阅读说明：本技术 一种节能环保阻燃剂四溴双份a的制备方法 (Preparation method of energy-saving environment-friendly flame retardant tetrabromo double-part A ) 是由 王盛海 郭建树 赵震 于 2021-02-02 设计创作，主要内容包括：本发明提供一种节能环保阻燃剂四溴双份A的制备方法,包括如下步骤：(1)将一定量的双酚A加入氯化苯中搅拌至物料混合均匀,搅拌时间为0.5h,在特定的温度下,同时滴加溴素和双氧水,得到四溴双酚A的溶液。(2)反应体系升温进行熟化反应,熟化完成后静置分出水相,收集有机相进行四次静置分层处理,四次静置分层后收集的有机相采用冷冻盐水降温至8℃,抽滤,得到四溴双份A产品。本发明的制备方法母液使用次数可达到100次以上,减少了废渣的产生,亚钠用量可节约50%；母液循环使用100次,产品色度为20,纯度为99.35%,收率为99.8%；产品综合收率99.6%,产品平均纯度99.54%。(The invention provides a preparation method of an energy-saving environment-friendly flame retardant tetrabromo double part A, which comprises the following steps: (1) adding a certain amount of bisphenol A into chlorobenzene, stirring until the materials are uniformly mixed, wherein the stirring time is 0.5h, and simultaneously dropwise adding bromine and hydrogen peroxide at a specific temperature to obtain a tetrabromobisphenol A solution. (2) Heating the reaction system to carry out curing reaction, standing and separating out a water phase after curing is finished, collecting an organic phase to carry out standing and layering treatment for four times, cooling the collected organic phase to 8 ℃ by adopting frozen brine after standing and layering for four times, and carrying out suction filtration to obtain a tetrabromo-bis-A product. The preparation method has the advantages that the using frequency of the mother liquor can reach more than 100 times, the generation of waste residues is reduced, and the using amount of sodium sulfite can be saved by 50 percent; the mother liquor is recycled for 100 times, the chroma of the product is 20, the purity is 99.35 percent, and the yield is 99.8 percent; the comprehensive yield of the product is 99.6 percent, and the average purity of the product is 99.54 percent.)

1. A preparation method of an energy-saving environment-friendly flame retardant tetrabromo double A is characterized by comprising the following steps:

(1) adding a certain amount of bisphenol A into chlorobenzene, stirring until the materials are uniformly mixed, wherein the stirring time is 0.5h, and simultaneously dropwise adding bromine and hydrogen peroxide at a specific temperature to obtain a tetrabromobisphenol A solution;

(2) heating the reaction system to carry out curing reaction, standing and separating out a water phase after curing is finished, collecting an organic phase to carry out standing and layering treatment for four times, cooling the collected organic phase to 8 ℃ by adopting frozen brine after standing and layering for four times, and carrying out suction filtration to obtain a tetrabromo-bis-A product.

2. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo double A as claimed in claim 1, characterized in that the four times of standing layering are as follows: standing for the first time for layering: adding 20g of 10% sodium sulfite solution into the organic phase for reduction, heating to 90 ℃, standing for 0.5h, separating out the water phase after standing, and collecting the organic phase;

standing and layering for the second time: and adding 20g of 10% sodium sulfite solution into the organic phase collected by the first standing and layering for bleaching, raising the temperature to 90 ℃, starting standing for 0.5h, separating out the water phase after the standing is finished, and collecting the organic phase.

3. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo double A as claimed in claim 2, characterized by further comprising the following steps: and (3) collecting bleaching wastewater generated by the secondary standing and layering, adding polypropionamide into the bleaching wastewater, stirring and dissolving, then adding polyaluminium chloride, stirring to separate out solids, filtering by using a sand core funnel of G4, wherein the solids are colored, the filtrate is treated sodium sulfite, the color is obviously lightened and the filtrate is ready for use, and the water obtained by secondary washing is also filtered by using a sand core funnel of G4, and the filtrate is used for use.

4. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo double A according to claim 1, characterized in that the dropping temperature of the bromine and the hydrogen peroxide is 0-30 ℃, preferably 20-30 ℃.

5. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo-bis-A as claimed in claim 1, wherein the mass ratio of the bisphenol A to the chlorobenzene is 1: 4-6.

6. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo double A as claimed in claim 1, characterized in that the bisphenol A: bromine: the molar ratio of hydrogen peroxide is 1: 2.01-2.1: 2.01-2.11.

7. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo-bis A as claimed in claim 1, wherein the curing reaction temperature is 0-95 ℃, and the curing time is 0.5-1 h.

8. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo-bis-A as claimed in claim 7, wherein the curing reaction temperature is 85-95 ℃.

9. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo-bis-A as claimed in claim 3, wherein the dosage of the polypropionamide is 0.05% -0.2% of the dosage of the sodium sulfite.

10. The preparation method of the energy-saving and environment-friendly flame retardant tetrabromo-bis A as claimed in claim 3, wherein the dosage of the polyaluminium chloride is 0.05% -0.2% of the dosage of sodium sulfite.

Technical Field

The invention relates to tetrabromobisphenol A, in particular to a preparation method of energy-saving and environment-friendly flame retardant tetrabromobisphenol A.

Background

Tetrabromobisphenol A is a reactive flame retardant and an additive flame retardant, is widely used for producing flame retardant plastics, and has good flame retardant effect. As a reactive flame retardant, the flame retardant can be used for producing flame retardant resins such as epoxy resin, polycarbonate and the like; as an additive flame retardant, the flame retardant is used for producing flame retardant resins such as polystyrene resin, ABS resin, phenolic resin and the like.

In the prior art, tetrabromobisphenol A is produced by using chlorobenzene as a solvent, and after the bisphenol A and the chlorobenzene are mixed, metered hydrogen peroxide is added, and then the mixture reacts with bromine to generate the tetrabromobisphenol A. The oxidation reaction is carried out in the reaction process to generate yellow substances, so that the color of the mother liquor is darker and darker in the production process, and the chroma of the product is also bigger and bigger; in order to ensure that the product chromaticity meets the requirement, mother liquor has to be distilled to remove colored substances, and the repeated use times of the chlorobenzene mother liquor are less. Meanwhile, tetrabromobisphenol A has higher solubility in chlorobenzene, so that the product loss is higher, the total yield of the product is lower, and the production cost is higher.

The invention with the application number of CN201710357593.0 discloses a method for producing tetrabromobisphenol A, which prepares a finished product of tetrabromobisphenol A through catalytic reaction, curing reaction, reduction reaction, washing process, crystallization process, centrifugal separation and vacuum drying. According to the technology, the purity of the product is gradually reduced along with the increase of the circulation times of the mother liquor, and meanwhile, the product quality is seriously influenced, so that the chromaticity of the product is higher and higher, and after the mother liquor of the technology is applied for 20 times, the product quality is seriously reduced, and the requirements of customers cannot be met; meanwhile, the patent technology can generate a large amount of waste residues and waste water in practical application, and influences the environment.

Disclosure of Invention

In order to solve the technical problems in the prior art, the invention provides a preparation method of an energy-saving and environment-friendly flame retardant tetrabromo double A, which achieves the following aims: the circulation times of the mother liquor are increased, and the quality and the yield of the product are ensured; the using amount of sodium sulfite is reduced, and the generation of waste residue is reduced; the washing water is recycled, so that the washing amount is reduced, and the generation of waste water is reduced.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

the invention relates to a preparation method of an energy-saving environment-friendly flame retardant tetrabromo double part A, which comprises the following steps:

(1) adding a certain amount of bisphenol A into chlorobenzene, stirring until the materials are uniformly mixed, wherein the stirring time is 0.5h, and simultaneously dropwise adding bromine and hydrogen peroxide at a specific temperature to obtain a tetrabromobisphenol A solution.

