CN111039484A - Device and method for extracting bromine from tetrabromobisphenol A wastewater - Google Patents
Device and method for extracting bromine from tetrabromobisphenol A wastewater Download PDFInfo
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- CN111039484A CN111039484A CN201911287837.8A CN201911287837A CN111039484A CN 111039484 A CN111039484 A CN 111039484A CN 201911287837 A CN201911287837 A CN 201911287837A CN 111039484 A CN111039484 A CN 111039484A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/09—Bromine; Hydrogen bromide
- C01B7/096—Bromine
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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Abstract
A method for extracting bromine from tetrabromobisphenol A wastewater belongs to the field of tetrabromobisphenol A production. The method comprises the steps of carrying out triple-effect desalination, concentration and acidification on waste water discharged in the production process of tetrabromobisphenol A, carrying out primary distillation and condensation to obtain crude bromine, absorbing the crude bromine by alkali liquor, then feeding the crude bromine into a second distillation tower for secondary distillation, and condensing bromine gas generated by the secondary distillation and separating bromine water to obtain finished bromine. The beneficial effects are that: the problem of the influence of triple effect desalination system sodium bromide concentration enrichment to apparatus for producing among the waste water treatment process of tetrabromobisphenol A is solved, the treatment effect of triple effect evaporation has been promoted to qualified bromine has been obtained, the recycle of bromine resource has been realized. The process flow is simple, common equipment is adopted, the investment cost is low, and good economic benefit can be obtained through the extracted bromine.
Description
Field of the invention
The invention relates to a bromine extraction technology in the field of wastewater treatment generated in the production process of tetrabromobisphenol A (TBBA for short).
Background
Tetrabromobisphenol A is a bromine flame retardant widely applied at present, and is prepared by taking bisphenol A, bromine, hydrogen peroxide, chlorobenzene, sulfuric acid and the like as raw materials through the operations of bromination dehydrogenation, heating and curing, neutralization and bleaching, multiple times of water washing, crystallization and filtration, drying and packaging and the like. In the operation of curing, bleaching, washing and the like, the generated waste water contains bromine ions because excessive bromine is added to ensure the conversion rate of the bisphenol A. The main inorganic salt in the wastewater of TBBA is sodium sulfate, and bromide ions exist in the wastewater in the form of sodium bromide. The sodium sulfate is treated in a mode of triple effect evaporation in the wastewater treatment process, and the sodium sulfate is concentrated, separated and filtered, and the mother liquor is circulated. Because the solubility of sodium bromide will be far more than the solubility of sodium sulfate, sodium bromide is concentrated the enrichment in circulating the mother liquor, can progressively increase the proportion of mother liquor, causes triple effect evaporation circulating pump current to continuously rise, and the boiling point of evaporation rises, influences triple effect evaporation effect, can cause overload when serious, and the motor burns out, blocks up the problem of heating chamber tubulation.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a novel device and a method for extracting bromine from wastewater. And meanwhile, recovering bromine resources in the wastewater.
The technical scheme adopted by the invention is as follows:
an apparatus for extracting bromine from waste water of tetrabromobisphenol A, comprising:
the triple-effect evaporator is used for triple-effect desalination and concentration of wastewater discharged in the production process of tetrabromobisphenol A, so that the wastewater contains bromide ion with concentration of 2-3g/L, and the bromide ion concentration of the mother liquor discharged after 20 times of triple-effect desalination and concentration reaches 40-60 g/L;
the filter is connected with the triple-effect evaporator and is used for filtering the mother liquor concentrated by the triple-effect evaporator;
comprises an acidifier connected with a filter, wherein mother liquor discharged from the filter is acidified by adding acid, the pH value is adjusted to 2-3, and the mother liquor enters a first distillation tower;
the first distillation tower is connected with the acidifier and is used for introducing chlorine and steam into the acidified mother liquor entering the distillation tower and carrying out first distillation at the temperature of 92-95 ℃;
the condenser is connected with the first distillation tower and is used for condensing bromine obtained by distillation in the first distillation tower to obtain crude bromine;
the absorption tower is connected with the condenser and is used for absorbing the crude bromine by 10 percent sodium hydroxide lye to obtain sodium bromide mixed solution;
the second distillation tower is connected with the absorption tower and is used for adding dilute sulfuric acid and steam into the sodium bromide mixed solution entering the distillation tower and carrying out second distillation at the temperature of 92-95 ℃;
and the condensation separator is connected with the second distillation tower and is used for condensing and separating bromine water generated by the second distillation to obtain finished bromine.
