Preparation method of ammonium polyphosphate flame retardation material

A technology of ammonium polyphosphate and flame retardant materials, applied in the field of flame retardants, which can solve the problems of high hygroscopicity and low degree of polymerization, and achieve the effects of easy separation, high degree of polymerization, and easy regulation

Inactive Publication Date: 2018-07-20
山东永浩新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The disadvantage of the existing ammonium polyphosphate products is that the degree of polymerization is small, resulting in high hygroscopicity, which leads to the easy precipitation and degradation of flame retardants in the corresponding materials. Therefore, it is necessary to develop an ammonium polyphosphate with a higher degree of polymerization products, which is conducive to improving the service life of flame retardant materials and ensuring the life of their flame retardant properties

Method used

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  • Preparation method of ammonium polyphosphate flame retardation material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1. Resin supported catalyst

[0017] In parts by weight, 1000 g of flake-shaped porous polyimide resin, 0.5 g of 1-n-butyl-3-methylimidazolium hexafluorophosphate, (2-carboxyethyl) triphenyltribromo Phosphine 5g, 2,2-bis(4-carboxyphenyl)hexafluoropropane 100g, 2,2'-bipyridine-4,4'-dicarboxylic acid 25g, europium trifluoroacetate 35g, heat up to 85°C, mix 5h, the resin catalyst product was obtained.

[0018] 2. Melt Polymerized Ammonium Polyphosphate

[0019] In parts by weight, add 10Kg of diammonium hydrogen phosphate, 9Kg of phosphorus pentoxide, 2.25Kg of urea, 0.2Kg of type II ammonium polyphosphate, and 0.3Kg of resin catalyst into the reactor, heat up to 200°C, and react for 4 hours. The resin catalyst is separated, and the product is filtered, washed, dried and pulverized to obtain the ammonium polyphosphate flame retardant material.

Embodiment 2

[0021] 1. Resin supported catalyst

[0022] In parts by weight, 1000 g of flake-shaped porous polyimide resin, 0.1 g of 1-n-butyl-3-methylimidazolium hexafluorophosphate, (2-carboxyethyl) triphenyltribromo Phosphine 1g, 2,2-bis(4-carboxyphenyl)hexafluoropropane 50g, 2,2'-bipyridine-4,4'-dicarboxylic acid 10g, europium trifluoroacetate 20g, heat up to 75°C, mix 4h, the resin catalyst product was obtained.

[0023] 2. Melt Polymerized Ammonium Polyphosphate

[0024] In parts by weight, add 10Kg of diammonium hydrogen phosphate, 8Kg of phosphorus pentoxide, 1.5Kg of urea, 0.1Kg of type II ammonium polyphosphate, and 0.2Kg of resin catalyst into the reactor, heat up to 180°C, and react for 4 hours. The resin catalyst is separated, and the product is filtered, washed, dried and pulverized to obtain the ammonium polyphosphate flame retardant material.

Embodiment 3

[0026] 1. Resin supported catalyst

[0027] In parts by weight, 1000 g of flake-shaped porous polyimide resin, 1 g of 1-n-butyl-3-methylimidazolium hexafluorophosphate, (2-carboxyethyl) triphenyl tribromide Phosphine 10g, 2,2-bis(4-carboxyphenyl)hexafluoropropane 150g, 2,2'-bipyridine-4,4'-dicarboxylic acid 50g, europium trifluoroacetate 50g, heat up to 95°C, mix for 6h , to obtain the resin catalyst product.

[0028] 2. Melt Polymerized Ammonium Polyphosphate

[0029] In parts by weight, add 10Kg of diammonium hydrogen phosphate, 10Kg of phosphorus pentoxide, 3Kg of urea, 0.3Kg of type II ammonium polyphosphate, and 0.4Kg of resin catalyst into the reactor, heat up to 220°C, react for 6 hours, and separate after the reaction The resin catalyst is extracted, and the product is filtered, washed, dried, and pulverized to obtain ammonium polyphosphate flame-retardant material.

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Abstract

The invention relates to a preparation method of an ammonium polyphosphate flame retardation material. Catalytic resin and high polymerization degree ammonium polyphosphate are added to a raw material, and uniform heating and stable reacting are performed in the production process to produce the high polymerization degree ammonium polyphosphate product, so the long-term existence of the product asa fireproofing agent in application materials is benefited.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a method for preparing an ammonium polyphosphate flame retardant material. Background technique [0002] Ammonium polyphosphate is widely used in intumescent fire retardant coatings, polyethylene, polypropylene, polyurethane, epoxy resin, rubber products, fiberboard and dry powder fire extinguishing agent, etc. It is a safe and efficient phosphorus-based non-halogen smoke suppressant flame retardant. Ammonium polyphosphate has high flame retardancy, dimensional stability, hydrolysis resistance and heat resistance in rigid polyurethane foam. The generation of toxic and corrosive gases to rigid polyurethane foam is even comparable to that of unflammable similar materials. The production of carbon monoxide and hydrogen chloride is also much lower than that of halogenated polyurethane foam. [0003] CN106586997A discloses a method for preparing type II ammonium polyphosphate: by adding ammonia ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/32C01B25/40B01J31/06
CPCB01J31/06C01B25/405C08K3/32C08K2003/323
Inventor 王大可谷灿波
Owner 山东永浩新材料科技有限公司
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