(2) Heating the reaction system for curing reaction, standing and separating out a water phase after curing is finished, collecting an organic phase for standing and layering for four times, cooling the collected organic phase after standing and layering for four times to 8 ℃ by using frozen brine, and performing suction filtration to obtain a tetrabromobisphenol A product.

Preferably, the four standing layers are: standing for the first time for layering: adding 20g of 10% sodium sulfite solution into the organic phase for reduction, heating to 90 ℃, standing for 0.5h, separating out the water phase after standing, and collecting the organic phase;

standing and layering for the second time: adding 20g of 10% sodium sulfite solution into the organic phase collected by the first standing and layering for bleaching, heating to 90 ℃, starting standing for 0.5h, separating out the water phase after the standing is finished, and collecting the organic phase;

standing and layering for the third time: adding 50g of water into the organic phase collected by the second standing and layering, heating to 90 ℃, starting standing for 0.5h, separating out the water phase after the standing is finished, and collecting the organic phase;

standing and layering for the fourth time: adding 50g of water into the organic phase collected by the third standing and layering, heating to 90 ℃, starting standing for 0.5h, separating out the water phase after the standing is finished, and collecting the organic phase.

Preferably, the bleaching wastewater generated by the second standing and layering is collected, the polypropionamide is added into the bleaching wastewater, stirred and dissolved, then the polyaluminium chloride is added, the solid is separated out by stirring, the obtained solution is filtered by a sand core funnel of G4, the solid is colored, the filtrate is the treated sodium sulfite, the color is obviously lightened and the sodium sulfite is ready for use, the water obtained by the second washing is also filtered by a sand core funnel of G4, and the filtrate is used for use.

Preferably, the dropping temperature of the bromine and the hydrogen peroxide is 0-30 ℃, preferably 20-30 ℃.

Preferably, the mass ratio of the bisphenol A to the chlorobenzene is 1: 4-6.

Preferably, the bisphenol a: bromine: the molar ratio of hydrogen peroxide is 1: 2.01-2.1: 2.01-2.11.

Preferably, the curing reaction temperature is 0-95 ℃, and preferably 85-95 ℃; the curing time is 0.5-1 h.

Preferably, the dosage of the polypropiocetamide is 0.05% -0.2% of the dosage of the sodium sulfite;

preferably, the dosage of the polyaluminium chloride is 0.05-0.2% of the dosage of sodium sulfite.

Compared with the prior art, the invention has the beneficial effects that:

(1) according to the preparation method of the energy-saving and environment-friendly flame retardant tetrabromobisphenol A, the yield of the tetrabromobisphenol A product is 80%, the product purity is 99.8%, and the product detection chromaticity is 5.

(2) According to the preparation method of the energy-saving and environment-friendly flame retardant tetrabromo double A, the using frequency of the mother liquor can reach more than 100 times, the generation of waste residues is reduced, and the using amount of sodium sulfite can be saved by 50%.

(3) According to the preparation method of the energy-saving and environment-friendly flame retardant tetrabromo double A, the mother liquor is recycled for 100 times, the product chromaticity is 20, the purity is 99.35%, and the yield is 99.8%; the comprehensive yield of the product is 99.6 percent, and the average purity of the product is 99.54 percent.

(4) According to the preparation method of the energy-saving and environment-friendly flame retardant tetrabromo double part A, waste water obtained by washing twice is filtered by the precision filter and then directly used for washing once, so that the generation of waste water is saved.

Detailed Description

In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.

Example 1

100g of benzene chloride and 22.8g of bisphenol A are added, and stirring is started for 0.5 h. After stirring, dropwise adding 33.2g of bromine and 25.8g of hydrogen peroxide at the same time, controlling the dropwise adding temperature to be 25 ℃, after dropwise adding, heating to 90 ℃, keeping the temperature for reaction for 1h, standing for layering, standing for 0.5h, separating out the water phase, adding 20g of 10% sodium sulfite solution into the organic phase for reduction, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of organic phase water, heating to 90 ℃, standing for 0.5h, separating out the water phase, heating to 90 ℃, standing for 0.5h, cooling the organic phase to 8 ℃ by using frozen saline, obtaining a tetrabromobisphenol A product and a filtrate, wherein the filtrate is recycled as a mother liquor.

