Composite flame-retardant agent containing hydroxymethylation melamine phosphide as well as preparation method and application thereof

A technology of methylolated melamine and composite flame retardant, which is applied in the field of composite flame retardant containing methylolated melamine phosphide and its preparation, can solve the problems of poor compatibility, inability to meet the requirements for the use of polymer materials, easy Problems such as moisture absorption, to achieve good compatibility, less threat to life safety, and not easy to absorb moisture

Inactive Publication Date: 2011-02-16
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this type of flame retardant has a good flame retardant effect, because the phosphate-based P-N flame retardant is easy to absorb moisture, the compatibility with polymer materials is generally poor, and the salt structure it contains also makes This type of flame retardant cannot meet the requirements of some polymer materials

Method used

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  • Composite flame-retardant agent containing hydroxymethylation melamine phosphide as well as preparation method and application thereof
  • Composite flame-retardant agent containing hydroxymethylation melamine phosphide as well as preparation method and application thereof
  • Composite flame-retardant agent containing hydroxymethylation melamine phosphide as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Preparation of methylolated melamine phosphide:

[0028] (1) Mix 100 parts by weight of melamine with 100 parts by weight of 25% formaldehyde solution, adjust pH=9 with 4 parts by weight of triethylamine, and react for methylolation at 75°C for 20 minutes, and then rotary evaporation Removal of the remaining formaldehyde to obtain methylolated melamine;

[0029] (2) Adjust step (1) The pH of the reaction system is 4, and then add 100 parts by weight of diethyl phosphite, 200 parts by weight of absolute ethanol, and 1000 parts by weight of water, adjust the temperature to 80°C, and react for 2 hours Afterwards, the precipitate is filtered, washed with deionized water to pH=7, and dried to obtain a powdery methylolated melamine silicide.

[0030] Preparation of composite flame retardant containing methylolated melamine phosphide: 100 parts by weight of methylolated melamine phosphide prepared in this example, 3 parts by weight of zinc borate, and 2 parts by weight of antimony t...

Embodiment 2

[0033] Preparation of methylolated melamine phosphide:

[0034] (1) Mix 100 parts by weight of melamine with 400 parts by weight of 20% formaldehyde solution, 0.2 parts by weight of triethylamine to adjust pH=7.5, at 85°C, methylolation reaction for 30 minutes, and then rotary evaporation to remove the remaining Formaldehyde to obtain hydroxylated melamine;

[0035] (2) Adjust step (1) pH of the reaction system = 3.8, then add 200 weight phosphoric acid and 100 weight parts of water to it, adjust the temperature to 75°C, after reacting for 5 hours, filter the precipitate, dry, and wash with deionized water Precipitate to pH=7, and dry the precipitate to obtain powdery methylolated melamine phosphide.

[0036] Preparation of composite flame retardant containing methylolated melamine phosphide: 100 parts by weight of methylolated melamine phosphide prepared in this example, 30 parts by weight of aluminum hydroxide, 40 parts by weight of antimony trioxide, 30 parts by weight Parts of ...

Embodiment 3

[0039] Preparation of methylolated melamine phosphide:

[0040] (1) Mix 100 parts by weight of melamine with 200 parts by weight of 37% formaldehyde solution, 1.8 parts by weight of triethylamine to adjust pH=8, at 60℃, methylolation reaction for 90 minutes, and then rotary evaporation to remove the remaining Of formaldehyde to obtain methylolated melamine;

[0041] (2) Adjust step (1) pH=4 of the reaction system, then add 50 parts by weight of diethyl phosphate, 200 parts by weight of absolute ethanol, and 500 parts by weight of water to it, adjust the temperature to 100°C, and react for 0.5 hours, The precipitate is filtered, dried, washed with deionized water to pH=7, and dried to obtain a powdery methylolated melamine phosphide.

[0042] Preparation of composite flame retardant containing methylolated melamine phosphide: 100 parts by weight of methylolated melamine phosphide prepared in this example, 30 parts by weight of magnesium hydroxide, 30 parts by weight of zinc borate an...

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Abstract

The invention relates to a composite flame-retardant agent containing hydroxymethylation melamine phosphide and application thereof. The composite flame-retardant agent is formed by compounding 10 parts by weight of hydroxymethylation melamine phosphide, 5-100 parts by weight of inorganic flame-retardant agent and 0-100 parts by weight of inorganic filler. The invention has simple process and easily-obtained raw materials and is suitable for being popularized and applied on large scale; the prepared composite flame-retardant agent has no halogen, releases fewer toxic substances during combustion, is environment-friendly and has smaller threat on the life safety of people; in addition, the composite flame-retardant agent has the advantages of high thermal stability, high limited oxygen index, strong flame retardance, low possibility of moisture absorption and better compatibility with polymer materials and can effectively improve the heat resistance and the flame retardance of vinyl chloride, epoxy resin, polypropylene, polyester and other high polymer materials. The developed composite flame-retardant agent successfully solves the problems of toxicity, no environment-friendly performance, poor flame retardance, high possibility of moisture absorption, incompatibility with the high polymer materials and the like of the traditional flame-retardant agent.

Description

Technical field [0001] The invention relates to the field of flame retardant materials, in particular to a composite flame retardant containing methylolated melamine phosphide, and a preparation method and application thereof. Background technique [0002] At present, flame retardants with better flame retardant effects include halogen-containing flame retardants, organic phosphorus flame retardants, etc. Among them, decabromodiphenyl ether and hexabromocyclododecane are more commonly used for halogen-containing flame retardants. However, after this type of flame retardant is added to polymer materials, it is easy to produce toxic gases and smoke during the combustion process and pollute the environment, causing "secondary disasters" and gradually restricting its use; phosphorous flame retardants are due to Low toxicity, anti-dripping, low smoke, high flame retardant efficiency, and gradually attracted attention, but organic phosphorus flame retardants tend to have low thermal st...

Claims

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Application Information

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IPC IPC(8): C08K5/521C08K3/34C08K3/26C08L27/06C08K3/22C08L67/00C08K5/524C07F9/6521C08K3/38C08L23/12C08L63/00
Inventor 刘伟区魏振杰
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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