Preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether

A technology of tetrabromobisphenol and monomethyl ether, which is applied in the field of preparation of simultaneous synthesis of tetrabromobisphenol A monomethyl ether and dimethyl ether, and can solve the problems of high price, low yield, complicated preparation method and the like , to achieve the effect of low cost, high yield and easy availability of raw materials

Active Publication Date: 2020-05-15
JIANGSU UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to fill the market gap of TBBPA monomethyl ether and solve the technical problems of complex preparation methods, low yield and high price of commercially available imported dimethyl ether standard products, a simultaneous synthesis of tetrabromobisphenol A monomethyl ether is provided. The preparation method of ether and dimethyl ether, the method of the present invention controls the methylation process of TBBPA, so that it can not only ensure the high conversion efficiency of raw materials, but also reduce the conversion of TBBPA monomethyl ether to TBBPA dimethyl ether

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  • Preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether
  • Preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether
  • Preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether

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Embodiment 1

[0030] A preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether, comprising the steps:

[0031] Take 1g (1.8mmol) of TBBPA in a 25mL pear-shaped flask, add 20mL of acetonitrile to fully dissolve, then add 0.15g (3.6mmol) of sodium hydroxide and vortex to mix, and quickly add 345μL of iodomethane (5.4mmol, ρ=2.28 g / mL), stirred magnetically at room temperature for 15 minutes, heated to 60°C and stirred and refluxed for 4 hours. After the reaction, cooled in an ice bath to terminate the reaction, dissolved and washed with 5 mL of dichloromethane for several times, and filtered to remove sodium hydroxide. After removing water with sodium sulfate, filter and transfer to another pear-shaped bottle, use a rotary evaporator to reduce pressure and rotate to a small volume to obtain a concentrated solution, in which there are unreacted TBBPA, tetrabromobisphenol A monomethyl Tetrabromobisphenol A dimethyl ether and tetrabromobisphen...

Embodiment 2

[0037] A preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether, comprising the steps:

[0038] Take 1g (1.8mmol) of TBBPA in a 25mL pear-shaped flask, add 20mL of acetonitrile to fully dissolve, then add 0.15g (3.6mmol) of sodium hydroxide and vortex to mix, and quickly add 115μL of iodomethane (1.8mmol, ρ=2.28 g / mL), magnetically stirred at room temperature for 15 minutes, heated to 60°C and stirred and refluxed for 4 hours, after the reaction was completed, cooled in an ice bath to terminate the reaction, dissolved and washed with 5 mL of dichloromethane several times, filtered to remove sodium hydroxide, and a small amount of anhydrous After removing water by sodium sulfate, filter and transfer to another pear-shaped bottle, use a rotary evaporator to reduce the pressure and rotate to a small volume to obtain a concentrated solution, in which there are unreacted TBBPA, tetrabromobisphenol A monomethyl ether and tetrabro...

Embodiment 3

[0043] A preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether, comprising the steps:

[0044] Take 1g (1.8mmol) of TBBPA in a 25mL pear-shaped flask, add 20mL of acetonitrile to fully dissolve, then add 0.15g (3.6mmol) of sodium hydroxide and vortex to mix, and quickly add 345μL of iodomethane (5.4mmol, ρ=2.28 g / mL), magnetically stirred at room temperature for 15 minutes, heated to 60°C and stirred for 2 hours under reflux. After removing water by sodium sulfate, filter and transfer to another pear-shaped bottle, use a rotary evaporator to reduce the pressure and rotate to a small volume to obtain a concentrated solution, in which there are unreacted TBBPA, tetrabromobisphenol A monomethyl ether and tetrabromobisphenol A dimethyl ether; the relative percentages of tetrabromobisphenol A monomethyl ether and tetrabromobisphenol A dimethyl ether in the concentrate are 62.5% and 25% respectively.

[0045] According to the m...

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Abstract

The invention relates to a preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether. The preparation method comprises the steps: dissolving TBBPA into acetonitrile; deprotonating with sodium hydroxide, adding methyl iodide, heating to perform methylation reaction, cooling in an ice bath after the reaction is finished, dissolving and cleaning withdichloromethane, filtering, dewatering and concentrating to obtain a concentrated solution, and separating and purifying the concentrated solution by adopting medium-pressure preparative chromatography to obtain tetrabromobisphenol A monomethyl ether and tetrabromobisphenol A dimethyl ether simultaneously. Monomethyl ether and dimethyl ether of TBBPA can be obtained at the same time only throughone-step reaction, and especially the high yield of monomethyl ether is guaranteed; meanwhile, the post-treatment steps are simplified, and losses caused by multiple times of extraction in an existingmethod are avoided; the medium-pressure preparative chromatography adopts silica gel column chromatography, is suitable for purification of constant samples, can accurately separate components in theproduct through real-time control, and ensures the purity of the product.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method for simultaneously synthesizing tetrabromobisphenol A monomethyl ether and dimethyl ether. Background technique [0002] Tetrabromobisphenol A (TBBPA) scientific name is 4,4'-isopropylidene bis(2,6-dibromophenol), the appearance is off-white powder, non-toxic, slightly soluble in water, soluble in methanol, ethanol, etc. Organic solvent has a relatively low vapor pressure at room temperature, its melting point usually ranges from 178°C to 181°C, and its boiling point is about 316°C. It is mainly used as a reactive flame retardant for flame retardancy of printed circuit boards It can also be used as an additive flame retardant in the flame retardant of ABS, HIPS and other materials. It is currently the largest and most widely used brominated flame retardant in the world. [0003] However, whether it is a reactive or additive product, the TBBPA in it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/23C07C43/225
CPCC07C41/16C07C43/23C07C43/225
Inventor 陈娴马璇潘亚男包丽婧顾轩宁罗世鹏程洁红
Owner JIANGSU UNIV OF TECH
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