The mother liquor comprises tetrabromobisphenol A and tribromobisphenol A.

Calculated by bisphenol A, the yield of the tetrabromobisphenol A product is 80%, the purity of the product is 99.8%, and the product detection chromaticity is 5.

And adding 0.02G of polypropylacetamide into the bleaching wastewater obtained by the standing and layering separation in the second step, stirring and dissolving, then adding 0.02G of polyaluminum chloride, stirring to separate out solids, filtering by using a sand core funnel of G4, wherein the solids are colored, the filtrate is the treated sodium sulfite, the color is obviously lightened and the sodium sulfite is ready for use, and the water obtained by secondary washing is also filtered by using a sand core funnel of G4, and the filtrate is used for use.

Example 2

The mother liquor of example 1 was used and 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added, and stirring was started for 0.5 h. After stirring, dropwise adding 33.2g of bromine and 25.8g of hydrogen peroxide at the same time, controlling the dropwise adding temperature to be 25 ℃, after dropwise adding, heating to 88 ℃, keeping the temperature for reaction for 0.5h, standing for layering, standing for 0.5h, separating out the water phase, reducing 20g of recovered sodium sulfite in an organic phase in a sleeving manner, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, heating to 90 ℃, standing for 0.5h, cooling the organic phase to 8 ℃ by using frozen saline, obtaining a tetrabromobisphenol A product and filtrate, and recycling the filtrate as mother liquor.

Based on bisphenol A, the yield of the tetrabromobisphenol A product is 99.75%, the purity of the product is 99.78%, and the product detection chromaticity is 5; the overall yield of the product of example 1-2 was 89.875%.

And adding 0.03G of polypropylacetamide into the bleaching wastewater obtained by standing, layering and separating, stirring for dissolving, then adding 0.03G of polyaluminum chloride, stirring to separate out a solid, filtering by using a sand core funnel of G4, wherein the solid is colored, the filtrate is the treated sodium sulfite, the color is obviously lightened for use, and the water obtained by secondary washing is also filtered by using a sand core funnel of G4, and the filtrate is used for use.

Example 3

The mother liquor of example 2 was used and 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added, and stirring was started for 0.5 h. After stirring, simultaneously dripping 32.6g of bromine and 25.5g of hydrogen peroxide, controlling the dripping temperature to be 30 ℃, after finishing dripping, heating to 88 ℃, keeping the temperature for reaction for 0.5h, standing for layering, standing for 0.5h, separating out a water phase, reducing 20g of recovered sodium sulfite in an organic phase in a sleeving manner, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, heating to 90 ℃, standing for 0.5h, cooling the organic phase to 8 ℃ by adopting frozen saline, obtaining a tetrabromobisphenol A product and a filtrate, and recycling the filtrate as a mother solution.

Based on bisphenol A, the yield of the tetrabromobisphenol A product is 99.8%, the purity of the product is 99.72%, the product detection chromaticity is 5, and the comprehensive yield of the products of examples 1-3 is 93.18%.

And (3) adding 0.03G of polypropylacetamide into the bleaching wastewater obtained by the standing and layering separation in the second step, stirring and dissolving, then adding 0.03G of polyaluminum chloride, stirring to separate out a solid, filtering by using a sand core funnel of G4, wherein the solid is colored, the filtrate is the treated sodium sulfite, the color is obviously lightened and the sodium sulfite is ready for use, and the water obtained by secondary washing is also filtered by using a sand core funnel of G4, and the filtrate is used for use.

