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Method for preparing polyimide intercalated grafted magnesium hydroxide flame retardant

A technology of magnesium hydroxide and polyimide, applied in the direction of fire-resistant coatings, etc., can solve the problems of great influence on physical-mechanical properties and processing properties, large specific surface area, low tensile strength and limiting oxygen index, etc., to achieve flame retardancy The effect is remarkable, the preparation process is simple, and the effect of good application prospect

Inactive Publication Date: 2010-07-28
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, magnesium hydroxide also has the following disadvantages: (1) The high addition amount has a great influence on the physical-mechanical properties and processing properties of the material
(2) Ordinary magnesium hydroxide is mostly hexagonal crystal or amorphous crystal, with large specific surface area, strong agglomeration between crystal grains, and poor dispersion in resin, so it is difficult to be compatible with plastics. The fuel needs special treatment to make it have a special structure
[0008] The disadvantage of this method is: low tensile strength and limiting oxygen index
[0012] (2) As the amount of stearic acid (SA) surface modifier increases, the flame retardant performance of the magnesium hydroxide-EVA flame retardant system gradually deteriorates: the oxygen index decreases; the horizontal combustion and vertical combustion become worse
[0015] The disadvantage of this method is: low tensile strength and limiting oxygen index

Method used

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  • Method for preparing polyimide intercalated grafted magnesium hydroxide flame retardant
  • Method for preparing polyimide intercalated grafted magnesium hydroxide flame retardant
  • Method for preparing polyimide intercalated grafted magnesium hydroxide flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] 2.0 g (0.01 mol) of 4,4'-diaminodiphenyl ether aromatic dibasic primary amine, 1.2 g of aminopropyltrimethoxysilane (KH-550) amino-terminated coupling agent and 1000 ml of N, N-dimethylacetamide mixed with a strong polar aprotic organic solvent, stirred evenly at room temperature, added 100.0 grams of magnesium hydroxide powder, and dispersed by high-speed emulsification machine (6000-10000r / min) for 20min-30min, added 2.18 grams (0.01 moles) of pyromellitic dianhydride powder, stirred and reacted at room temperature for 1-2 hours, added 0.1 grams of toluenesulfonic acid catalyst and 20 ml of toluene aromatic hydrocarbon solvent, heated and refluxed for 6-8 hours after water separation , separate toluene and 20%~40%vol. (relative to the volume of the original strong polar aprotic organic solvent) N, N-dimethylacetamide solvent, cooling, standing, filtering, drying, to obtain 102.9 grams of poly Imide intercalation grafted magnesium hydroxide flame retardant powder.

[...

Embodiment 2

[0046] 21.62 grams (0.1 mole) of 3,3'-diamino-4,4'-dihydroxybiphenyl aromatic dibasic primary amine, the amino terminal group coupling agent of 1.81 gram end aminopropyltriethoxysilane and Mix 4,300 ml of N-methyl-2-pyrrolidone with a strong polar aprotic organic solvent, stir evenly at room temperature, add 216.2 g of magnesium hydroxide powder, and use a high-speed emulsifier (6000-10000r / min) for high-speed shear dispersion for 20min- 30min, add 32.34 grams (0.11 mole) 3,3',4,4'-tetracarboxylic acid biphenyl dianhydride powder, stir and react at room temperature for 1-2 hours, add 2.16 grams of toluenesulfonic acid catalyst and 430 milliliters of xylene Aromatic hydrocarbon solvent, after heating and reflux for water separation for 6-8 hours, separate xylene and 20% to 40% vol. of N-methyl-2-pyrrolidone solvent, cool, stand still, filter, and dry to obtain 266.2 grams Polyimide intercalation grafted magnesium hydroxide flame retardant powder.

[0047] 57.0 grams of the obt...

Embodiment 3

[0050] 2.0 grams (0.01 moles) of 4,4'-diaminodiphenyl ether and 2.48 grams (0.01 moles) of 4,4'-diaminodiphenylsulfone aromatic dibasic primary amines, 1.8 grams of terminal aminopropyl trimethoxy base silane (KH-550) amino terminal coupling agent and 2700 milliliters of N, N-dimethylacetamide strong polar aprotic organic solvent, stir well at room temperature, add 180.0 grams of magnesium hydroxide powder, and use high-speed Emulsifier (6000-10000r / min) high-speed shear dispersion for 20min-30min, add 2.18g (0.01mol) of pyromellitic dianhydride powder and 2.94g (0.01mol) of 3,3',4,4'-tetracarboxylic acid Biphenyl dianhydride powder, stirred and reacted at room temperature for 1-2 hours, added 0.31 g of toluenesulfonic acid catalyst, 20 ml of toluene and 50 ml of xylene aromatic hydrocarbon solvent, heated and refluxed for 6-8 hours, separated Toluene and 20% to 40% vol. of N, N-dimethylacetamide solvent, cooling, standing, filtering, and drying to obtain 188.5 grams of polyim...

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Abstract

The invention relates to a method for preparing polyimide intercalated grafted magnesium hydroxide flame retardant. The method comprises: mixing binary primary amine, amino end-group coupling agent and strong polar non-proton organic solvent; uniformly stirring the mixture at room temperature; adding magnesium hydroxide powder; performing high-speed shearing dispersion for 20 to 30 minutes; adding aromatic dianhydride powder, catalysts and aromatic hydrocarbon solvent; performing water-separating reaction for 6 to 8 hours; and separating out aromatic solvent and part of strong polar non-proton organic solvent to obtain the polyimide intercalated grafted magnesium hydroxide flame retardant. The polyimide intercalated grafted magnesium hydroxide flame retardant has the vertical combustion level at V-0, limiting oxygen index up to 32, tensile strength up to over 13.6 MPa, significant flame retardant effect and good application prospects. In addition, the method has the advantages of simple preparation process, low cost, convenient operation, friendliness to environment, capability of completing preparation in general equipment and help to industrial production.

Description

technical field [0001] The invention belongs to the field of non-halogen smoke suppressing flame retardant polymer materials, in particular to a preparation method of a polyimide intercalation grafted magnesium hydroxide flame retardant. Background technique [0002] With the rapid development of plastic industry, wire and cable, printed circuit board, automobile, aerospace, textile and clothing, decorative fabrics, etc., there is a demand for flame retardants, especially for non-toxic and smoke-suppressing inorganic flame retardants. will be more urgent. [0003] Due to the low toxicity of inorganic flame retardants, it is fully in line with the current general trend of flame retardants to be environmentally friendly. However, since inorganic flame retardants (such as aluminum hydroxide, magnesium hydroxide, zinc borate, etc.) are fillers, they are added in a large amount in the resin, which often affects the processing performance and mechanical properties of the material...

Claims

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Application Information

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IPC IPC(8): C09K21/14C08G73/10C08L79/08C08L23/08C08L31/04C08L23/06C08L23/12C08L77/00C08L63/00
Inventor 虞鑫海李四新
Owner DONGHUA UNIV
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