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A method for synthesizing crystalline type II ammonium polyphosphate by polyphosphoric acid catalysis

A polyphosphoric acid catalysis method and polyphosphoric acid catalyst technology, applied in the direction of phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as easy moisture absorption, and achieve the effects of easy control of reaction conditions, improved efficiency, and stable crystal form

Active Publication Date: 2017-06-09
YUNNAN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But type I APP is prone to hygroscopic phenomenon

Method used

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  • A method for synthesizing crystalline type II ammonium polyphosphate by polyphosphoric acid catalysis
  • A method for synthesizing crystalline type II ammonium polyphosphate by polyphosphoric acid catalysis

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0020] Example 1: Using industrial-grade phosphorus pentoxide as raw material, add monoammonium phosphate and melamine for mixing. The mass ratio of industrial-grade phosphorus pentoxide, monoammonium phosphate, and melamine is 1:1:0.2, and mix the three evenly Then add to the polymerization reactor for mixing. Add reaction catalyst polyphosphoric acid in the polymerization reactor simultaneously, concentration is 110%. The mass ratio of polyphosphoric acid to the mixture in the reactor is 0.3:1. Feed the mixed gas of ammonia and nitrogen into the polymerization reactor, maintain the pressure in the reactor at 0.2-0.3 MPa, raise the temperature of the reactor to 300°C, and keep the partial pressure of the mixed gas to react for 3 hours. After the reaction is finished, cool, discharge, and crush to obtain crystalline type II ammonium polyphosphate product. During the whole reaction process, the partial pressure of ammonia was maintained at 0.2-0.3 MPa, and the flow rate was 1...

Embodiment 2

[0021] Example 2: Using industrial-grade phosphorus pentoxide as raw material, add monoammonium phosphate and melamine for mixing. The mass ratio of industrial-grade phosphorus pentoxide, monoammonium phosphate, and melamine is 1:1.2:0.3, and mix the three evenly Then add to the polymerization reactor for mixing. Add reaction catalyst polyphosphoric acid in the polymerization reactor simultaneously, concentration is 95%. The mass ratio of polyphosphoric acid to the mixture in the reactor is 0.5:1. Feed the mixed gas of ammonia and nitrogen into the polymerization reactor, maintain the pressure in the reactor at 0.3-0.4 MPa, raise the temperature of the reactor to 320°C, and keep the partial pressure of the mixed gas to react for 2 hours. After the reaction is finished, cool, discharge, and crush to obtain crystalline type II ammonium polyphosphate product. During the whole reaction process, the partial pressure of ammonia was maintained at 0.3-0.4 MPa, and the flow rate was ...

Embodiment 3

[0022] Example 3: Using industrial-grade phosphorus pentoxide as a raw material, add monoammonium phosphate and melamine for mixing. The mass ratio of industrial-grade phosphorus pentoxide, monoammonium phosphate, and melamine is 1:1.5:0.5, and mix the three evenly Then add to the polymerization reactor for mixing. Add reaction catalyst polyphosphoric acid in the polymerization reactor simultaneously, concentration is 105%. The mass ratio of polyphosphoric acid to the mixture in the reactor is 0.35:1. Feed the mixed gas of ammonia and nitrogen into the polymerization reactor, maintain the pressure in the reactor at 0.15-0.2MPa, raise the temperature of the reactor to 340°C, and keep the partial pressure of the mixed gas to react for 4 hours. After the reaction is finished, cool, discharge, and crush to obtain crystalline type II ammonium polyphosphate product. During the whole reaction process, the partial pressure of ammonia was maintained at 0.15-0.2 MPa, and the flow rate...

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Abstract

The invention discloses a method for synthesizing crystalline type II ammonium polyphosphate by polyphosphoric acid catalysis. In this method, polyphosphoric acid is used as a reaction catalyst and phosphorus pentoxide is used as a raw material to obtain crystalline type II ammonium polyphosphate with stable crystal form through one-step reaction. Mix phosphorus pentoxide, monoammonium phosphate and melamine, mix them evenly and put them into the polymerization reactor, and add the reaction catalyst polyphosphoric acid at the same time, and complete the process at 240℃~350℃, 0.15~0.4MPa ammonia and nitrogen mixed atmosphere pressure reaction to obtain crystalline type II ammonium polyphosphate product. The reaction equipment adopted in the one-step preparation method of the present invention is a continuous reaction device with strong crushing effect and sealing and pressure bearing effect. The invention has the advantages of easy operation and short total reaction time.

Description

technical field [0001] The invention discloses a method for synthesizing crystalline type II ammonium polyphosphate by polyphosphoric acid catalysis, and in particular relates to a method for synthesizing a phosphorus-based flame retardant. It belongs to the field of inorganic phosphorus chemical industry. 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 flame-retardant application properties. [0003] Type I and T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/40
Inventor 古思廉刘晨曦李云东马航
Owner YUNNAN CHEM RES INST
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