Example 4

The mother liquor from example 3 was used and 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added, and stirring was started for 0.5 h. After stirring, simultaneously dripping 32.6g of bromine and 25.5g of hydrogen peroxide, controlling the dripping temperature to be 25 ℃, after finishing dripping, heating to 88 ℃, keeping the temperature for reaction for 40min, standing for layering, standing for 0.5h, separating out a water phase, adding 20g of recycled sodium sulfite for reduction in an organic phase, heating to 90 ℃, standing for 0.5h, separating out a water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of organic phase water, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, cooling the organic phase to 8 ℃ by adopting frozen saline, and performing suction filtration to obtain a tetrabromobisphenol A product and a filtrate, wherein the filtrate is used as a mother solution for recycling.

Based on bisphenol A, the yield of the tetrabromobisphenol A product is 99.82%, the product purity is 99.75%, the product detection chromaticity is 5, and the comprehensive yield of the products of examples 1-4 is 94.84%.

And (3) adding 0.04G of polypropylacetamide into the bleaching wastewater obtained by the standing and layering separation in the second step, stirring and dissolving, then adding 0.04G of polyaluminum chloride, stirring to separate out solids, filtering by using a sand core funnel of G4, wherein the solids are colored, the filtrate is the treated sodium sulfite, the color is obviously lightened and the sodium sulfite is ready for use, and the water obtained by secondary washing is also filtered by using a sand core funnel of G4, and the filtrate is used for use.

Example 5

The mother liquor of example 4 was used and 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added, and stirring was started for 0.5 h. After stirring, simultaneously dripping 32.4g of bromine and 25.1g of hydrogen peroxide, controlling the dripping temperature to be 25 ℃, after finishing dripping, heating to 88 ℃, keeping the temperature for reaction for 40min, standing for layering, standing for 0.5h, separating out a water phase, adding 20g of recycled sodium sulfite for reduction in an organic phase, heating to 90 ℃, standing for 0.5h, separating out a water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of organic phase water, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, cooling the organic phase to 8 ℃ by adopting frozen saline, and performing suction filtration to obtain a tetrabromobisphenol A product and a filtrate, wherein the filtrate is used as a mother solution for recycling.

Based on bisphenol A, the yield of the tetrabromobisphenol A product is 99.78%, the purity of the product is 99.73%, the product detection chromaticity is 5, and the comprehensive yield of the products in examples 1-5 is 95.83%.

And (3) adding 0.03G of polypropylacetamide into the bleaching wastewater obtained by the standing and layering separation in the second step, stirring and dissolving, then adding 0.03G of polyaluminum chloride, stirring to separate out a solid, filtering by using a sand core funnel of G4, wherein the solid is colored, the filtrate is the treated sodium sulfite, the color is obviously lightened and the sodium sulfite is ready for use, and the water obtained by secondary washing is also filtered by using a sand core funnel of G4, and the filtrate is used for use.

Example 6

The mother liquor from example 5 was used, 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added, and stirring was started for 0.5 h. After stirring, simultaneously dripping 32.4g of bromine and 25.1g of hydrogen peroxide, controlling the dripping temperature to be 20 ℃, after finishing dripping, heating to 88 ℃, keeping the temperature for reaction for 50min, standing for layering, standing for 0.5h, separating out a water phase, adding 20g of recycled sodium sulfite for reduction in an organic phase, heating to 90 ℃, standing for 0.5h, separating out a water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of organic phase water, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, cooling the organic phase to 8 ℃ by adopting frozen saline, and performing suction filtration to obtain a tetrabromobisphenol A product and a filtrate, wherein the filtrate is used as a mother solution for recycling.

Based on bisphenol A, the yield of the tetrabromobisphenol A product is 99.85 percent, the purity of the product is 99.75 percent, the product detection chromaticity is 5, and the comprehensive yield of the products of examples 1 to 6 is 96.5 percent.

