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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 problem of easy moisture absorption, poor compatibility and unsatisfactory polymer materials. Use requirements and other issues to achieve the effect of good compatibility, high thermal stability, and less threat to life safety

Inactive Publication Date: 2012-02-29
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
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of hydroxymethylated melamine phosphides:

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

[0029] (2) Adjust the pH value of the reaction system in step (1) to 4, 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 Finally, filter the precipitate, wash the precipitate with deionized water until pH = 7, and dry the precipitate to obtain a powdery methylolated melamine silicide.

[0030] Preparation of a composite flame retardant containing methylolated melamine phosphide: take 100 parts by weight of the methylolated melamine phosphide prepared in this example, 3 parts...

Embodiment 2

[0033] Preparation of hydroxymethylated melamine phosphides:

[0034] (1) 100 parts by weight of melamine and 400 parts by weight of 20% formaldehyde solution are mixed, 0.2 parts by weight of triethylamine is adjusted to pH=7.5, and at 85° C., the methylolation reaction is carried out for 30 minutes, and then rotary evaporation removes the remaining formaldehyde to obtain hydroxylated melamine;

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

[0036] Preparation of a composite flame retardant containing methylolated melamine phosphide: take 100 parts by weight of the methylolated melamine phosphide prepared in this example, 30 parts by weight of aluminum hydroxide, 40 p...

Embodiment 3

[0039] Preparation of hydroxymethylated melamine phosphides:

[0040] (1) 100 parts by weight of melamine and 200 parts by weight of 37% formaldehyde solution are mixed, 1.8 parts by weight of triethylamine is adjusted to pH=8, at 60°C, the methylolation reaction is carried out for 90 minutes, and then rotary evaporation removes the remaining formaldehyde to obtain methylolated melamine;

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

[0042] Preparation of a composite flame retardant containing methylolated melamine phosphide: take 100 parts by weight of the methylolated melamine phosphide prepared in this example, 30 pa...

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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 its preparation method and application. Background technique [0002] At present, flame retardants with better flame retardant effects include halogen-containing flame retardants, organophosphorus flame retardants, etc. Among them, decabromodiphenyl ether, hexabromocyclododecane, etc. etc., but after this kind of flame retardant is added to polymer materials, it is easy to produce toxic gas and smoke during the combustion process and pollute the environment, causing "secondary disasters", which gradually restricts its use; phosphorus flame retardants are due to Low toxicity, anti-dripping, low smoke, and high flame retardant efficiency have gradually attracted attention. However, organophosphorus flame retardants often have low thermal stability and are easy to hydrolyze, which limits their applica...

Claims

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Application Information

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