CN106586963B - A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in the waste water from bromide - Google Patents
A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in the waste water from bromide Download PDFInfo
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- CN106586963B CN106586963B CN201610967913.XA CN201610967913A CN106586963B CN 106586963 B CN106586963 B CN 106586963B CN 201610967913 A CN201610967913 A CN 201610967913A CN 106586963 B CN106586963 B CN 106586963B
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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
- C01B7/093—Hydrogen bromide
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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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The present invention relates to a kind of methods that bromine and co-producing high-purity hydrobromic acid are recycled in waste water from bromide, it takes three-tower rectification mode, and bromine, hydrobromic acid mixture are detached.First tower is except hydrogen chloride column, and tower top is the hydrochloric acid solution containing a small amount of bromine, and tower reactor is bromine and hydrobromic acid, and is sent to second tower；Two towers are bromine extraction towers, using normal pressure or negative pressure rectifying, are more than 99% bromine in overhead extraction content, tower reactor is low-concentration hydrogen bromic acid；Three towers are hydrobromic acid concentration towers, take extracting rectifying, and tower top obtains 48 ~ 62% hydrobromic acid.This method is simple for process, easy to control；The hydrobromic acid purity of preparation is high, and production cost is low.This method is simple for process, easy to control；The hydrobromic acid purity of preparation is high, and production cost is low.
Description
Technical field
The present invention relates to a kind of methods that bromine and co-producing high-purity hydrobromic acid are recycled in waste water from bromide, belong to industry
Technical field of waste water processing.
Background technology
Bromine and hydrobromic acid are important one of industrial chemicals, by bromide derived from it, bromate and brominated organise
Close object has special value in the national economic development.In decabromodiphenylethane product process is produced, generate it is a large amount of it is brominated,
Hydrobromic acid waste water.If bromine therein is recycled and improves the concentration of wherein hydrobromic acid, cost can be substantially reduced, generates visitor
The economic benefit of sight.
At present in China, bromine extracting method is based on steam distillation and air blowout method.This method needs to consume a large amount of
Oxidising agent.Hydrobromic acid has strong volatility at higher concentrations, and industrial is difficult that batch prepares high concentration of hydrogen bromic acid,
The hydrobromic acid of high concentration is needed in some industry, improves the concentration of hydrobromic acid, market different demands can be met.
Invention content
The object of the present invention is to provide a kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in waste water from bromide,
It is simple for process, it is easy to control；The hydrobromic acid purity of preparation is high, and production cost is low.
Technical solution is used by the present invention solves the above problems：One kind recycles bromine and coproduction from bromide waste water
The method of high-purity hydrogen bromic acid, it takes three-tower rectification mode, and bromine, hydrobromic acid mixture are detached.First tower is dechlorination
Change hydrogen tower, tower top is the hydrochloric acid solution containing a small amount of bromine, and tower reactor is bromine and hydrobromic acid, and is sent to second tower；Two towers are bromines
Element extraction tower using normal pressure or negative pressure rectifying, is more than 99% bromine, tower reactor is low-concentration hydrogen bromic acid in overhead extraction content；Three
Tower is hydrobromic acid concentration tower, and extractant is added to take extracting rectifying, and tower top obtains 48 ~ 62% hydrobromic acid.
Specifically include following steps：
(1) it is heated to a tower, at 100-110 DEG C, tower top temperature is controlled at 30-45 DEG C for tower column bottom temperature control；
(2) it is heated to two towers, at 110-120 DEG C, tower top temperature is controlled at 45-60 DEG C the control of two tower column bottom temperatures；
(3) it is heated to three towers, at 121-128 DEG C, tower top temperature is controlled at 123-126 DEG C the control of three tower column bottom temperatures；
(4) bromide waste water is pumped into the middle part of a tower；After the condensed device condensation of tower top material, part reflux, reflux ratio
Control is in 0.5-2；Tower top is low-concentration hcl, and kettle material is sent into two towers；
(5) a tower tower reactor product is pumped into the middle part of two towers；After the condensed device condensation of tower top material, part reflux is returned
Stream is than control in 0.5-2；Tower top is more than 99% bromine for content, and kettle material is sent into three towers；
(6) two tower tower reactor products are pumped into the middle part of three towers；Extractant, the condensed device condensation of tower top material are added in tower reactor
Afterwards, part reflux, reflux ratio are controlled in 0.5-3；Tower top obtains 48 ~ 62% hydrobromic acids, and tower reactor is less than 1% hydrogen bromine for hydrobromic acid
Acid is sent into tail gas absorbing system.
Further, a tower uses atmospheric distillation mode, and two tower uses normal pressure or negative pressure rectifying mode, described
Three towers use extracting rectifying mode.
Further, the two towers vacuum cavitations are in -0.03 ~ -0.08MPa.
Further, solvent selection inorganic non-volatile acid and corresponding salt, bromine system/chlorine system inorganic salts.
