BDP into a solvent, carrying out acid pickling, alkaline pickling and washing, and then, carrying out reduced-pressure distillation to obtain the BDP product. According to the industrial preparation method, the bisphenol A bis(diphenyl phosphate) with low triphenyl phosphate content is obtained by blowing down the residual phosphoryl chloride by creatively utilizing vacuum under the assistance of hydrogen chloride gas generated by a reactant on the premise that the equipment is not additionally arranged or changed.

Description

technical field [0001] The present invention relates to a kind of industrial preparation method of bisphenol A phenylphosphorus polycondensate, more specifically relates to a kind of bisphenol A phenylphosphorus polycondensate BDP with low content of triphenyl phosphate The industrial preparation method, the product is an excellent flame retardant for various engineering plastics. Background technique [0002] The use of flame-retardant materials such as flame-retardant plastics to improve the fire safety of products is receiving more and more attention and attention in various sectors of the national economy. Various application fields of engineering plastics have put forward more and more stringent requirements on the flame retardancy of materials, especially in the electronic information industry. In recent years, the application industry of flame-retardant engineering plastics is expanding day by day. Among the five major engineering plastics, flame-retardant modificati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12
Inventor 金译平周奋沈高波
Owner ZHEJIANG WANSHENG
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