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DOPO structure containing polymeric flame retardant used for epoxy resin and preparation method

A flame retardant technology for epoxy resin, applied in the field of polymerized flame retardant containing DOPO structure for epoxy resin and its preparation, can solve the problems of poor water resistance and thermal stability of epoxy resin flame retardant, and achieve easy Industrial production, excellent flame retardant performance, good thermal stability effect

Inactive Publication Date: 2019-10-29
ANQING NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to solve the defects of poor water resistance and poor thermal stability of epoxy resin flame retardants, and provide a polymeric flame retardant containing DOPO structure

Method used

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  • DOPO structure containing polymeric flame retardant used for epoxy resin and preparation method
  • DOPO structure containing polymeric flame retardant used for epoxy resin and preparation method
  • DOPO structure containing polymeric flame retardant used for epoxy resin and preparation method

Examples

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Effect test

Embodiment 1

[0032] Under ice-bath conditions, mix 0.1 mol phosphorus oxychloride, 0.1 mol ODOPM, 0.1 mol triethylamine and 200 ml of acetonitrile, and stir for 2 hours; then dissolve 0.1 mol piperazine in 50 ml of acetonitrile, Then, together with 0.2 mol of triethylamine, it was slowly dropped into the reaction system of the previous step with a constant pressure dropping funnel. After the addition was completed, the temperature of the reaction system rose to 60 ° C, and then continued to stir for 12 hours, cooled to room temperature, and passed Suction filtration, washing with water and drying to obtain a white final product, ie flame retardant FR-1.

[0033] figure 1 Be the phosphorus spectrogram of the flame retardant FR-1 gained in this embodiment, from figure 1 It can be seen that there are only two chemical environments for phosphorus, the shifts are -0.9 and 31ppm, respectively, and there are no other by-products, which shows that the synthesis of the target product is successful...

Embodiment 2

[0036] Under ice bath conditions, mix 0.15 mol phosphorus oxychloride, 0.15 mol ODOPM, 0.15 mol triethylamine and 100 ml of toluene, stir for 4 hours; then dissolve 0.15 mol N-aminoethylpiperazine in 50 ml of toluene, and then slowly drop it into the reaction system of the previous step with a constant pressure dropping funnel together with 0.3 mol of triethylamine. After the addition is completed, the temperature of the reaction system rises to 70 ° C, and then continue to stir for 14 hours , cooled to room temperature, suction filtered, washed with water, and dried to obtain a white final product, namely flame retardant FR-2.

Embodiment 3

[0038] At 15°C, mix 0.1mol phosphorus oxychloride, 0.1mol ODOPM, 0.1mol pyridine and 100ml of 1,4-dioxane, and stir for 4 hours; then add 0.1mol 4' diaminodi Benzyl methane was dissolved in 50 ml of 1,4-dioxane, and then slowly dripped into the reaction system of the previous step together with 0.2 mol of pyridine using a constant pressure dropping funnel. After the addition was completed, the temperature of the reaction system rose to 90°C, then continue to stir and react for 18 hours, cool to room temperature, filter with suction, wash with water, and dry to obtain a yellow final product, namely flame retardant FR-3.

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Abstract

The invention provides a DOPO structure containing polymeric flame retardant used for epoxy resin. The invention solves the problems of poor water resistance and poor thermal stability of an epoxy resin flame retardant. The preparation method for the DOPO structure containing polymeric flame retardant comprises the following steps: A, adding a dried raw material 1 and raw material 2, an acid binding agent and a solvent into a reaction container under the condition of 0 DEG C to 25 DEG C, and carrying out a reaction under continuous stirring for 2 to 12 hours; B, dissolving a raw material 3 into a solvent, slowly dropwise adding an obtained mixture together with an acid binding agent into a reaction system, carrying out heating to 60 to 90 DEG C, and carrying out a reaction for 12 to 24 hours; and C, after the reaction is completed, carrying out cooling to a room temperature, carrying out vacuum filtering, and carrying out washing with water so as to obtain a polymeric flame retardant.The acid binding agent is one selected from the group consisting of triethylamine and pyridine.

Description

technical field [0001] This patent application is supported by the key project of the Anhui Provincial Department of Education (fund number: KJ2018A0381) and the Anhui Provincial Key Laboratory Open Fund (fund number: ZD2017003). It relates to a flame retardant, in particular to a polymeric flame retardant for epoxy resin. Background technique [0002] With the development of science and technology, polymer materials are widely used in aerospace, electronic appliances and other fields due to their excellent mechanical properties, dimensional stability, high temperature resistance, chemical corrosion resistance and electrical insulation properties. Among them, epoxy resin has become the most widely used polymer material. However, ordinary epoxy resins are very flammable, which greatly limits the application of epoxy resins. Therefore, it is of great significance to endow epoxy resin with flame retardancy. [0003] Adding flame retardants can effectively solve the flammabil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/02C08G73/06C08L63/00C08L85/02C08L79/04
CPCC08G79/02C08G73/0644C08L63/00C08L2201/02C08L85/02C08L79/04
Inventor 汪婕赵顺平郭玉孔学军鲍青燕
Owner ANQING NORMAL UNIV
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