The inorganic non-volatile acid is phosphoric acid or sulfuric acid.
The bromine system/chlorine system inorganic salts include sodium salt, sylvite, calcium salt, magnesium salts.
Compared with prior art, the advantage of the invention is that：
This method is simple for process, easy to control；The hydrobromic acid purity of preparation is high, and production cost is low.
Specific embodiment
The present invention is described in further detail with reference to embodiments.
Embodiment 1：
A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in waste water from bromide, the method includes by bromination
The object waste water middle part for being pumped into a tower, one tower column bottom temperature of control are 102 DEG C, and tower top temperature is 30 DEG C, and air-distillation is adjusted
Reflux ratio 0.5, tower top are that content of hydrochloric acid is 10.1%, bromine content 1.5%.
One tower bottom of towe component is sent to the middle part of two towers, and two tower column bottom temperatures of control are 110 DEG C, and tower top temperature is 60 DEG C, and two
For tower vacuum cavitations in -0.05MPa, it is 2 to adjust reflux ratio, and tower top is bromine, content 99.1%.
Two column overhead components are sent in the middle part of three towers, and sodium bromide 600kg is added in tower reactor, control 126 DEG C of three tower column bottom temperature,
Tower top temperature is 125 DEG C, and it is 2 to adjust reflux ratio, and tower top is hydrobromic acid, a concentration of 52%.Bottom of towe is containing aqueous sodium bromide, warp
Cross concentration and recovery sodium bromide.
Embodiment 2：
A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in waste water from bromide, the method includes by bromination
The object waste water middle part for being pumped into a tower, one tower column bottom temperature of control are 105 DEG C, and tower top temperature is 35 DEG C, and air-distillation is adjusted
Reflux ratio 1, tower top are that content of hydrochloric acid is 9.8%, bromine content 1.3%.
One tower bottom of towe component is sent to the middle part of two towers, and two tower column bottom temperatures of control are 115 DEG C, and tower top temperature is 50 DEG C, and two
For tower vacuum cavitations in -0.03MPa, it is 1.5 to adjust reflux ratio, and tower top is bromine, content 99.5%.
Two column overhead components are sent in the middle part of three towers, and magnesium bromide 1000kg is added in tower reactor, control three tower column bottom temperatures 122
DEG C, tower top temperature is 126 DEG C, and it is 2.5 to adjust reflux ratio, and tower top is hydrobromic acid, a concentration of 61.8%.Bottom of towe is water containing magnesium bromide
Solution, by concentration and recovery magnesium bromide.
Embodiment 3：
A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in waste water from bromide, the method includes by bromination
The object waste water middle part for being pumped into a tower, one tower column bottom temperature of control are 110 DEG C, and tower top temperature is 45 DEG C, and air-distillation is adjusted
Reflux ratio 1.5, tower top are that content of hydrochloric acid is 10.0%, bromine content 1.0%.
One tower bottom of towe component is sent to the middle part of two towers, and two tower column bottom temperatures of control are 120 DEG C, and tower top temperature is 45 DEG C, and two
For tower vacuum cavitations in -0.08MPa, it is 1 to adjust reflux ratio, and tower top is bromine, content 99.6%.
Two column overhead components are sent in the middle part of three towers, and calcium chloride 800kg is added in tower reactor, control 128 DEG C of three tower column bottom temperature,
Tower top temperature is 126 DEG C, and it is 1.5 to adjust reflux ratio, and tower top is hydrobromic acid, a concentration of 61.5%.Bottom of towe is water-soluble for chloride containing calcium
Liquid, by concentration and recovery calcium chloride.
Embodiment 4：
A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in waste water from bromide, the method includes by bromination
The object waste water middle part for being pumped into a tower, one tower column bottom temperature of control are 108 DEG C, and tower top temperature is 43 DEG C, and air-distillation is adjusted
Reflux ratio 2, tower top are that content of hydrochloric acid is 10.1%, bromine content 1.5%.
One tower bottom of towe component is sent to the middle part of two towers, and two tower column bottom temperatures of control are 118 DEG C, and tower top temperature is 55 DEG C, and two
For tower vacuum cavitations in -0.07MPa, it is 0.6 to adjust reflux ratio, and tower top is bromine, content 99.5%.
Two column overhead components are sent in the middle part of three towers, and sodium chloride 600kg is added in tower reactor, control 125 DEG C of three tower column bottom temperature,
Tower top temperature is 123 DEG C, and it is 3 to adjust reflux ratio, and tower top is hydrobromic acid, a concentration of 53%.Bottom of towe is sodium chloride-containing aqueous solution, is passed through
Cross concentration and recovery sodium chloride.
In addition to the implementation, it is all to use equivalent transformation or equivalent replacement the invention also includes there is an other embodiment
The technical solution that mode is formed should all be fallen within the scope of the hereto appended claims.
