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Preparation method of ammonium polyphosphate having high polymerization degree

A technology of ammonium polyphosphate and high degree of polymerization, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as low degree of polymerization, temperature rise, and difficult temperature in the synthesis process, so as to achieve stable reaction and easy temperature control , The effect of increasing the degree of polymerization of the product

Active Publication Date: 2017-04-26
山东瑞兴阻燃科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, in the production of high-polymerization-degree ammonium polyphosphate at home and abroad, phosphorus pentoxide and diammonium hydrogen phosphate are used as the basic raw materials for synthesis. However, because the reaction is extremely violent with phosphoric acid and the temperature rises extremely rapidly, the synthesis process It is very difficult to control the temperature, which makes the overall degree of polymerization of the synthesized products low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Preparation of solid catalyst

[0022] In parts by weight, 100 parts of high-flow butyl agarose microspheres, 16 parts of 1-decyl-3-methylimidazole-p-toluenesulfonic acid, and 3 parts of 2-adamantanone-5-carboxylic acid were mixed at 30°C 2h, obtain solid catalyst;

[0023] (2) Synthesis reaction

[0024] By weight, 100 parts of diamine hydrogen phosphate and 110 parts of phosphorus pentoxide, 13 parts of melamine, 1 part of type II ammonium polyphosphate, 2 parts of solid catalyst, react in an ammonia atmosphere, the temperature is 290 ° C, and the reaction is 2h. Filtration, washing, drying, and crushing to obtain Type II ammonium polyphosphate flame retardant. Product number M-1.

Embodiment 2

[0026] (1) Preparation of solid catalyst

[0027] In parts by weight, 100 parts of high-flow butyl agarose microspheres, 10 parts of 1-decyl-3-methylimidazole-p-toluenesulfonic acid, and 1 part of 2-adamantanone-5-carboxylic acid were mixed at 20°C 5h, obtain solid catalyst;

[0028] (2) Synthesis reaction

[0029] In parts by weight, 100 parts of diamine hydrogen phosphate and 70 parts of phosphorus pentoxide, 10 parts of melamine, 0.5 part of type II ammonium polyphosphate, and 1 part of solid catalyst are reacted in an ammonia atmosphere at a temperature of 250 ° C for 5 hours. Filtration, washing, drying, and crushing to obtain Type II ammonium polyphosphate flame retardant. Product number M-2.

Embodiment 3

[0031] (1) Preparation of solid catalyst

[0032] In parts by weight, 100 parts of high-flow butyl agarose microspheres, 30 parts of 1-decyl-3-methylimidazole p-toluenesulfonic acid, 5 parts of 2-adamantanone-5-carboxylic acid, mixed at 50 ° C 5h, obtain solid catalyst;

[0033] (2) Synthesis reaction

[0034] By weight, 100 parts of diamine hydrogen phosphate and 130 parts of phosphorus pentoxide, 20 parts of melamine, 2 parts of type II ammonium polyphosphate, 5 parts of solid catalyst, react in an ammonia atmosphere, the temperature is 320 ° C, and the reaction is 1h. Filtration, washing, drying, and crushing to obtain Type II ammonium polyphosphate flame retardant.

[0035] Product number M-3.

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PUM

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Abstract

The invention provides a preparation method of ammonium polyphosphate having high polymerization degree. II type ammonium polyphosphate is added and acts as a seed crystal and a solid catalyst is added, so that a polymerization reaction of II type ammonium polyphosphate is more uniform and is stable, the temperature in a synthetic process is easy to control, and the polymerization degree of a synthetized product is improved.

Description

technical field [0001] The invention relates to a method for preparing ammonium polyphosphate, in particular to a method for preparing ammonium polyphosphate with a high degree of polymerization. Background technique [0002] Type I and Type II are widely used in ammonium polyphosphate products at present. There are three main synthesis methods for crystalline type II ammonium polyphosphate. One is the technical route of phosphorus pentoxide, which uses phosphorus pentoxide and diammonium hydrogen phosphate as raw materials, and at the same time adds urea, melamine, ammonium sulfate, etc. as condensation agents. Under the ammonia atmosphere, the crystalline type II ammonium polyphosphate is produced by reaction in a kneader; the other is to use diammonium hydrogen phosphate as the main raw material, add a specific condensing agent, and synthesize the crystal II polyphosphate through the control of the ammonia atmosphere. Type I ammonium polyphosphate; there is also a crysta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/40
CPCC01B25/405
Inventor 王荣军吴健泳
Owner 山东瑞兴阻燃科技有限公司
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