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Preparation method of tetrabromobisphenol A bis(dibromoalkane)ether series compounds

A technology of dibromoalkyl and tetrabromobisphenol, which is applied in the field of compound preparation, can solve the problems of high energy consumption, long bromination reaction time, and low final product content, and achieve low reaction temperature, easy industrial production, and products The effect of high yield

Inactive Publication Date: 2016-06-08
WEIFANG YUKAI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the synthetic method of existing bis(dibromoalkyl) ether of tetrabromobisphenol A, only disclose the synthetic method of octabromoether, do not see other bis(dibromoalkyl) ethers of tetrabromobisphenol A Synthetic method, the existing synthetic method of octabromoether, its bromination reaction time is long, energy consumption is high, and final product content is not high

Method used

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  • Preparation method of tetrabromobisphenol A bis(dibromoalkane)ether series compounds
  • Preparation method of tetrabromobisphenol A bis(dibromoalkane)ether series compounds
  • Preparation method of tetrabromobisphenol A bis(dibromoalkane)ether series compounds

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Embodiment 1

[0025] The preparation method of bis(2,3-dibromo-2-methylpropyl) ether of tetrabromobisphenol A, described preparation method comprises the following steps:

[0026] Take 1000kg of tetrabromobisphenol A, 2400kg of methanol, 2400kg of water, mix well, add 170kg of sodium hydroxide, stir to dissolve, adjust the pH to 8.0, then add 380kg of chlorinated isobutylene dropwise, and the chlorinated isobutylene will be dropped within 80 minutes. Reflux at 65°C for 6 hours. After the reaction, cool down to 25°C, centrifuge, take the filter cake, rinse with water, and dry at 75°C to obtain a white intermediate.

[0027] Take 700kg of intermediate, add 1700kg of dichloromethane, add 150kg of dioxane, stir to dissolve, pour 347kg of bromine into the metering tank, add bromine dropwise, and drop bromine completely in about 1 to 2 hours.

[0028] After dripping bromine, react at 42°C for 2 hours. After the reaction is completed, slowly add sodium sulfite aqueous solution (the weight ratio of...

Embodiment 2

[0033] The preparation method of bis(3,4-dibromo-3-methylbutyl) ether of tetrabromobisphenol A, described preparation method comprises the following steps:

[0034] Take 1000kg of tetrabromobisphenol A, 2400kg of methanol, 2400kg of water, mix well, add 170kg of sodium hydroxide, stir to dissolve, adjust the pH to 8.5, then add 438kg of chlorinated isopentene dropwise. After dropping, the temperature was raised to 65°C and refluxed for 6 hours. After the reaction, the temperature was lowered to 25°C, centrifuged, the filter cake was taken, washed with water, and dried at 75°C to obtain a white intermediate.

[0035] Take 700kg of the intermediate, add 1700kg of dichloromethane, add 130kg of tetrahydrofuran, and 0.3kg of sodium bromide, stir to dissolve, put 330kg of bromine into the metering tank, add bromine dropwise, and drop the bromine completely in about 1 to 2 hours.

[0036] After dripping bromine, react at 44°C for 1 hour. After the reaction is completed, slowly add so...

Embodiment 3

[0041] The preparation method of bis(3,4-dibromobutyl) ether of tetrabromobisphenol A, described preparation method comprises the following steps:

[0042] Take 1000kg of tetrabromobisphenol A, 2400kg of methanol, 2400kg of water, mix well, add 170kg of sodium hydroxide, stir to dissolve, adjust the pH to 9.5, then dropwise add 380kg of 4-chloro-1-butene, 4-chloro-1- The butene was dropped within 80 minutes, and the temperature was raised to 65°C to reflux for 6 hours. After the reaction, the temperature was lowered to 25°C, centrifuged, the filter cake was taken, rinsed with water, and dried at 75°C to obtain a white intermediate.

[0043] Take 700kg of the intermediate, add 1700kg of dichloromethane, add 130kg of tetrahydrofuran, and 0.3kg of sodium bromide, stir to dissolve, pour 347kg of bromine into the metering tank, add bromine dropwise, and drop the bromine completely in about 1 to 2 hours.

[0044] After dripping bromine, react at 36°C for 5 hours. After the reaction ...

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Abstract

The invention belongs to the technical field of compound preparation, and particularly relates to a preparation method of tetrabromobisphenol A bis(dibromoalkane)ether series compounds. The preparation method includes the following steps that tetrabromobisphenol A, methyl alcohol and water are mixed evenly, alkali is added and stirred to be completely dissolved, chloroalkene is dripped, and an intermediate is obtained; the intermediate is dissolved in an organic solvent, a catalyst is added and stirred to be completely dissolved, bromine is dripped, heat-preserved reflux is carried out, standing is carried out for layering after a reaction is finished, an organic layer is taken, elutriation crystallization, centrifugation and drying are carried out, and the tetrabromobisphenol A bis(dibromoalkane)ether series compounds are obtained. According to the method, the catalyst is added in the bromination process and can change the polarity of the organic solvent, so that by-products generated in the reaction process are reduced, and the content of the end product is increased by about 10%; the bromination reaction temperature is low, the reaction time is short, and reaction conditions are mild and easy to control; besides, production energy consumption is low, no rigorous reaction condition is needed in any step, the product yield is high, product quality is good, and the flame-retardant effect is good.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation method of tetrabromobisphenol A bis(dibromoalkyl) ether series compounds. Background technique [0002] Tetrabromobisphenol A bis (dibromoalkyl) ether is a downstream series of products based on tetrabromobisphenol A. The tetrabromobisphenol A bis (dibromoalkyl) ether commonly used in the market is octabromobisphenol A Ether, tetrabromobisphenol A bis(2,3-dibromopropyl) ether is one of this series of compounds. [0003] Compared with tetrabromobisphenol A, octabromoether has the characteristics of low dosage, good flame retardant effect, and little influence on the physical properties of materials. It is mainly used in EPS, polypropylene and other styrene resins, and can better show its Excellent performance. In addition, it is suitable for flame retardant treatment of knitted fabrics, styrene-butadiene rubber, adhesives, coatings and unsa...

Claims

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Application Information

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IPC IPC(8): C07C41/22C07C43/225
CPCC07C41/22C07C41/16C07C43/225C07C43/2055
Inventor 王艳红
Owner WEIFANG YUKAI CHEM
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