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Preparation method of bisphenol A bis(diphenyl phosphate)

A technology of diphenyl phosphate and bisphenol, which is applied in the preparation of bisphenol A bis(diphenyl phosphate) and the field of bisphenol A bis(diphenyl phosphate), can solve the problem that the preparation method has many reaction steps, Production environment pollution, corrosion of equipment and other problems, to achieve the effect of short reaction time, increase economic benefits, and reduce waste water

Pending Publication Date: 2013-07-24
天津市联瑞阻燃材料有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0007] At present, there are also many preparation methods of bisphenol A bis(diphenyl phosphate) in the prior art, and these methods also have their advantages respectively, but there are also many reaction steps, long routes, low efficiency, and energy in the preparation methods. Defects such as high consumption, corrosion of equipment, and great pollution to the production environment

Method used

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  • Preparation method of bisphenol A bis(diphenyl phosphate)

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Embodiment Construction

[0044] The present invention will be further described in detail below through the specific examples, the following examples are only descriptive, not restrictive, and cannot limit the protection scope of the present invention with this.

[0045] The reagents used in the present invention, unless otherwise specified, are commercially available conventional reagents; the methods used, unless otherwise specified, are conventional methods in the art.

[0046] The main raw material that the present invention uses:

[0047] BPA, phenol, phosphorus oxychloride, catalyst

[0048] The preparation steps of the catalyst used in the present invention are as follows:

[0049] (1) Mix HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, turmeric powder and water to obtain a mixed solution;

[0050] The mass ratio of HZSM-5 molecular sieve, calcium sulfate, magnesium chloride and sage powder to each 1L of mixed solution is 10:2.9:2.5:1;

[0051] (2) Under stirring conditions...

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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) mixing phosphorus oxychloride and a catalyst, heating to 80 DEG C, and mixing bisphenol A; (2) heating to 105 DEG C at the speed of 4 DEG C / h, and balancing the temperature for 2h, then evaporating excessive phosphorus oxychloride, controlling the temperature not to be higher than 120 DEG C, and cooling to 73-78 DEG C after evaporation; (3) adding molten phenol, heating to react, balancing the temperature of 95 DEG C for 1.5h, the temperature of 115 DEG C for 1h and the temperature of 135 DEG C for 1, finally uniformly and stably heating to 155 DEG C until no acidic gas appears, and ending the reaction to obtain raw ester; (4) subjecting the raw ester to purification, polarization, alkali neutralization, washing and impurity removal to obtain wet raw ester; and (5) carrying out reduced pressure distillation on the wet raw ester, sampling and analyzing an acid value to be smaller than or equal to 0.15mgKOH / g, and filtering the wet raw ester to obtain the bisphenol A bis(diphenyl phosphate). The preparation method provided by the invention is simple in operation, simple and convenient in condition, short in reaction time, low in energy consumption, little in corrosion and pollution, high in purity of products and high in yield higher than 88%.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to bisphenol A bis(diphenyl phosphate), especially a preparation method of bisphenol A bis(diphenyl phosphate). Background technique [0002] Bisphenol A bis (diphenyl phosphate), referred to as BDP, also known as oligomeric phosphate flame retardant BDP, the English name is Oligomeric Resorcinol Bis, molecular formula: C 39 h 34 o 8 P 2 ;CAS 125997-79-5 [0003] Its structural formula is as follows: [0004] [0005] Bisphenol A bis (diphenyl phosphate) is a colorless or light yellow viscous liquid. It is an oligomeric aromatic phosphate flame retardant. It has excellent flame retardant effect and is insoluble in water. It is compatible with toluene and methyl ethyl ketone. Miscible; density about 1.3, low toxicity, good thermal stability, low volatility, no migration, strong hydrolysis resistance. [0006] Bisphenol A bis (diphenyl phosphate) is a high molecular weight phos...

Claims

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Application Information

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IPC IPC(8): C07F9/12
Inventor 张云刚张传义赵春忠刘雪坤
Owner 天津市联瑞阻燃材料有限公司
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