Preparation method of flame retardant material

A technology of flame retardant materials and flame retardants, applied in the field of flame retardant materials, can solve the problems of poor hydrolysis resistance, poor high temperature resistance, low phosphorus content, etc., achieve excellent flame retardant performance, increase thermal degradation temperature, and high melting point Effect

Active Publication Date: 2019-12-13
SHANGHAI UNIV OF ENG SCI
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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of low phosphorus content, poor high temperature resistance, poor hydrolysis resistance, and low melting point of organic phosphorus-based additive flame retardants in the prior art, and provide a hydrolysis-resistant flame retardant with high phosphorus content. And the flame retardant material is made from it. The present invention obtains a high phosphorus content, high temperature resistance, hydrolysis resistance, and high melting point by transesterifying the hydroxylated DDP and the cage structure flame retardant PEPA with hydrolysis resistance. The organophosphorus-based additive flame retardant, and further prepared flame-retardant masterbatch and flame-retardant fiber with excellent flame-retardant effect

Method used

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  • Preparation method of flame retardant material
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  • Preparation method of flame retardant material

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Effect test

Embodiment 1

[0029] A high phosphorus content hydrolysis-resistant flame retardant, its preparation method is as follows:

[0030] (1) Preparation of hydroxylated DDP: DDP and ethylene glycol with a molar ratio of 1:2.50 are used as raw materials, and under the protection of nitrogen, esterification reaction is carried out, accompanied by vacuum distillation, to obtain hydroxylated DDP , wherein, the temperature of the esterification reaction is 160°C, the time is 3.5h, and the vacuum degree of the vacuum distillation is 5KPa;

[0031] (2) Preparation of high-phosphorus-content hydrolysis-resistant flame retardant: using hydroxylated DDP with a molar ratio of 1:2.00 and caged pentaerythritol phosphate as raw materials, under the protection of nitrogen, first carry out high-pressure transesterification reaction, and then carry out vacuum Transesterification reaction to produce a high phosphorus content hydrolysis-resistant flame retardant, wherein the temperature of the high-pressure transe...

Embodiment 2

[0036] A high phosphorus content hydrolysis-resistant flame retardant, its preparation method is as follows:

[0037] (1) Preparation of hydroxylated DDP: use DDP and ethylene glycol with a molar ratio of 1:3.00 as raw materials, under the protection of nitrogen or inert gas, carry out esterification reaction, accompanied by vacuum distillation, to obtain terminal hydroxyl The converted DDP, wherein the temperature of the esterification reaction is 180°C, the time is 1.0h, and the vacuum degree of the vacuum distillation is 10KPa;

[0038] (2) Preparation of high-phosphorus content hydrolysis-resistant flame retardant: use hydroxylated DDP and caged pentaerythritol phosphate with a molar ratio of 1:2.01 as raw materials, and under the protection of nitrogen, perform high-pressure transesterification first, and then vacuum transesterification reaction to produce a high phosphorus content hydrolysis-resistant flame retardant, wherein the temperature of the high-pressure transest...

Embodiment 3

[0043] A high phosphorus content hydrolysis-resistant flame retardant, its preparation method is as follows:

[0044] (1) Preparation of hydroxylated DDP: DDP and ethylene glycol with a molar ratio of 1:2.50 are used as raw materials, and under the protection of nitrogen, esterification reaction is carried out, accompanied by vacuum distillation, to obtain hydroxylated DDP , wherein, the temperature of the esterification reaction is 175°C, the time is 2.5h, and the vacuum degree of the vacuum distillation is 8KPa;

[0045] (2) Preparation of high-phosphorus content hydrolysis-resistant flame retardant: use hydroxylated DDP and caged pentaerythritol phosphate with a molar ratio of 1:2.01 as raw materials, and under the protection of nitrogen, perform high-pressure transesterification first, and then vacuum Transesterification reaction to produce a high phosphorus content hydrolysis-resistant flame retardant, wherein the temperature of the high-pressure transesterification react...

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Abstract

The present invention relates to a preparation method of a flame retardant material. The flame retardant material is prepared from plastic matrix and an additive type flame retardant, and the plasticmatrix is one or more of PET, PBT, PTT, PEF, and PA6. A structural formula of the additive type flame retardant is as follows: the additive type flame retardant has a phosphorus content of 13.5-13.8 wt% and a melting point of 228-236 DEG C, after the additive type flame retardant is treated in a sodium hydroxide solution at a temperature of 80 DEG C and a concentration of 0.1 mol / L for 8 h, a phosphorus content retention rate is large than 98%. The preparation method of the flame retardant material is simple in technology and relatively low in cost, and can obtain flame-retardant masterbatch and flame-retardant fiber. The used additive type flame retardant therein is obtained by a transesterification reaction of PEPA with a reactive hydroxyl structure and hydroxyl-terminated DDP, excellentin hydrolysis resistance and high temperature resistance, relatively high in phosphorus content, excellent in flame retardancy and relatively high in melting point.

Description

technical field [0001] The invention belongs to the technical field of flame retardant materials, and relates to a preparation method of flame retardant materials, in particular to a preparation method of flame retardant master batches and flame retardant fibers. Background technique [0002] With the increasing demand for plastic products, its heat resistance and flammability have become research hotspots at home and abroad. The combustion conditions of plastics are related to the temperature of the environment, the composition and structure of plastics, and the concentration of oxygen in the air. As a plastic processing aid, flame retardant is similar to other plastic additives (plasticizers, fillers, colorants, antistatic agents, etc.) need. The limiting oxygen index (LOI) and UL94 grade are commonly used internationally to judge the flame retardant performance of flame retardants in plastics. [0003] According to the application scenarios of flame retardants, the fla...

Claims

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Application Information

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IPC IPC(8): C08L67/02C08L77/02C08K5/5313C07F9/6574C08J3/22D01F1/07D01F6/90D01F6/92
CPCC07F9/65748C08J3/226C08J2367/02C08J2377/02C08J2467/02C08J2477/02C08K5/5313D01F1/07D01F6/90D01F6/92
Inventor 江振林饶品华金亮李利红朱敏胡优贤崔亚慧于运歌
Owner SHANGHAI UNIV OF ENG SCI
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