Further, the condensation separator is provided with a finished bromine outlet and a bromine water outlet, wherein the bromine water outlet is connected with the second distillation tower, and bromine water obtained by the condensation separator returns to the second distillation tower.
Furthermore, a pipeline connected with an inlet of the triple-effect evaporator is arranged at an outlet of the filter.
Further, the first distillation tower and the second distillation tower are provided with a liquid discharge outlet for discharging the distilled liquid waste.
A method for extracting bromine from tetrabromobisphenol A wastewater is realized by the above device, and comprises the following steps:
1) the waste water discharged in the production process of tetrabromobisphenol A contains bromide ions, the concentration of the bromide ions is 2-3g/l, and the concentration of the bromide ions of the mother liquor discharged after triple effect desalination and concentration is 20 times reaches 40-60 g/l;
2) acidifying the discharged mother liquor by adding acid, adjusting the pH value to 2-3, introducing into a first distillation tower, introducing chlorine gas and steam for first distillation, and controlling the temperature of the first distillation tower to be 92-95 ℃;
3) condensing the bromine obtained by distillation to obtain crude bromine containing bromine water and low-boiling point organic matters;
4) absorbing the crude bromine by 10% sodium hydroxide lye to obtain sodium bromide mixed liquor;
5) feeding the sodium bromide mixed solution into a second distillation tower, adding dilute sulfuric acid and steam for second distillation, and controlling the temperature of the second distillation tower to be 92-95 ℃;
6) and condensing and separating bromine water from bromine gas generated by the second distillation to obtain finished bromine.
The temperature of the first distillation column and the second distillation column is controlled to be the same.
The invention has the advantages and beneficial effects that: the problem of TBBA's waste water treatment in-process triple effect desalination system sodium bromide concentration enrichment to apparatus for producing is solved, the treatment effect of triple effect evaporation has been promoted to obtain qualified bromine, realized the recycle of bromine resource. The process flow is simple, common equipment is adopted, the investment cost is low, and good economic benefit can be obtained through the extracted bromine.
Drawings
FIG. 1: the invention has a structure and a flow diagram;
Detailed Description
For further understanding of the contents, features and effects of the present invention, the following embodiments are enumerated in conjunction with the accompanying drawings, and the following detailed description is given:
referring to fig. 1, the apparatus of the present invention comprises:
the triple-effect evaporator is used for triple-effect desalination and concentration of wastewater discharged in the production process of tetrabromobisphenol A, so that the wastewater contains bromide ion with concentration of 2-3g/L, and the bromide ion concentration of the mother liquor discharged after 20 times of triple-effect desalination and concentration reaches 40-60 g/L;
the filter is connected with the triple-effect evaporator and is used for filtering the mother liquor concentrated by the triple-effect evaporator;
comprises an acidifier connected with a filter, wherein mother liquor discharged from the filter is acidified by adding acid, the pH value is adjusted to 2-3, and the mother liquor enters a first distillation tower;
the first distillation tower is connected with the acidifier and is used for introducing chlorine and steam into the acidified mother liquor entering the distillation tower and carrying out first distillation at the temperature of 92-95 ℃;
the condenser is connected with the first distillation tower and is used for condensing bromine obtained by distillation in the first distillation tower to obtain crude bromine;
the absorption tower is connected with the condenser and is used for absorbing the crude bromine by 10 percent sodium hydroxide lye to obtain sodium bromide mixed solution;
the second distillation tower is connected with the absorption tower and is used for adding dilute sulfuric acid and steam into the sodium bromide mixed solution entering the distillation tower and carrying out second distillation at the temperature of 92-95 ℃;
and the condensation separator is connected with the second distillation tower and is used for condensing and separating bromine water generated by the second distillation to obtain finished bromine.
