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Preparation method of methyl octabromoether

A technology of methyl octabromo ether and etherifying agent, applied in the field of preparation of methyl octabromo ether, can solve the problems of hindering the use of materials, low process safety, easy thermal degradation and discoloration, etc. Convenient, mildly responsive effect

Inactive Publication Date: 2019-02-12
山东东信新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are still some defects in the existing methyl octabromoether production process: bromine is used as the bromination agent, liquid bromine is a highly corrosive fuming liquid and air pollutant, the process safety is low, and special storage equipment and safety measures are required At the same time, the by-product hydrobromic acid will be released; the product methyl octabromoether has poor thermal stability. When it is used as a flame retardant for material processing, the material added with methyl octabromoether is prone to overheating, degradation and discoloration during processing, hindering The material is used in a wider range of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of methyl octabromoether, comprising the following steps:

[0019] (1) Bisphenol A and etherification agent 2-methallyl chloride are carried out etherification under the alkaline condition of pH 8 (10wt% sodium hydroxide solution can be used to adjust the pH) to generate bisphenol A Bisallyl ether intermediate, the etherification reaction temperature is 30°C, the reaction time is 5h, and the molar ratio of bisphenol A to etherification agent is 1:1.8;

[0020] (2) After the above-mentioned reaction finishes, remove excess etherifying agent and volatile by-product by atmospheric distillation earlier, then the reaction product is adjusted to pH to neutrality, add brominating agent and carry out bromination reaction, described brominating agent is Hydrobromic acid and solid sodium bromide, the temperature of the bromination reaction is 25°C, the bromination reaction time is 4h, the molar ratio of the bromination agent to bisphenol A is 1.5:1, hydrobrom...

Embodiment 2

[0024] A preparation method of methyl octabromoether, comprising the following steps:

[0025] (1) Bisphenol A and etherification agent 2-methallyl chloride are carried out etherification under the alkaline condition of pH 8 (10wt% sodium hydroxide solution can be used to adjust the pH) to generate bisphenol A Bisallyl ether intermediate, the etherification reaction temperature is 45°C, the reaction time is 7h, and the molar ratio of bisphenol A to etherification agent is 1:1.8;

[0026] (2) After the above-mentioned reaction finishes, remove excess etherifying agent and volatile by-product by atmospheric distillation earlier, then the reaction product is adjusted to pH to neutrality, add brominating agent and carry out bromination reaction, described brominating agent is Hydrobromic acid and solid sodium bromide, the temperature of the bromination reaction is 40°C, the bromination reaction time is 6h, the molar ratio of the bromination agent to bisphenol A is 1.7:1, hydrobrom...

Embodiment 3

[0030] A preparation method of methyl octabromoether, comprising the following steps:

[0031] (1) Bisphenol A and etherification agent 2-methallyl chloride are carried out etherification under the alkaline condition of pH 8 (10wt% sodium hydroxide solution can be used to adjust the pH) to generate bisphenol A Bisallyl ether intermediate, the etherification reaction temperature is 55°C, the reaction time is 8h, and the molar ratio of bisphenol A to etherification agent is 1:1.8;

[0032] (2) After the above-mentioned reaction finishes, remove excess etherifying agent and volatile by-product by atmospheric distillation earlier, then the reaction product is adjusted to pH to neutrality, add brominating agent and carry out bromination reaction, described brominating agent is Hydrobromic acid and solid sodium bromide, the temperature of the bromination reaction is 55°C, the bromination reaction time is 8h, the molar ratio of the bromination agent to bisphenol A is 2:1, hydrobromic...

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Abstract

The invention discloses a preparation method of methyl octabromoether, belonging to the technical field of production of the fire retardant methyl octabromoether. The method comprises the following steps: (1) enabling bisphenol A and an etherifying agent 2-methylallyl chloride to be subjected to an etherification reaction under the alkaline condition with a pH value of 8 so as to generate a bisphenol A bisallyl ether intermediate; (2) after the reaction is completed, firstly removing the excessive etherifying agent and volatile by-products by means of atmospheric distillation, then adjusting the pH of the reaction product to be neutral, and adding a brominating agent for carrying out a bromination reaction, wherein the brominating agent is hydrobromic acid and solid sodium bromide; (3) after the bromination reaction is completed, cooling to the room temperature, filtering, washing with deionized water, transferring the reaction product into a crystallization kettle, adding an emulsifier, additives, seed crystal, water and dichloromethane, sealing the crystallization kettle, and heating for desolventizing; finally, separating by means of suction filtration, washing with deionized water, and drying to obtain the methyl octabromoether.

Description

technical field [0001] The invention relates to the technical field of production of flame retardant methyl octabromoether, in particular to a preparation method of methyl octabromoether. Background technique [0002] Methyl octabromoether is one of the brominated flame retardant products, which can be widely used in the flame retardancy of polyethylene, polypropylene, polystyrene and other polyolefins and their copolymers. At present, the scientific research on the new process of brominated flame retardants in various countries in the world is also in-depth and continuous. As one of the high-efficiency brominated flame retardant products, methyl octabromoether is produced and used in compliance with RoHS standards. It is an upgraded product of environmentally friendly flame retardants and brominated flame retardants, and will surely develop into a brominated flame retardant product. The leading product in the fuel market. [0003] There are still some defects in the exist...

Claims

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Application Information

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IPC IPC(8): C07C41/22C07C43/225C07C41/16C07C43/205C07C41/40
CPCC07C41/22C07C41/16C07C41/40C07C43/225C07C43/2055
Inventor 李善录刘冰洋
Owner 山东东信新材料科技股份有限公司
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