Preparation method of methyl octabromo-ether

A technology of methyl octabromoether and methallyl chloride, which is applied in the field of preparation of methyl octabromoether, can solve the problems of low purity of methyl octabromoether, low process safety, complicated process, etc., and achieve Ease of industrial production, simple process operation, and low bromination reaction temperature

Inactive Publication Date: 2019-02-15
WEIFANG RIXING CHEM
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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 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, special equipment is required for storage and safety measures, and it will release By-product hydrobromic acid; the process is more complicated, and the resulting product methyl octabromoether is not high in purity and poor in quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of methyl octabromoether, comprising the following steps:

[0023] (1) Tetrabromobisphenol A is added into water to dissolve, the molar ratio of water to tetrabromobisphenol A is 2:1, the pH value is adjusted with sodium hydroxide, the pH value is 8, and the first insulation is carried out , then, dropwise add methallyl chloride organic solution, add phase transfer catalyst, carry out second insulation after dropwise addition, then cool down to room temperature, separate layers, get organic layer;

[0024] (2) The brominating agent is added into an organic solvent and dissolved to obtain a brominating agent solution, and the above-mentioned organic layer is added to the catalyst and the brominating agent solution is added dropwise to carry out the bromination reaction. The mole of the brominating agent and tetrabromobisphenol A The ratio is 2:1, and the temperature is 25-55 °C for the third time of heat preservation, then add sodium sulfite aqueous ...

Embodiment 2

[0028] A preparation method of methyl octabromoether, comprising the following steps:

[0029] (1) Tetrabromobisphenol A is added into water to dissolve, the molar ratio of water to tetrabromobisphenol A is 5:1, the pH value is adjusted with sodium hydroxide, the pH value is 9, and the first insulation is carried out , then, dropwise add methallyl chloride organic solution, add phase transfer catalyst, carry out second insulation after dropwise addition, then cool down to room temperature, separate layers, get organic layer;

[0030] (2) The brominating agent is added into an organic solvent and dissolved to obtain a brominating agent solution, and the above-mentioned organic layer is added to the catalyst and the brominating agent solution is added dropwise to carry out the bromination reaction. The mole of the brominating agent and tetrabromobisphenol A The ratio is 3:1, and the temperature is 25-55°C for the third time of heat preservation, then add sodium sulfite aqueous s...

Embodiment 3

[0034] A preparation method of methyl octabromoether, comprising the following steps:

[0035] (1) Tetrabromobisphenol A is added to water for dissolution, the molar ratio of water to tetrabromobisphenol A is 8:1, the pH value is adjusted with sodium hydroxide, the pH value is 10, and the first insulation is carried out , then, dropwise add methallyl chloride organic solution, add phase transfer catalyst, carry out second insulation after dropwise addition, then cool down to room temperature, separate layers, get organic layer;

[0036] (2) The brominating agent is added into an organic solvent and dissolved to obtain a brominating agent solution, and the above-mentioned organic layer is added to the catalyst and the brominating agent solution is added dropwise to carry out the bromination reaction. The mole of the brominating agent and tetrabromobisphenol A The ratio is 4:1, and the temperature is 25-55 ℃ for the third time to keep warm, then add sodium sulfite aqueous soluti...

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Abstract

The invention discloses a preparation method of methyl octabromo-ether and belongs to the technical field of fire retardant methyl octabromo-ether production. The preparation method comprises the following steps: dissolving tetrabromobisphenol A in water, regulating a pH (potential of hydrogen) value with sodium hydroxide, performing heat preservation for the first time, dropwise adding a methallyl chloride organic solution, adding a phase transfer catalyst, after dropwise adding, performing heat preservation for the second time, then cooling to a room temperature, performing lamination, taking an organic layer, dissolving a brominating agent in an organic solvent to form a brominating agent solution, adding the organic layer into a catalyst, dropwise adding the brominating agent solutionfor brominating reaction, performing heat preservation for the third time at 25-55 DEG C, adding a sodium sulfite aqueous solution for reaction, washing with water after the reaction, standing for lamination, taking a lower organic layer, adding into an emolsifier aqueous solution, performing distillation to remove the organic solvent, performing suction filtration to form a material, and drying the material to prepare a product, wherein a mole ratio of the water to tetrabromobisphenol A is (2-8):1; and a range of the pH value is 8-10.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/225C07C41/16
CPCC07C41/16C07C43/225
Inventor 宗先庆张国强郭安昊孙美玲邱亮泽
Owner WEIFANG RIXING CHEM
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