Two-stage type production method of V crystal form type APP (ammonium polyphosphate)

A technology of ammonium polyphosphate and its production method, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as ineffective application in industrial production, and achieve the effects of improving the production environment, increasing efficiency, and stabilizing the crystal form

Active Publication Date: 2015-02-18
YUNNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The development and research of crystalline V-type ammonium polyphosphate began in the 1970s. In previous studies, the preparation conditions of crystalline V-type ammonium polyphosphate were only for laboratory research and could not be effectively applied to industrial production.

Method used

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  • Two-stage type production method of V crystal form type APP (ammonium polyphosphate)
  • Two-stage type production method of V crystal form type APP (ammonium polyphosphate)

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Use industrial-grade phosphorus pentoxide as raw material, add urea for mixing, the mass ratio of industrial-grade phosphorus pentoxide and urea is 1:0.3, mix the two evenly and put them into the polymerization reactor, at 220℃~240℃ After continuing to react at high temperature for 3 minutes, transfer the material into a pressure reactor with a stirring device, raise the temperature to 240°C, and react for 3 hours to obtain a crystalline V-type ammonium polyphosphate product. The ammonia partial pressure was maintained at 0.05MPa and the flow rate was 0.5L / min throughout the reaction process.

Embodiment 2

[0026] Use industrial-grade phosphorus pentoxide as raw material, add urea for mixing, the mass ratio of industrial-grade phosphorus pentoxide and urea is 1:0.4, mix the two evenly and put them into the polymerization reactor, at 160℃~180℃ After continuing to react at high temperature for 60 minutes, transfer the material into a pressure reactor with a stirring device, raise the temperature to 280°C, and react for 2 hours to obtain a crystalline V-type ammonium polyphosphate product. The ammonia partial pressure was maintained at 0.08MPa and the flow rate was 0.3L / min throughout the reaction process.

Embodiment 3

[0028] Use industrial-grade phosphorus pentoxide as raw material, add urea and melamine for mixing, the mass ratio of industrial-grade phosphorus pentoxide, urea and melamine is 1:0.4:0.05, mix the three evenly and add them to the polymerization reactor, After continuing to react at a temperature of 180°C to 200°C for 30 minutes, transfer the material into a pressure reactor with a stirring device, raise the temperature to 280°C, and react for 2 hours to obtain a crystalline V-type ammonium polyphosphate product. The ammonia partial pressure was maintained at 0.1 MPa and the flow rate was 0.2 L / min throughout the reaction process.

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Abstract

The invention relates to a production method of a chemical product, and discloses a two-stage type production method of V crystal form type APP (ammonium polyphosphate). The production method comprises steps as follows: phosphorus pentoxide is adopted as a raw material, and V crystal form type APP with a stable crystal form is obtained through two stages of reaction; and in the first-stage reaction, phosphorus pentoxide is added to one of urea and tripolycyanamide or a mixture of urea and tripolycyanamide, the raw materials are uniformly mixed, react at the temperature of 160-240 DEG C under the protection of ammonia atmosphere in a polymerization reactor and react and polymerize at the temperature of 240-330 DEG C in a pressure reaction kettle provided with a stirring device so as to obtain the V crystal form type APP product with the stable crystal form. According to the two-stage type technological process, emergent gas in a later reaction process is taken as protection gas of a former reaction system, and the production method has the advantages that the tail gas emission is reduced, the production environment is improved, and the cost is reduced.

Description

technical field [0001] The invention relates to a production method of chemical products, in particular to a two-stage production method for synthesizing crystalline V-type ammonium polyphosphate with a single crystal form with short reaction process and simple steps. Background technique [0002] Ammonium polyphosphate (referred to as APP) is an inorganic halogen-free and environmentally friendly flame retardant developed rapidly in recent decades. It has the advantages of good flame retardant effect, good thermal stability and environmental friendliness. One of the main components of IFR) is widely used in the field of flame retardant. [0003] Ammonium polyphosphate can be divided into crystalline form and amorphous form according to its structure. Crystalline ammonium polyphosphate is a water-insoluble long-chain polyphosphate. At present, there are six known crystal forms of ammonium polyphosphate, which are Ⅰ, Ⅱ, Ⅲ, Ⅳ, Ⅴ, and Ⅵ. Among them, the appearance of crystall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/40
Inventor 刘晨曦古思廉梁雪松李云东
Owner YUNNAN CHEM RES INST
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