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Synthesis method of hexabromobenzene

A synthesis method and technology of hexabromobenzene, which are applied in chemical instruments and methods, preparation of halogenated hydrocarbons, disproportionation separation/purification of halogenated hydrocarbons, etc., can solve the problems of high reaction temperature requirements and low product yields, and achieve a high reaction temperature Low requirements, high product yield, good catalytic effect

Inactive Publication Date: 2019-05-21
LIANYUNGANG TECHN COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation method of hexabromobenzene in the prior art adopts iron triiodide (or iodine and iron powder) as catalyst, and the reaction temperature requirement is high, and product yield is lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1, a kind of synthetic method of hexabromobenzene, its steps are as follows:

[0017] (1) In the glass-lined reactor, add bromine, anhydrous aluminum trichloride and fuming sulfuric acid through the metering tank, and add benzene in the high tank; the volume of bromine, the quality of anhydrous aluminum trichloride, and fuming sulfuric acid The mass to benzene mass ratio is 280L: 3.2KG: 32KG: 52KG;

[0018] (2) Start stirring, heat the reaction kettle with a water bath, maintain the temperature in the kettle at 45°C, and start to add benzene dropwise. The dropping speed of benzene is controlled to drop 52KG of benzene at a uniform speed every 45 minutes. After 4 hours of reaction, the system is kept warm for 0.8 hour, discharge the hydrogen bromide in the system;

[0019] (3) Add pure water into the kettle, the volume ratio of the added pure water to the bromine added in step (1) is 280:380; pass steam into the reaction kettle for stripping until the residua...

Embodiment 2

[0020] Embodiment 2, a kind of synthetic method of hexabromobenzene, its steps are as follows:

[0021] (1) In the glass-lined reactor, add bromine, anhydrous aluminum trichloride and fuming sulfuric acid through the metering tank, and add benzene in the high tank; the volume of bromine, the quality of anhydrous aluminum trichloride, and fuming sulfuric acid The mass to benzene mass ratio is 320L: 2.8KG: 28KG: 48KG;

[0022] (2) Start stirring, heat the reaction kettle with a water bath, maintain the temperature in the kettle at 50°C, and start to add benzene dropwise. The dropping rate of benzene is controlled to drop 48KG of benzene at a uniform speed every 35 minutes. After 2 hours of reaction, the system is kept warm for 1.5 hour, discharge the hydrogen bromide in the system;

[0023] (3) Add pure water into the kettle, the volume ratio of the added pure water to the bromine added in step (1) is 320: 420; pass steam into the reaction kettle for stripping, until the residu...

Embodiment 3

[0024] Embodiment 3, a kind of synthetic method of hexabromobenzene, its steps are as follows:

[0025] (1) In the glass-lined reactor, add bromine, anhydrous aluminum trichloride and fuming sulfuric acid through the metering tank, and add benzene in the high tank; the volume of bromine, the quality of anhydrous aluminum trichloride, and fuming sulfuric acid The mass to benzene mass ratio is 300L: 3KG: 30KG: 50KG;

[0026] (2) Start stirring, heat the reaction kettle with a water bath, maintain the temperature in the kettle at 48°C, start to add benzene dropwise, and control the dropping rate of benzene to drop 50KG of benzene at a uniform speed every 40 minutes. After reacting for 3 hours, keep the system warm for 1 Hour, discharge the hydrogen bromide in the system; The discharged hydrogen bromide absorbs with sodium hydroxide, obtains by-product sodium bromide;

[0027] (3) Add pure water to the kettle, the volume ratio of the added pure water to the bromine added in step ...

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PUM

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Abstract

The invention relates to a synthesis method of hexabromobenzene, and belongs to the technical field of synthesis of bromine-containing flame retardants. The method includes the following steps that bromine, anhydrous aluminum trichloride and fuming sulfuric acid are added in a glass-enameled reaction kettle, and benzene is added in a head tank; stirring starts, the reaction kettle is heated in water bath, the temperature in the kettle is maintained not more than 50 DEG C, benzene is dropwise added, the dripping speed of benzene is controlled for reaction, the reaction system is subjected to heat preservation, and hydrogen bromide is discharged from the system, wherein 48-52 kg of benzene is dripped at constant speed every 35-45 minutes; pure water is added in the kettle, steam is introduced into the reaction kettle for steam stripping until remaining bromine is completely steamed out, and red products in the reaction kettle are changed into opalescent crystals; after cooling to room temperature and filtering, a filter cake is washed with water and dried to obtain the product. Anhydrous aluminum trichloride serves as a catalyst, the catalytic effect is better, the reaction temperature requirement is low, the product yield is increased by about 10%, meanwhile the use of organic solvents is effectively reduced, and the method is more environmentally friendly and safe.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a synthesis method of hexabromobenzene. Background technique [0002] Hexabromobenzene, English: Hexabromobenzene Chemical formula: C 6 Br 6 HBB, referred to as HBB, is a new bromine-containing environmentally friendly flame retardant. It is insoluble in water, slightly soluble in ethanol, soluble in benzene, and is a non-toxic and environmentally friendly chemical substance. It is mainly used in the industry for thermosetting resins. Combustible processing, especially epoxy resin, ABS, polystyrene, polyethylene, polypropylene, unsaturated resin, polyester and synthetic fiber, etc. have excellent flame retardant effect. It has good heat resistance and good compatibility with resin. It is mainly used for thermosetting resins, especially epoxy resins. With the research of graphene materials, it is also used in the synthesis of graphene materials. [0003] In the prior art, the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/12C07C17/38C07C17/383C07C17/392C07C25/02
Inventor 陈守德孙绪军
Owner LIANYUNGANG TECHN COLLEGE
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