The condensation separator is provided with a finished bromine outlet and a bromine water outlet, wherein the bromine water outlet is connected with the second distillation tower, and bromine water obtained by the condensation separator returns to the second distillation tower for further rectification. The outlet of the filter is provided with a pipeline connected with the inlet of the triple-effect evaporator and used for refluxing partial mother liquor so as to control the pressure of the device and the amount of the mother liquor entering the acidifier. The first distillation tower and the second distillation tower are provided with liquid discharge outlets for discharging the distilled waste liquid, and are connected to other process devices for acidifying the waste water of other processes.
Example 1:
the waste water discharged in the production process of tetrabromobisphenol A contains bromide ions, the concentration of the bromide ions is about 2-3g/L, the bromide ions are concentrated to a certain degree in a triple-effect evaporation system, the operation of extracting bromine is carried out through filtered mother liquor, and the bromide ion concentration of the mother liquor reaches 40g/L after the mother liquor is subjected to triple-effect desalination and concentration by 20 times. Along with the discharge of partial mother liquor, can effectual control evaporation system's sodium bromide concentration, eliminate the influence that causes because of sodium bromide enrichment.
Acidifying the discharged mother liquor by adding acid, adjusting pH to 2, introducing into a first distillation tower, and introducing chlorine (2 Br)-+cl2＝＝Br2+2cl-) And carrying out primary distillation on the steam, controlling the temperature of a first distillation tower to be 92 ℃, and condensing the bromine obtained by displacement to obtain crude bromine. The crude bromine obtained by extracting from the waste water of tetrabromobisphenol A contains organic matters with low boiling point.
Absorbing the crude bromine by 10% sodium hydroxide lye (3 Br)2+6NaOH＝＝5NaBr+NaBrO3+3H2O) to bromineDissolving sodium mixed solution, absorbing organic matter with alkali solution, introducing the absorption solution into a second distillation tower, and adding dilute sulfuric acid (5NaBr + NaBrO)3+3H2SO4＝3Br2+Na2SO4+3H2O) and steam are distilled for the second time, the temperature of the second distillation tower is controlled to be 92 ℃, the generated bromine gas is condensed and separated from bromine water to obtain the bromine finished product.
Example 2:
the waste water discharged in the production process of tetrabromobisphenol A contains bromide ions, the concentration of the bromide ions is about 2-3g/L, the bromide ions are concentrated to a certain degree in a triple-effect evaporation system, the operation of extracting bromine is carried out through filtered mother liquor, and the bromide ion concentration of the mother liquor reaches 50g/L after the mother liquor is subjected to triple-effect desalination and concentration by 20 times. Along with the discharge of partial mother liquor, can effectual control evaporation system's sodium bromide concentration, eliminate the influence that causes because of sodium bromide enrichment.
Acidifying the discharged mother liquor by adding acid, adjusting pH to 2, introducing into a first distillation tower, and introducing chlorine (2 Br)-+cl2＝＝Br2+2cl-) And carrying out primary distillation on the steam, controlling the temperature of a first distillation tower to be 93 ℃, and condensing the bromine obtained by displacement to obtain crude bromine. The crude bromine obtained by extracting from the waste water of tetrabromobisphenol A contains organic matters with low boiling point.