Claims (6)
1. the method for bromine and co-producing high-purity hydrobromic acid is recycled in a kind of waste water from bromide, it is characterised in that：It takes three
Tower rectifying mode detaches bromine, hydrobromic acid mixture；First tower is except hydrogen chloride column, and tower top is the salt containing a small amount of bromine
Acid solution, tower reactor is bromine and hydrobromic acid, and is sent to second tower；Two towers are bromine extraction towers, using normal pressure or negative pressure rectifying,
It is more than 99% bromine in overhead extraction content, tower reactor is low-concentration hydrogen bromic acid；Three towers are hydrobromic acid concentration towers, and extractant is added to adopt
Extracting rectifying is taken, tower top obtains 48 ~ 62% hydrobromic acid；
The extractant is inorganic non-volatile acid and corresponding salt or is bromine system/chlorine system inorganic salts.
2. the method for bromine and co-producing high-purity hydrobromic acid is recycled in a kind of waste water from bromide according to claim 1,
It is characterized in that, described method includes following steps：
(1) it is heated to a tower, at 100-110 DEG C, tower top temperature is controlled at 30-45 DEG C for tower column bottom temperature control；
(2) it is heated to two towers, at 110-120 DEG C, tower top temperature is controlled at 45-60 DEG C the control of two tower column bottom temperatures；
(3) it is heated to three towers, at 121-128 DEG C, tower top temperature is controlled at 123-126 DEG C the control of three tower column bottom temperatures；
(4) bromide waste water is pumped into the middle part of a tower；After the condensed device changes in temperature of tower top material, part reflux, reflux ratio control
In 0.5-2；Tower top is low-concentration hcl, and kettle material is sent into two towers；
(5) a tower tower reactor product is pumped into the middle part of two towers；After the condensed device changes in temperature of tower top material, part reflux, reflux ratio
Control is in 0.5-2；Kettle material is sent into three towers；
(6) two tower tower reactor products are pumped into the middle part of three towers；Extractant is added in tower reactor；After the condensed device changes in temperature of tower top material,
Part reflux, reflux ratio are controlled in 0.5-3；Tower reactor is less than 1% hydrobromic acid for hydrobromic acid, is sent into tail gas absorbing system.
3. the method for bromine and co-producing high-purity hydrobromic acid is recycled in a kind of waste water from bromide according to claim 2,
It is characterized in that：One tower uses atmospheric distillation mode.
4. the method for bromine and co-producing high-purity hydrobromic acid is recycled in a kind of waste water from bromide according to claim 2,
It is characterized in that：The two towers vacuum cavitations are in -0.03 ~ -0.08MPa.
5. bromine and co-producing high-purity hydrobromic acid are recycled in a kind of waste water from bromide according to one of claim 1-4
Method, it is characterised in that：The inorganic non-volatile acid is phosphoric acid or sulfuric acid.
6. bromine and co-producing high-purity hydrobromic acid are recycled in a kind of waste water from bromide according to one of claim 1-4
Method, it is characterised in that：The bromine system/chlorine system inorganic salts are sodium salt, sylvite, calcium salt or magnesium salts.
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| CN201610967913.XA CN106586963B (en) | 2016-11-05 | 2016-11-05 | A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in the waste water from bromide |
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| CN201610967913.XA CN106586963B (en) | 2016-11-05 | 2016-11-05 | A kind of method that bromine and co-producing high-purity hydrobromic acid are recycled in the waste water from bromide |
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| CN110562924A (en) * | 2019-09-12 | 2019-12-13 | 天津中科拓新科技有限公司 | Preparation method of electronic grade hydrogen bromide |
| CN114132898B (en) * | 2021-12-02 | 2023-01-17 | 海南昂扬科技有限公司 | Method for recovering hydrobromic acid |
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| US5457267A (en) * | 1992-03-28 | 1995-10-10 | Hoechst Aktiengesellschaft | Process for disposing of halons or halon-containing fluorocarbons or chlorofluorocarbons |
| JP2875480B2 (en) * | 1994-09-14 | 1999-03-31 | 日本エア・リキード株式会社 | High-purity hydrogen bromide purification method and apparatus |
| CN101657378A (en) * | 2007-02-16 | 2010-02-24 | 雅宝公司 | The technology of combination producing bromine and calcium chloride |
| CN101544439A (en) * | 2009-05-07 | 2009-09-30 | 党葆和 | Comprehensive extraction and processing method of industrial wastewater |
| CN101830438A (en) * | 2010-05-14 | 2010-09-15 | 山东大地盐化集团有限公司 | Method for purifying simple substance bromine from hydrobromic acid mother liquor |
| CN104229737A (en) * | 2014-09-18 | 2014-12-24 | 中盐工程技术研究院有限公司 | Method and device for producing bromine from brominated butyl rubber wastewater through steam distillation |
| CN105600753A (en) * | 2015-12-30 | 2016-05-25 | 山东昌邑廒里盐化有限公司 | Method for extracting bromine from brine |
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