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Synthesizing method of tetrabromobisphenol A dual (2,3-dibromo-2-methyl propyl) ether

A technology of tetrabromobisphenol and methyl propyl group, applied in the synthesis field of tetrabromobisphenol A bis(2,3-dibromo-2-methylpropyl) ether, can solve problems such as not being involved, To achieve the effect of easy control, low reaction temperature and high product purity

Active Publication Date: 2013-07-10
SHANDONG RUNKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] None of the prior art relates to the synthetic method of tetrabromobisphenol A bis(2,3-dibromo 2-methylpropyl) ether of the present invention

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Tetrabromobisphenol A and sodium hydroxide are added to water, the mol ratio of tetrabromobisphenol A and sodium hydroxide is 1:1, the amount of water used by tetrabromobisphenol A and sodium hydroxide is the same as that of tetrabromobisphenol A The molar ratio is 2:1; the first heat preservation is carried out after the complete dissolution at room temperature, and the time of the first heat preservation is 0.5h; the pH value is adjusted to 8-9, and the dispersant p-octylphenol polyoxyethylene ether is added to disperse The massfraction that agent accounts for tetrabromobisphenol A is 2%; Then dropwise add methallyl chloride in 1h, the mol ratio of methallyl chloride and tetrabromobisphenol A is 2:1; Carry out the second After the second heat preservation for 5 hours, the temperature was lowered to room temperature for suction filtration, the filter cake was washed with water three times the mass of tetrabromobisphenol A, and dried at 80°C to obtain an intermediate pro...

Embodiment 2

[0026] Tetrabromobisphenol A and sodium hydroxide are added to water, and the mol ratio of tetrabromobisphenol A and sodium hydroxide is 1:2, and the amount of water used for tetrabromobisphenol A and sodium hydroxide is the same as that of tetrabromobisphenol A. The molar ratio is 5:1; the first heat preservation is carried out after the complete dissolution at room temperature, and the time of the first heat preservation is 0.6h; adjust the pH value to 8-10, add dispersant sodium dodecylsulfonate, dispersant Accounting for the mass fraction of tetrabromobisphenol A is 3%; then dropwise add methallyl chloride in 2h, the molar ratio of methallyl chloride and tetrabromobisphenol A is 3:1; carry out the second Insulate for 6 hours, cool down to room temperature and filter with suction, wash the filter cake with water 4 times the mass of tetrabromobisphenol A, and dry at 80°C to obtain an intermediate product.

[0027] Add the intermediate product to the organic solvent chlorofor...

Embodiment 3

[0029] Tetrabromobisphenol A and sodium hydroxide are added to water, the mol ratio of tetrabromobisphenol A and sodium hydroxide is 1:3, the amount of water used by tetrabromobisphenol A and sodium hydroxide is the same as that of tetrabromobisphenol A The molar ratio is 10:1; the first heat preservation is carried out after the complete dissolution at room temperature, and the time of the first heat preservation is 0.7h; the pH value is adjusted to 8-9, and the dispersant sodium stearate is added, and the dispersant accounts for tetrabromo The mass fraction of bisphenol A is 4%; Then dropwise add methallyl chloride in 3h, the molar ratio of methallyl chloride and tetrabromobisphenol A is 2.5:1; Carry out second insulation 7h, Cool down to room temperature and filter with suction, wash the filter cake with water 5 times the mass of tetrabromobisphenol A, and dry at 80°C to obtain an intermediate product.

[0030] Add the intermediate product to the organic solvent dichloroeth...

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PUM

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Abstract

The invention discloses a synthesizing method of a tetrabromobisphenol A dual (2,3-dibromo-2-methyl propyl) ether. The method comprises the following steps: adding tetrabromobisphenol and an alkali into water; stirring until completely dissolving; then carrying out the primary heat preservation; regulating the pH value; adding a dispersing agent; dropwise adding methylallyl chloride and carrying out the secondary heat preservation; after carrying out the primary aftertreatment, obtaining an intermediate product; adding the intermediate product into an organic solvent; stirring until the intermediate product is completely dissolved, and then dropwise adding the bromine; refluxing and carrying out the tertiary heat preservation; and after finishing the tertiary heat preservation, obtaining a product by carrying out the secondary aftertreatment. The method is simple; the adopted solvent can be recycled and reused; the temperature of the bromination reaction is low; the reaction condition is moderate and is easy to control; the energy consumption during the production is low; and the strict reaction conditions are not required by all steps, so that the method is favorable for industrial production. The tetrabromobisphenol A dual (2,3-dibromo-2-methyl propyl) ether as the product is high in yield, good in quality, good in heat stability and high in content, thereby lightening the environmental-protection stress. In addition, the tetrabromobisphenol A dual (2,3-dibromo-2-methyl propyl) ether is high in purity, low in impurity content and free of generating 'three wastes' and environmental pollution.

Description

technical field [0001] The invention relates to the field of flame retardant synthesis, in particular to a synthesis method of tetrabromobisphenol A bis(2,3-dibromo-2-methylpropyl) ether. Background technique [0002] Tetrabromobisphenol A bis(2,3-dibromo-2-methylpropyl) ether is the main product of deep processing of tetrabromobisphenol A. Olefins (such as PP, PE, polybutene, etc.) and thermoplastic elastomer materials. Product use: It is used for flame retardant of polypropylene plastics and fibers, polystyrene foam plastics, and can also be used for flame retardant finishing of polyester fabrics and flame retardant of vinylon coated double-sided leather; used as an additive flame retardant, suitable for Polystyrene, unsaturated polyester, polycarbonate, polypropylene, synthetic rubber, etc. [0003] Tetrabromobisphenol A bis(2,3-dibromo-2-methylpropyl) ether has the characteristics of low dosage, good flame retardant effect, and little influence on the physical properti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/225C07C41/22
Inventor 宗先庆
Owner SHANDONG RUNKE CHEM
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