Absorbing the crude bromine by 10% sodium hydroxide lye (3 Br)2+6NaOH＝＝5NaBr+NaBrO3+3H2O) into sodium bromide mixed solution, absorbing the organic matter by alkali liquor, feeding the absorbing solution into a second distillation tower, adding dilute sulfuric acid (5NaBr + NaBrO)3+3H2SO4＝3Br2+Na2SO4+3H2And O) and steam are subjected to secondary distillation, the temperature of a second distillation tower is controlled to be 93 ℃, generated bromine gas is condensed and separated from bromine water, and a finished product of bromine is obtained.
Example 3:
the waste water discharged in the production process of tetrabromobisphenol A contains bromide ions, the concentration of the bromide ions is about 2-3g/L, the bromide ions are concentrated to a certain degree in a triple-effect evaporation system, the operation of extracting bromine is carried out through filtered mother liquor, and the bromide ion concentration of the mother liquor reaches 60g/L after the mother liquor is subjected to triple-effect desalination and concentration by 20 times. Along with the discharge of partial mother liquor, can effectual control evaporation system's sodium bromide concentration, eliminate the influence that causes because of sodium bromide enrichment.
Acidifying the discharged mother liquor by adding acid, adjusting pH to 3, introducing into a first distillation tower, and introducing chlorine (2 Br)-+cl2＝＝Br2+2cl-) And carrying out primary distillation on the steam, controlling the temperature of a first distillation tower to be 95 ℃, and condensing the bromine obtained by displacement to obtain crude bromine. The crude bromine obtained by extracting from the waste water of tetrabromobisphenol A contains organic matters with low boiling point.
Absorbing the crude bromine by 10% sodium hydroxide lye (3 Br)2+6NaOH＝＝5NaBr+NaBrO3+3H2O) into sodium bromide mixed solution, absorbing the organic matter by alkali liquor, feeding the absorbing solution into a second distillation tower, adding dilute sulfuric acid (5NaBr + NaBrO)3+3H2SO4＝3Br2+Na2SO4+3H2O) and steam are distilled for the second time, the temperature of the second distillation tower is controlled to be 95 ℃, generated bromine gas is condensed and separated from bromine water to obtain finished bromine.
Claims (9)
1. A device for extracting bromine from tetrabromobisphenol A wastewater is characterized by comprising:
the triple-effect evaporator is used for triple-effect desalination and concentration of wastewater discharged in the production process of tetrabromobisphenol A, so that the wastewater contains bromide ion with concentration of 2-3g/L, and the bromide ion concentration of the mother liquor discharged after 20 times of triple-effect desalination and concentration reaches 40-60 g/L;
the filter is connected with the triple-effect evaporator and is used for filtering the mother liquor concentrated by the triple-effect evaporator;
comprises an acidifier connected with a filter, wherein mother liquor discharged from the filter is acidified by adding acid, the pH value is adjusted to 2-3, and the mother liquor enters a first distillation tower;
the first distillation tower is connected with the acidifier and is used for introducing chlorine and steam into the acidified mother liquor entering the distillation tower and carrying out first distillation at the temperature of 92-95 ℃;
the condenser is connected with the first distillation tower and is used for condensing bromine obtained by distillation in the first distillation tower to obtain crude bromine;
the absorption tower is connected with the condenser and is used for absorbing the crude bromine by 10 percent sodium hydroxide lye to obtain sodium bromide mixed solution;
the second distillation tower is connected with the absorption tower and is used for adding dilute sulfuric acid and steam into the sodium bromide mixed solution entering the distillation tower and carrying out second distillation at the temperature of 92-95 ℃;
and the condensation separator is connected with the second distillation tower and is used for condensing and separating bromine water generated by the second distillation to obtain finished bromine.
2. The device for extracting bromine from tetrabromobisphenol A wastewater as claimed in claim 1, wherein: the condensation separator is provided with a finished bromine outlet and a bromine water outlet, wherein the bromine water outlet is connected with the second distillation tower, and bromine water obtained by the condensation separator returns to the second distillation tower.
3. The device for extracting bromine from tetrabromobisphenol A wastewater as claimed in claim 1, wherein: and a pipeline connected with the inlet of the triple-effect evaporator is arranged at the outlet of the filter.
