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Branched modifier and corresponding flame retardant nylon resin

A flame retardant nylon and modifier technology, applied in the field of nylon resin, can solve the problems of poor high temperature resistance, affecting the application range, easy decomposition, etc., and achieve fast reaction rate, high melt fluidity, and high flame retardant efficiency Effect

Active Publication Date: 2015-11-04
ZHUZHOU TIMES NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the Chinese patent CN1266445A, CEPPA is used as a reactive flame retardant to prepare a reactive flame retardant nylon 66 resin. This resin has the characteristics of halogen-free flame retardant and no flame retardant precipitation. However, when this flame retardant nylon resin burns It will drip, and at the same time, the high temperature resistance is poor, and it is easy to decompose at high temperature, which will affect the application range

Method used

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  • Branched modifier and corresponding flame retardant nylon resin
  • Branched modifier and corresponding flame retardant nylon resin
  • Branched modifier and corresponding flame retardant nylon resin

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0039] Preparation method of carboxyl-terminated ring triphosphazene branched modifier

[0040] Taking six (4-carboxyphenoxy) cyclotriphosphazene as an example, its synthesis steps are as follows:

[0041] Equipped with a magnet, a thermometer, a constant pressure dropping funnel, a condensing reflux tube and N 2In the 1L three-neck flask of the protection device, add 125g of p-hydroxybenzaldehyde, 140g of anhydrous potassium carbonate and 500ml of tetrahydrofuran in sequence, stir at room temperature to dissolve it; weigh 50g of hexachlorocyclotriphosphazene and dissolve it in 100ml of tetrahydrofuran, and slowly Add it dropwise to the above reaction system, and reflux at 65°C for 24h after the dropwise addition. Filtrate, concentrate the filtrate, pour it into deionized water to produce a white precipitate, the precipitate obtained is washed twice with deionized water, recrystallized in ethyl acetate, and vacuum-dried at room temperature for 24h, the intermediate product he...

preparation example 2

[0045] Preparation method of amino-terminated cyclotriphosphazene branched modifier

[0046] Taking six (4-aminophenoxy) cyclotriphosphazene as an example, its synthesis steps are as follows:

[0047] Equipped with a magnet, thermometer, constant pressure dropping funnel, condensing return tube and N 2 In the 500ml there-necked flask of protection device, add 20g hexachlorocyclotriphosphazene, 58g p-nitrophenol, 58g potassium carbonate and 250ml tetrahydrofuran successively; 2 Heated and stirred under protection, and refluxed at 65°C for 24h. The reacted mixture was filtered while it was hot, and the filter residue was washed with ice water, acetone, methanol and diethyl ether in sequence, and finally the solid was put into a vacuum drying oven and dried at room temperature for 24 hours to obtain a white powder as the intermediate product hexa(4-nitrophenoxy ) cyclotriphosphazene with a yield of 84.7%.

[0048] Weigh 10g of hexa(4-nitrophenoxy)cyclotriphosphazene, 60g of st...

Embodiment

[0051] Embodiment 1-6 and comparative example 1-4 all prepare nylon resin by raw material and consumption shown in table 1, wherein comparative example 1 and 2 do not use reactive flame retardant and branched modifier, comparative example 3 does not use branched Chemical modifier, comparative example 4 did not use reactive flame retardant. The specific preparation method is as follows:

[0052] (1) According to the ratio shown in Table 1, first salt the reactive flame retardant with diamine or dicarboxylic acid in water, and then mix the obtained salt solution with nylon polymer monomer and branched modifier evenly .

[0053] (2) Put the prepared materials into the high-pressure reaction kettle, close the feeding cover tightly, and connect the condensed water; fill the high-purity nitrogen until the pressure in the kettle is 0.2-0.5MPa, and slowly open the exhaust valve to vacuum to make the pressure in the kettle Reduce to -0.03 to -0.05MPa, repeat this operation 3 times, a...

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Abstract

The invention discloses a branched modifier having the structure shown in the formula (VII), wherein R2-R7 are the same or different and are independently hydrocarbonyl or substituted hydrocarbonyl containing 1-20 carbon atoms, the substituted hydrocarbonyl is hydrocarbonyl containing terminated carboxyl or terminated amino, and at least one of R2-R7 is substituted hydrocarbonyl containing terminated carboxyl or terminated amino. The invention also provides a flame retardant nylon resin, a reactive flame retardant and diamine or dicarboxylic acid form a salt with equal mole ratio, the obtained salt solution is mixed with a nylon polymeric monomer and the branched modifier, and then a polycondensation reaction is carried out to obtain the flame retardant nylon resin. The flame retardant nylon resin has the characteristics of no halogen, environmental protection, no dripping during combustion, high flame retardant efficiency, high flame retardant grade, permanent flame retardancy and no migration.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a branched modifier and a nylon resin using the branched modifier. Background technique [0002] Nylon is widely used in the fields of automobiles, electronic appliances, mechanical equipment, national defense and military industry due to its good mechanical properties, heat and weather resistance and electrical insulation properties. However, due to the low oxygen index, fast burning speed, and high heat release of nylon materials, especially during the combustion process, a large amount of smoke and molten droplets are generated, which can easily spread flames and endanger the safety of life and property, which greatly limits its application range. . Therefore, it is imminent to improve the flame retardancy of nylon materials. [0003] In order to improve the flame retardant performance of nylon, it is mainly achieved by physical blending in industry. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/42C07F9/6593
Inventor 胡天辉王春花杨克俭汤鑫焱王文志曹凯凯邓凯恒姜其斌
Owner ZHUZHOU TIMES NEW MATERIALS TECH
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