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Method for preparing crystal II-type ammonium polyphosphate with distribution of high polymerization degree and narrow molecular weight

A technology with narrow molecular weight distribution and high degree of polymerization, which is applied in the field of preparation of crystalline type II ammonium polyphosphate, can solve the problem that the complete transformation of the material state in the kneader cannot be realized, the mixing, kneading, and crushing functions of the kneader are not strong enough, and no Measures to control the severity of the reaction and other issues, to achieve the effect of high purity of crystal type II, promotion of the formation of prepolymers, and high degree of polymerization

Active Publication Date: 2009-12-09
GUANGDONG JUSHI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The high degree of polymerization ammonium polyphosphate produced in the prior art is all synthesized with phosphorus pentoxide and diammonium hydrogen phosphate as raw materials, but because of process control and equipment design, the range of polymerization degree of the synthesized product is relatively wide, wherein Doped with a relatively large amount of low-molecular-weight ammonium polyphosphate; because no effective cooling measures were taken during the reaction process, the product was broken due to high temperature in the kneader, affecting the quality of the chain, and no measures were taken to control the intensity of the reaction; In addition, the mixing, kneading, and crushing functions of the kneader are not strong enough to realize the complete transformation of the state of the material in the kneader; at the same time, a large amount of excess ammonia will be generated during the synthesis process

Method used

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  • Method for preparing crystal II-type ammonium polyphosphate with distribution of high polymerization degree and narrow molecular weight
  • Method for preparing crystal II-type ammonium polyphosphate with distribution of high polymerization degree and narrow molecular weight

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Put 110Kg phosphorus pentoxide and 102Kg diammonium hydrogen phosphate into 0.5m 3 In the kneader, the flow rate is 8m 3 Preheat and mix at the same time under the protection of helium gas per hour; control the temperature rise rate of the material to 5°C / min, when the temperature of the material in the kneader rises to 200°C, stop the flow of helium and start the flow of ammonia. Flow control is 15m 3 / h, after the flow rate is maintained for 1.0h, the ammonia gas flow is stopped, the temperature is controlled at 220°C, the ammonia gas flow is resumed after the homogenization process is carried out for 1.0h, and the flow rate is controlled at 20m 3 / h; continue to heat up for 2 hours, when the temperature of the material rises to 300 ° C, put 3.18Kg of melamine cyanurate into the kneader, continue to keep stirring for 4 hours under the condition of ammonia gas; then transfer the material to a closed container, that is, through the feeding Transfer the material to the...

Embodiment 2

[0026] Put 130Kg phosphorus pentoxide and 121Kg diammonium hydrogen phosphate into 0.5m 3 In the kneader, at a flow rate of 2m 3 Carry out preheating and mixing under nitrogen protection at the same time; control the temperature rise rate of the material to 5°C / min, when the temperature of the material in the kneader rises to 150°C, stop the nitrogen flow and start the ammonia flow, the flow control of the ammonia gas 5m 3 / h, after the flow rate is maintained for 0.5h, the ammonia gas flow is stopped, the temperature is controlled at 150°C, the ammonia gas flow is resumed after the homogenization process is carried out for 0.5h, and the flow rate is controlled at 15m 3 / h; continue to heat up for 2h, when the temperature of the material rises to 250°C, put 3.765Kg of epoxy resin into the kneader, continue to keep stirring under the condition of ammonia for 1h; then transfer the material to a closed container, that is, through the feeding Transfer the material to the materia...

Embodiment 3

[0028] Put 150Kg phosphorus pentoxide and 139Kg diammonium hydrogen phosphate into 0.5m 3 In the kneader, at a flow rate of 10m 3 Preheat and mix at the same time under the protection of argon gas per hour; control the temperature rise rate of the material to 5°C / min, when the temperature of the material in the kneader rises to 250°C, stop the flow of argon and start the flow of ammonia, the ammonia gas Flow control is 20m 3 / h, after the flow rate is maintained for 3.0 hours, the ammonia gas flow is stopped, the temperature is controlled at 200°C, the ammonia gas flow is resumed after the homogenization process is carried out for 1.5 hours, and the flow rate is controlled at 25m 3 / h; continue to heat up for 2h, when the temperature of the material rises to 350°C, put 4.335Kg of aminosilane into the kneader, and continue to keep stirring under the condition of ammonia for 4h; then transfer the material to a closed container, that is, through the feeding port Transfer the ma...

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Abstract

The invention discloses a method for preparing crystal II-type ammonium polyphosphate with distribution of high polymerization degree and narrow molecular weight. The method comprises the following steps: putting phosphorus pentoxide and diammonium phosphate which have equal molar ratio into a malaxator which can accurately control a temperature and heated by conducting oil for mixing; under the protection of inert gas, heating the materials in the malaxator to between 100 and 250 DEG C through the circulatory conducting oil; stopping introducing the inert gas; performing ammonification on the materials and heating the materials under an atmosphere of ammonia gas till the materials are totally molten down; stopping introducing the ammonia gas; after homogenization, introducing the ammonia gas again and heating the materials; throwing a surface treating agent into the malaxator; after material throwing is completed, continuously introducing the ammonia gas, keeping warm and mixing the materials; after reaction is finished, transferring the materials to a closed vessel and reducing the temperature; simultaneously, continuously introducing the ammonia gas till the temperature of the materials is below 100 DEG C; and obtaining a finished product. The method can prepare the crystal II -type ammonium polyphosphate with the distribution of the high polymerization degree and the narrow molecular weight; and the product has the characteristics of uniform granularity shape, small water-solubility, good heat resistance, high polymerization degree, narrow distribution of molecular weight and high crystal II-type purity.

Description

technical field [0001] The invention belongs to the field of preparation methods of chemical raw materials, and discloses a preparation method of crystalline type II ammonium polyphosphate with high polymerization degree and narrow molecular weight distribution. Background technique [0002] Ammonium polyphosphate (APP) is a highly efficient and environmentally friendly flame retardant with high nitrogen and phosphorus content. It has a variety of crystal forms from I to V, among which type II ammonium polyphosphate has the best thermal stability and water resistance, so it is widely used in the flame retardant fields of high-grade refractory coatings, resins, rubber paper, wood, fibers, etc. , which has the characteristics of low toxicity, no dripping, low smoke, etc., and is a good substitute for halogen flame retardants. [0003] The high degree of polymerization ammonium polyphosphate produced in the prior art is all synthesized with phosphorus pentoxide and diammonium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/40
Inventor 谢思正
Owner GUANGDONG JUSHI CHEM CO LTD
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