4. The device for extracting bromine from tetrabromobisphenol A wastewater as claimed in claim 1, wherein: the first distillation tower and the second distillation tower are provided with liquid discharge outlets for discharging waste liquid.
5. A method for extracting bromine from waste water of tetrabromobisphenol A, which is realized by the device of any one of claims 1 to 4, and is characterized by comprising the following steps:
1) the waste water discharged in the production process of tetrabromobisphenol A contains bromide ions, the concentration of the bromide ions is 2-3g/l, and the concentration of the bromide ions of the mother liquor discharged after triple effect desalination and concentration is 20 times reaches 40-60 g/l;
2) acidifying the discharged mother liquor by adding acid, adjusting the pH value to 2-3, introducing into a first distillation tower, introducing chlorine gas and steam for first distillation, and controlling the temperature of the first distillation tower to be 92-95 ℃;
3) condensing the bromine obtained by distillation to obtain crude bromine containing bromine water and low-boiling point organic matters;
4) absorbing the crude bromine by 10% sodium hydroxide lye to obtain sodium bromide mixed liquor;
5) feeding the sodium bromide mixed solution into a second distillation tower, adding dilute sulfuric acid and steam for second distillation, and controlling the temperature of the second distillation tower to be 92-95 ℃;
6) and condensing and separating bromine water from bromine gas generated by the second distillation to obtain finished bromine.
6. The method of extracting bromine from waste water of tetrabromobisphenol A as claimed in claim 5, wherein: after the mother liquor is desalted and concentrated by 20 times in a triple effect manner, the concentration of bromide ions is 40g/L, and the temperatures of the first distillation tower and the second distillation tower are respectively controlled to be 92 ℃.
7. The method of extracting bromine from waste water of tetrabromobisphenol A as claimed in claim 5, wherein: after the mother liquor is desalted and concentrated by 20 times in a triple effect manner, the concentration of bromide ions is 50g/L, and the temperatures of the first distillation tower and the second distillation tower are respectively 93 ℃.
8. The method of extracting bromine from waste water of tetrabromobisphenol A as claimed in claim 5, wherein: after the mother liquor is desalted and concentrated by 20 times in a triple effect manner, the concentration of bromide ions is 60g/L, and the temperatures of the first distillation tower and the second distillation tower are respectively controlled to be 95 ℃.
9. The method of extracting bromine from waste water of tetrabromobisphenol A as claimed in claim 5, wherein: the temperature of the first distillation column and the second distillation column is controlled to be the same.
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| CN201911287837.8A CN111039484A (en) | 2019-12-15 | 2019-12-15 | Device and method for extracting bromine from tetrabromobisphenol A wastewater |
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| CN201911287837.8A CN111039484A (en) | 2019-12-15 | 2019-12-15 | Device and method for extracting bromine from tetrabromobisphenol A wastewater |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111514833A (en) * | 2020-06-15 | 2020-08-11 | 天津长芦汉沽盐场有限责任公司 | Tetrabromobisphenol A liquid separation operation method |
| CN113736467A (en) * | 2021-09-27 | 2021-12-03 | 济宁市兖州区碧海化工有限公司 | Method for preparing soil conditioner by using waste bromide |
| CN115466000A (en) * | 2022-11-01 | 2022-12-13 | 天俱时工程科技集团有限公司 | Processing system to bromine system fire retardant waste water bromide ion |
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| CN113736467A (en) * | 2021-09-27 | 2021-12-03 | 济宁市兖州区碧海化工有限公司 | Method for preparing soil conditioner by using waste bromide |
| CN113736467B (en) * | 2021-09-27 | 2023-08-04 | 济宁市兖州区碧海化工有限公司 | Method for preparing soil conditioner by utilizing waste bromide |
| CN115466000A (en) * | 2022-11-01 | 2022-12-13 | 天俱时工程科技集团有限公司 | Processing system to bromine system fire retardant waste water bromide ion |
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