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Method for preparing nitrogen phosphate sulfur-containing reactive flame retardant applied to epoxy resin

A technology of reactive flame retardants and epoxy resins, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of decreased mechanical properties of the matrix and poor compatibility of the polymer matrix and other issues, to achieve the effects of improving flame retardancy, easy post-processing, easy control and industrial production

Active Publication Date: 2017-05-31
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the operation is simple, it is accompanied by some problems in use, such as poor compatibility with the polymer matrix, resulting in a decrease in the mechanical properties of the matrix, etc.

Method used

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  • Method for preparing nitrogen phosphate sulfur-containing reactive flame retardant applied to epoxy resin
  • Method for preparing nitrogen phosphate sulfur-containing reactive flame retardant applied to epoxy resin
  • Method for preparing nitrogen phosphate sulfur-containing reactive flame retardant applied to epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a container equipped with a condenser tube and a stirrer, 13.42g p-hydroxybenzaldehyde, 16.5g 2-aminobenzothiazole and 200ml ethanol were added successively under stirring, nitrogen gas was fed into it, and after 2 hours of reaction at 50°C, 23.76g of DOPO was added and the reaction was continued for 24 hours. After the reaction, the system was suction filtered, washed 3 times with ethanol, and dried to obtain the white product 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-(4-hydroxyphenyl) (2 -iminobenzothiazole)methane-10-oxide (D-P-ABZ), yield 89%.

Embodiment 2

[0023] In a container equipped with a condenser tube and a stirrer, 16.10 g of p-hydroxybenzaldehyde, 19.8 g of 2-aminobenzothiazole and 120 ml of acetone were added successively under stirring, nitrogen gas was introduced, and after 1.8 hours of reaction at 52 ° C, 23.76g of DOPO was added and the reaction was continued for 26 hours. After the reaction is complete, filter the solution with suction, wash with acetone for 3 to 4 times, and dry to obtain the white product 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-(4-hydroxyphenyl) (2-Iminobenzothiazole)methane-10-oxide (D-P-ABZ), yield 78%.

Embodiment 3

[0025] In a container equipped with a condenser tube and a stirrer, 14.76g of p-hydroxybenzaldehyde, 18.15g of 2-aminobenzothiazole and 250ml of acetone were added successively under stirring, nitrogen gas was introduced, and after 2.2 hours of reaction at 48°C, Add 23.76g DOPO, continue to react for 26 hours. After the reaction, the system was suction filtered, washed 3 times with acetone, and dried to obtain the white product 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-(4-hydroxyphenyl) (2 -iminobenzothiazole)methane-10-oxide (D-P-ABZ), yield 70%.

[0026] The test and analysis results of the flame retardant D-P-ABZ prepared by the present embodiment are as follows:

[0027] 1 H NMR (400MHz, DMSO-d 6 ), δ (ppm): 9.54, 9.51 (s, 1H), 8.98-9.10 (m, 1H), 8.14-8.21 (m, 2H), 7.44-7.78 (m, 4H), 7.13-7.41 (m, 6H ), 6.96-7.08(m, 2H), 6.69-6.74(m, 2H), 5.57-5.85(m, 1H);

[0028] 31 P-NMR (162MHz, DMSO-d 6 ), δ (ppm): 28.59, 29.96;

[0029] HRMS (EI + ): calcd.for C 26 h 20...

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Abstract

The invention relates to a method for preparing nitrogen phosphate sulfur-containing reactive flame retardant applied to epoxy resin. The preparation method comprises the following steps: sequentially adding p-hydroxy benzaldehyde, aminothiazole and a solvent into a reactor which is provided with a condensing pipe and a stirrer, and introducing inert gas to perform first reaction; adding 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to carry out second reaction; and pumping, filtering, washing and drying the system to obtain white or light brown nitrogen phosphate sulfur-containing reactive flame retardant after the reaction is completed. The method has the advantages that 1, the synthesizing process is short, the cycle is short, post-treatment is easy, and control and industrial production are easy; 2, the prepared flame retardant contains nitrogen, phosphate and sulfur three flame-retardant elements at the same time, has a synergistic flame-retardant effect, and can be used for remarkably improving the flame retarding performance of epoxy resin; and 3, the prepared flame retardant is a reactive flame retardant, and can be used for keeping stability and mechanical performance of cured epoxy resin while improving the flame retarding effect of the cured epoxy resin.

Description

technical field [0001] The invention relates to a preparation method of a reactive flame retardant, in particular to a preparation method of a phosphorus, nitrogen and sulfur reactive flame retardant used in epoxy resin. Background technique [0002] As a typical thermosetting polymer, epoxy resin has excellent adhesion, mechanical properties, electrical insulation and corrosion resistance, as well as low shrinkage, easy processing and low cost, etc. It is used in integrated circuits, transportation , Aerospace and other high-tech fields have been widely used. However, epoxy resin is a flammable material, and when it burns, it has a large heat release rate, high calorific value, fast flame propagation speed, is not easy to extinguish, and sometimes produces dense smoke and toxic gases, causing harm to the environment and endangering people's lives and property. Security poses a huge threat. Therefore, improving the flame retardant properties of epoxy resins has become a ho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08G59/62C08G59/56
CPCC07F9/657172C08G59/56C08G59/621
Inventor 简荣坤王盼夏龙余小琴郑雪琳
Owner FUJIAN NORMAL UNIV
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