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A kind of preparation method of segmental synthesis crystal II type ammonium polyphosphate

A ammonium polyphosphate, segmented synthesis technology, applied in the direction of phosphate, phosphorus oxyacid, etc., can solve the problems of limitation, lower decorative performance, lower flame retardant performance, etc., achieve short reaction time, stable product quality, and improve efficiency Effect

Active Publication Date: 2017-08-01
YUNNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of this, Type I APP is mostly used for flame retardancy of paper and fabrics, and is greatly limited in other aspects.
For flame retardants used as resins and molding substances, due to the high hygroscopicity and hydrolysis of Type I APP, ammonium polyphosphate with a low degree of polymerization dialysis to the surface, which not only reduces the decorative performance of the product, but also reduces the product's durability. Flame retardant properties

Method used

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  • A kind of preparation method of segmental synthesis crystal II type ammonium polyphosphate

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Experimental program
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Effect test

Embodiment 1

[0022] 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 280℃~290℃ Under the temperature, keep the partial pressure of ammonia to react for 30 minutes to complete a stage of reaction.

[0023] After the above-mentioned first-stage reaction is completed, the first-stage reaction product is mixed with industrial-grade phosphorus pentoxide and ammonium dihydrogen phosphate, and the mass ratio of the three is 1:0.5:0.5. After the three are mixed evenly, they are added to a pressure polymerization kettle for two-stage reaction. The temperature of the reaction kettle is raised to 260°C, and the partial pressure of ammonia is maintained for 3 hours to obtain a crystalline type II ammonium polyphosphate product.

[0024] The ammonia partial pressure was maintained at 0.1 MPa and the flow rate was 1.0 L / min througho...

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 1:0.5, mix the two evenly and put them into the polymerization reactor, at 220℃~230℃ Under the temperature, keep the partial pressure of ammonia to react for 120 minutes to complete a stage of reaction.

[0027] After the above-mentioned first-stage reaction is completed, the first-stage reaction product is mixed with industrial-grade phosphorus pentoxide and diammonium hydrogen phosphate, and the mass ratio of the three is 1:0.6:0.75. After the three are mixed evenly, they are added to a pressure polymerization kettle for two-stage reaction. The temperature of the reaction kettle is raised to 320°C, and the partial pressure of ammonia is maintained for 2 hours to obtain a crystalline type II ammonium polyphosphate product.

[0028] During the whole reaction process, the ammonia partial pressure was maintained at 0.07MPa, an...

Embodiment 3

[0030] Use industrial-grade phosphorus pentoxide as raw material, add urea for mixing, the mass ratio of industrial-grade phosphorus pentoxide and urea is 1:0.8, mix the two evenly and put them into the polymerization reactor, at 160℃~170℃ Under the temperature, keep the partial pressure of ammonia to react for 150 minutes to complete a stage of reaction.

[0031] After the above-mentioned first-stage reaction is completed, the first-stage reaction product is mixed with industrial-grade phosphorus pentoxide and ammonium dihydrogen phosphate, and the mass ratio of the three is 1:0.5:0.5. After the three are mixed evenly, they are added to a pressure polymerization kettle for two-stage reaction. The temperature of the reaction kettle is raised to 310°C, and the partial pressure of ammonia is maintained for 1.5 hours to obtain a crystalline type II ammonium polyphosphate product.

[0032] The ammonia partial pressure was maintained at 0.05MPa and the flow rate was 0.5L / min throug...

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Abstract

The present invention discloses a preparation method for sectional synthesis of crystal II type ammonium polyphosphate. According to the method, phosphorus pentoxide is adopted as a raw material and is subjected to a two-stage reaction to obtain the crystal II type ammonium polyphosphate with the stable crystal form, wherein in the first-stage reaction, a mixture comprising one or two selected from urea and melamine is added to phosphorus pentoxide, the raw materials are uniformly mixed and are subjected to reaction polymerization at a temperature of 160-330 DEG C in a polymerization reactor so as to complete the first-stage reaction, the first-stage reaction product, phosphorus pentoxide and ammonium phosphate selected from ammonium dihydrogen phosphate and diammonium hydrogen phosphate are mixed, the second-stage reaction at a temperature of 260-350 DEG C is performed in a pressure polymerization kettle after the three materials are uniformly mixed, and cooling, material discharge and crushing are sequentially performed to obtain the crystal II type ammonium polyphosphate product with the stable crystal form. Compared with other preparation method, the crystal II type ammonium polyphosphate synthesis method of the present invention has the following characteristic that: with the simple and easy-operation two-stage reaction, the crystal II type ammonium polyphosphate product with the stable crystal form can be synthesized in a short reaction time.

Description

technical field [0001] The invention relates to a preparation method for segmentally synthesizing crystalline type II ammonium polyphosphate. The method has low reaction temperature, easy operation, short total reaction time and stable crystal form of the obtained crystalline type II ammonium polyphosphate. Background technique [0002] Ammonium polyphosphate (hereinafter referred to as APP), as a halogen-free intumescent flame retardant, has been widely used in various fields of the flame retardant material industry for its non-toxic, tasteless, non-toxic gas, and excellent performance. application. There are currently six known crystal forms of APP, namely type I to type VI, but only type I, type II and type V are stable crystal forms. Among the currently known stable crystal forms of APP, since type II has better water resistance, heat resistance and stability than type I, it has wider applications and better performance in flame retardant applications. [0003] Current...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/28
Inventor 古思廉刘晨曦梁雪松李云东谌芳
Owner YUNNAN CHEM RES INST
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