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Production method of low-residue tetrabromobisphemol A brominated epoxy resin

A technology of brominated epoxy resin and tetrabromobisphenol, which is applied in the production field of low residual tetrabromobisphenol A brominated epoxy resin, can solve the problem of tetrabromobisphenol A brominated epoxy resin production process, which has not been reported and other issues to achieve the effect of reducing product cost and improving product quality

Inactive Publication Date: 2010-09-15
开美化学科技(南通)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Domestic related reports: Shandong Brothers Technology Co., Ltd. and Weifang Brothers Chemical Co., Ltd. (China Patent 200910016470.6), Shandong Ocean Chemical Research Institute ("Chemical Propellants and Polymer Materials"), Dalian University of Technology School of Chemical Engineering ("China Adhesives "), Baling Petrochemical Co., Ltd. ("Chemical Progress"), Guangrao Yutai Salt Chemical Co., Ltd. (China Patent 200410075424.0) and other units have successively reported the production methods of brominated epoxy resins with various molecular weights. The products produced by the process have been partially put into production and recognized by the market, but the production process of low-residual tetrabromobisphenol A brominated epoxy resin has not been reported so far

Method used

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Embodiment 1

[0020] The production method of low residual tetrabromobisphenol A brominated epoxy resin,

[0021] Step 1, etherification reaction: put 450.3Kg epichlorohydrin and 540.5Kg tetrabromobisphenol A into the etherification reaction kettle, add 4.95Kg catalyst benzyltriphenylammonium bromide, etherification temperature 94°C, etherification reaction 3.5h.

[0022] Step 2, ring-closing reaction: vacuumize to remove excess epichlorohydrin, then put in 150.3Kg toluene, control the temperature at about 70°C and put in 260.5Kg of NaOH with a mass concentration of 45% three times for 6 hours of ring-closing reaction.

[0023] Step 3, obtain the oligomer of brominated epoxy resin: put in 198.7Kg of water, add 300.5Kg of toluene, adjust the pH value to 7-8 with sodium dihydrogen phosphate, extract, distill, and recycle toluene to obtain brominated epoxy resin Oligomer 619.3Kg.

[0024] Step 4, synthesis step: After the brominated epoxy resin oligomer is heated, stirred and melted in the s...

Embodiment 2

[0028] The production method of low residual tetrabromobisphenol A brominated epoxy resin,

[0029] Step 1, etherification reaction: put 512.8Kg epichlorohydrin and 615.4Kg tetrabromobisphenol A into the etherification reaction kettle, add 5.64Kg catalyst benzyltriphenylammonium bromide, etherification temperature 95°C, etherification reaction 3.5h.

[0030] Step 2, ring-closing reaction: Vacuumize to remove excess epichlorohydrin, then add 179.3Kg toluene, control the temperature at about 70°C and add 298.6Kg of NaOH with a mass concentration of 45% in three times for 6 hours of ring-closing reaction.

[0031] Step 3, obtain brominated epoxy resin oligomer: put into 226.3Kg water, add 341.4Kg toluene, adjust the pH value to 7-8 with sodium dihydrogen phosphate, extract, distill, reclaim toluene, obtain brominated epoxy resin Oligomer 705.2Kg.

[0032] Step 4, synthesis step: After the brominated epoxy resin oligomer is heated, stirred and melted in the synthesis kettle, 546...

Embodiment 3

[0036] The production method of low residual tetrabromobisphenol A brominated epoxy resin,

[0037] Step 1, etherification reaction: put 1000.2Kg epichlorohydrin and 1200.3Kg tetrabromobisphenol A into the etherification reaction kettle, add 11.02Kg catalyst benzyltriphenylammonium bromide, etherification temperature 93 ℃, etherification reaction 3.5h.

[0038] Step 2, ring-closing reaction: Vacuumize to remove excess epichlorohydrin, then add 340.3Kg toluene, control the temperature at about 70°C and add 542.7Kg of NaOH with a mass concentration of 45% in three times for 6 hours of ring-closing reaction.

[0039] Step 3, obtain the oligomer of brominated epoxy resin: put in 430.1Kg of water, add 609.2Kg of toluene, adjust the pH value to 7-8 with sodium dihydrogen phosphate, extract, distill, and recover toluene to obtain brominated epoxy resin Oligomer 1380.6Kg.

[0040] Step 4, synthesis step: After the brominated epoxy resin oligomer is heated, stirred and melted in the ...

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Abstract

The invention relates to a production method of low-residue tetrabromobisphemol A brominated epoxy resin, comprising an etherification step, a ring-closure reaction step, a step of acquiring brominated epoxy resin oligomer and a synthesis step. The synthesis step comprises the following steps of: heating, stirring and melting the brominated epoxy resin oligomer in a synthesis kettle; adding the tetrabromobisphemol A according to the mass ratio of the tetrabromobisphemol A and the brominated epoxy resin oligomer of 1:1.1 to 1.4; after the materials are melted completely, adding compound auxiliaries accounting for 0.3 to 0.8% of the total mass of the brominated epoxy resin oligomer and the tetrabromobisphemol A in the step, and carrying out the synthesis reaction for 3 to 5h at the temperature of 150 to 200 DEG C and the pressure of 0.3 to 0.5 Pa. The invention greatly reduces the energy consumption and reduces the production cost; meanwhile, the product fills up the blank of the domestic product and meets the international requirements of environmental protection.

Description

technical field [0001] The invention relates to a production method of brominated epoxy resin, in particular to a production method of low residual tetrabromobisphenol A brominated epoxy resin. Background technique [0002] Brominated epoxy resins can be divided into three categories: low, medium and high according to the relative molecular weight, and can be divided into EP type and EC type according to the terminal structure, which can be applied to different plastic materials respectively. In recent years, domestic brominated epoxy resins have developed rapidly, especially the shortcomings of low bromine content, small relative molecular weight, and can only be used as insulating potting materials have been changed. The relative molecular weight of high polymers can be processed according to flame retardant requirements. Produce matching products to produce flame-retardant plastics with good heat resistance, good light resistance, and good impact strength. Today, the nat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/62C08G59/30
Inventor 邢正李召华陈建新
Owner 开美化学科技(南通)有限公司
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