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A kind of phosphorus silicon synergistic flame retardant containing epoxy group and preparation method thereof

A technology of phosphorus-silicon synergistic flame-retardant and epoxy groups, which is applied in the field of flame retardants to achieve the effects of good flame retardancy, long-lasting flame retardancy, and good char formation

Active Publication Date: 2021-11-16
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods solve the problem of migration and outflow of flame retardants, but are generally only suitable for the preparation of specific epoxy materials, and have great limitations in application

Method used

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  • A kind of phosphorus silicon synergistic flame retardant containing epoxy group and preparation method thereof
  • A kind of phosphorus silicon synergistic flame retardant containing epoxy group and preparation method thereof
  • A kind of phosphorus silicon synergistic flame retardant containing epoxy group and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Preparation of three (glycidyl ether) methyl silanes:

[0030] In a reaction flask equipped with a stirrer, a thermometer and a distillation condenser, add 6.85g of methyltrimethoxysilane, 11.20g of glycidyl alcohol and 0.65g of tetrabutyl titanate, stir, heat with a boiling water bath, and constantly have methanol distilled. After 2.5 hours of reaction, almost no methanol evaporated, and the system was evacuated for 5 minutes with a vacuum pump to completely remove methanol, and 12.68 g of white tris(glycidyl ether)methylsilane solid was collected, with a yield of 96.2%.

[0031] (2) Preparation of phosphorus-silicon synergistic flame retardant containing epoxy groups:

[0032] In a reaction flask equipped with a stirrer, a thermometer and a reflux condenser, add 12.68g of tris(glycidyl ether) methylsilane, 21.0g of DOPO, 1.9g of triphenylphosphine, and 36g of xylene, and react at 140°C for 4h, and finally The xylene solvent was removed under reduced pressure to ...

Embodiment 2

[0034] (1) Preparation of three (glycidyl ether) methyl silanes:

[0035] Add 6.98g of methyltrimethoxysilane, 11.42g of glycidyl alcohol and 0.66g of tetrabutyl titanate into a reaction flask equipped with a stirrer, a thermometer and a distillation condensing tube, stir, and keep warm at 95°C for a continuous reaction. Methanol distilled off. After reacting for 3 hours, almost no methanol was evaporated. The system was evacuated for 5 minutes with a vacuum pump to completely remove methanol, and 12.84 g of white tris(glycidyl ether)methylsilane solid was collected, with a yield of 95.6%.

[0036] (2) Preparation of phosphorus-silicon synergistic flame retardant containing epoxy groups:

[0037] In the reaction flask equipped with stirrer, thermometer and reflux condenser, add 12.84g tris(glycidyl ether) methyl silane, 21.2g DOPO, 2.0g triphenylphosphine, 40g ethylene glycol diethyl ether, 121 ℃ insulation reaction After 6 hours, the ethylene glycol diethyl ether solvent wa...

Embodiment 3

[0040] Weigh 1g of phosphorus-silicon synergistic flame retardant containing epoxy groups and 20g of epoxy resin E-51 in a beaker, stir and mix evenly, then add 2g of diethylenetriamine, stir and mix evenly, pour polytetrafluoroethylene In the mold, leave it at room temperature for one day to completely cure, take out the sample, the measured limiting oxygen index is 32, and the UL94 vertical combustion rating is V-1.

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Abstract

The invention provides a phosphorus-silicon synergistic flame retardant containing epoxy groups, which has the following molecular structure: the preparation method of the phosphorus-silicon synergistic flame retardants containing epoxy groups is divided into two steps: (1) using methyl trimethyl Oxysilane and glycidyl alcohol are raw materials, and tetrabutyl titanate is a catalyst, and the reaction generates tri(glycidyl ether) methyl silane; (2) tri(glycidyl ether) methyl silane and 9,10-dihydro ‑9‑oxa‑10‑phosphaphenanthrene‑10‑oxide (DOPO) reacts with triphenylphosphine as a catalyst to generate a phospho-silicon synergistic flame retardant containing epoxy groups. The preparation process is simple, the reaction conditions are mild, and the operation is easy. The flame retardant of the invention contains silicon and phosphorus double flame retardant elements and a reactive epoxy group. The flame retardant is mixed with the epoxy resin and then reacted with the curing agent. The flame retardant epoxy material formed has excellent flame retardant performance, good char formation, and the flame retardant will not segregate and move out, which has important application value.

Description

technical field [0001] The invention relates to the field of flame retardants, in particular to a phosphorus-silicon synergistic flame retardant containing epoxy groups and a preparation method thereof. Background technique [0002] Epoxy resin has excellent mechanical properties, chemical corrosion resistance, electrical insulation, bonding performance, and molding performance, and as a reactive cross-linking polymer, epoxy resin does not require solvents during curing and molding, and its own volatility Low and low, there is no pollution problem during use, so it is widely used in coatings, adhesives, electronic packaging materials, aerospace and automotive fields. However, the limiting oxygen index (LOI) of epoxy resin is only 19.8%, which belongs to combustibles, and there is a great fire safety hazard in use. [0003] In order to prepare a flame-retardant epoxy resin, people first think of adding a flame retardant during the curing and molding of the epoxy resin to imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/36C07F9/6574
CPCC07F9/657172C08G59/36
Inventor 袁福根周国庆杨雨蓉
Owner SUZHOU UNIV OF SCI & TECH