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Preparation method of triphenyl phosphate

A technology of triphenyl phosphate and acid value, which is applied in the chemical industry, can solve the problems of no patent publications, many reaction steps, environmental pollution, etc., and achieve the effects of short reaction time, simple conditions, and reduced production costs

Pending Publication Date: 2013-07-24
天津市联瑞阻燃材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are also many preparation methods of triphenyl phosphate in the prior art, and these methods also have their advantages respectively, but there are also many reaction steps, long routes, low efficiency, high energy consumption, corrosion equipment, and environmental problems in the preparation methods. Pollution etc.
[0007] Through the search, no patent publications related to this patent application were found

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Embodiment Construction

[0036] 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.

[0037] 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.

[0038] The preparation steps of the catalyst used in the present invention are as follows:

[0039] (1) Mix HZSM-5 type molecular sieve, calcium sulfate, magnesium chloride, turmeric powder and water to obtain a mixed solution;

[0040] 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;

[0041] (2) Under stirring conditions, heat to 80±5°C and react for 6~8h;

[0042] (3) After the reactant in the step (2) is filtered and suction filtered, i...

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Abstract

The invention relates to a preparation method of triphenyl phosphate. The preparation method comprises the following steps of: (1), adding a catalyst into molten phenol, putting a mixture into a reaction kettle, stirring the mixture until the temperature is reduced to be below 50 DEG C, stopping stirring and mixing phosphorus oxychloride; (2), performing constant pressure acid drainage and negative pressure acid drainage under a stirring condition to ensure that an acid value is less than or equal to 6mg KOH / g, and neutralizing and exhausting to obtain qualified coarse ester; and (3) raising the temperature of the qualified coarse ester to perform pressure reduction, distillation and separation and collecting a finished product; performing alkali washing and water washing, sampling and analyzing the finished product to ensure that the acid value is less than or equal to 0.05mg KOH / g, dehydrating and purifying, and sampling and analyzing the finished product to ensure that the acid value is less than or equal to 0.05mg KOH / g; and filtering to obtain triphenyl phosphate. The preparation method is easy to operate, mild in condition, short in reaction time, low in energy consumption, low in corrosion, low in pollution, and high in yield, and the product is pure, and the yield is up to more than 88 percent.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to triphenyl phosphate, in particular to a preparation method of triphenyl phosphate. Background technique [0002] Triphenyl phosphate (TPP), the molecular formula is: (C 6 h 5 O) 3 PO or C 18 h 15 o 4 P, CAS: 115-86-6, molecular weight 326.29, structural formula as follows: [0003] [0004] Triphenyl phosphate is white or slightly colored flake or powder crystal; odorless, non-flammable, slightly deliquescent; melting point: 50-51 ° C, insoluble in water, soluble in benzene, chloroform, ether, ethanol, acetone and other organic solvents. [0005] Triphenyl phosphate is a flame-retardant auxiliary plasticizer for cellulose resin, vinyl resin, natural rubber, and synthetic rubber; it has low volatility, excellent transparency, flexibility, toughness, and certain flame retardancy; It is a plasticizer and physical plasticizer for nitrocellulose, cellulose acetate (film base),...

Claims

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Application Information

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IPC IPC(8): C07F9/12B01J29/40
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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