And (3) adding 0.03G of polypropylacetamide into the bleaching wastewater obtained by the standing and layering separation in the second step, stirring and dissolving, then adding 0.03G of polyaluminum chloride, stirring to separate out a solid, filtering by using a sand core funnel of G4, wherein the solid is colored, the filtrate is the treated sodium sulfite, the color is obviously lightened and the sodium sulfite is ready for use, and the water obtained by secondary washing is also filtered by using a sand core funnel of G4, and the filtrate is used for use.

Example 7

The mother liquor collected in example 6 was used again 15 times, 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added each time, and stirring was started for 0.5 h. After stirring, simultaneously dripping 32.6g of bromine and 25.5g of hydrogen peroxide, controlling the dripping temperature to be 25 ℃, after finishing dripping, heating to 88 ℃, keeping the temperature for reaction for 40min, standing for layering, standing for 0.5h, separating out a water phase, adding 20g of recycled sodium sulfite for reduction in an organic phase, heating to 90 ℃, standing for 0.5h, separating out a water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of organic phase water, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, cooling the organic phase to 8 ℃ by adopting frozen saline, and performing suction filtration to obtain a tetrabromobisphenol A product and a filtrate, wherein the filtrate is used as a mother solution for recycling.

The 15 th time of mother liquor reuse (namely, the 20 times of mother liquor reuse collected in the example 1), the chroma of the product is 10, the purity is 99.65%, and the yield is 99.8%. The comprehensive yield of the products of examples 1-7 is 98.857%, and the average purity of the products is 99.72%.

Example 8

The mother liquor collected in example 7 was used again for 30 times, 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added each time, and stirring was started for 0.5 h. After stirring, simultaneously dripping 32.6g of bromine and 25.5g of hydrogen peroxide, controlling the dripping temperature to be 25 ℃, after finishing dripping, heating to 88 ℃, keeping the temperature for reaction for 40min, standing for layering, standing for 0.5h, separating out a water phase, adding 20g of recycled sodium sulfite for reduction in an organic phase, heating to 90 ℃, standing for 0.5h, separating out a water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of organic phase water, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, cooling the organic phase to 8 ℃ by adopting frozen saline, and performing suction filtration to obtain a tetrabromobisphenol A product and a filtrate, wherein the filtrate is used as a mother solution for recycling.

The 30 th time of mother liquor reuse (namely, the mother liquor collected in the example 1 is reused for 50 times), the chroma of the product is 15, the purity is 99.55%, and the yield is 99.8%. Examples 1 to 8 the overall yield of the product was 99.41%, and the average purity of the product was 99.63%

EXAMPLE 9

The mother liquor collected in example 8 was used again for 50 times, 1.5g of fresh chlorobenzene and 22.8g of bisphenol A were added each time, and stirring was started for 0.5 h. After stirring, simultaneously dripping 32.6g of bromine and 25.5g of hydrogen peroxide, controlling the dripping temperature to be 25 ℃, after finishing dripping, heating to 88 ℃, keeping the temperature for reaction for 40min, standing for layering, standing for 0.5h, separating out a water phase, adding 20g of recycled sodium sulfite for reduction in an organic phase, heating to 90 ℃, standing for 0.5h, separating out a water phase, adding 20g of 10% sodium sulfite solution into the organic phase for bleaching, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of organic phase water, heating to 90 ℃, standing for 0.5h, separating out the water phase, adding 50g of water into the organic phase, heating to 90 ℃, standing for 0.5h, separating out the water phase, cooling the organic phase to 8 ℃ by adopting frozen saline, and performing suction filtration to obtain a tetrabromobisphenol A product and a filtrate, wherein the filtrate is used as a mother solution for recycling.

The 50 th time of mother liquor reuse (namely the mother liquor collected in the example 1 is reused for 100 times), the chroma of the product is 20, the purity is 99.35%, and the yield is 99.8%. Examples 1 to 9 the overall yield of the product was 99.6%, and the average purity of the product was 99.54%

All percentages used in the present invention are mass percentages unless otherwise indicated.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.