CN106946385A - A kind of recoverying and utilizing method of high-concentration fluorine-containing waste water - Google Patents
A kind of recoverying and utilizing method of high-concentration fluorine-containing waste water Download PDFInfo
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- CN106946385A CN106946385A CN201710287539.3A CN201710287539A CN106946385A CN 106946385 A CN106946385 A CN 106946385A CN 201710287539 A CN201710287539 A CN 201710287539A CN 106946385 A CN106946385 A CN 106946385A
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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
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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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
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
- Removal Of Specific Substances (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of recoverying and utilizing method of high-concentration fluorine-containing waste water, it is characterised in that：Calcium chloride is added in the raw water of high-concentration fluorine-containing waste water first, chemical precipitation processing is carried out, then separation of solid and liquid, calcirm-fluoride solid is collected, fluorine is reclaimed；It is introduced into after gained supernatant liquor is pre-processed simultaneously in the diluting compartment and enriched chamber of electrodialysis plant, carries out electrodialysis process, realize that the concentration of fluorine ion in electrodialytic fresh water reaches below 10mg/L, then electrodialytic concentrated water is handled as raw water.Handling process of the invention is simple, workable, effluent characteristics are stable, can be widely used for the recycling of high-concentration fluorine-containing waste water.
Description
Technical field
The present invention relates to the process that a kind of high-concentration fluorine-containing waste water is recycled, and in particular to fluorine-containing in industrial production
The handling process of waste water.
Background technology
Fluorine is a kind of trace element, and Trace Fluoride plays the role of to promote upgrowth and development of children and anti-caries, fluorinated volume 0.5~
1.0mg/L water is useful and harmless to human body, but long-term high-fluorine water of the content more than 1.5mg/L of drinking then can bring unfavorable to human body
Influence, serious meeting causes den tal fluorosis and fluorosis of bone.Fluorine in nature is mainly lain in fluorite, fluor-apatite, ice crystal,
They are all industrial chemicals, are widely used in aluminium metallurgy, steel, organic synthesis chemical industry, electronics industry, atomic energy industry and organic
In the industrial productions such as fluorine lubricating oil, fluorination hydrazine, fluorine refrigeration machine, and substantial amounts of fluoride waste is discharged in these industrial productions, it is dirty
Contaminate environment, make animals and plants poisoning, influence agricultural and animal husbandry production, very big threaten more is caused to human body health.China is existing
's《Integrated wastewater discharge standard》(GB8978-1996) F in regulation discharge water-Mass concentration be no more than 10mgL-1.So
Fluorine-containing industrial wastewater must be acted upon.
At present, there are many kinds to the processing method of high-concentration fluorine-containing waste water both at home and abroad, but main the having of industrialized method
Learn the precipitation method and coagulation sedimentation.
Chinese patent (CN104478059A) reports a kind of acidic high-strength fluorine-containing wastewater treatment method, and being first will be fluorine-containing
Then the pH value regulation of waste water adds calcium chloride solution, stirring sedimentation, using the method to 8.5~9.5 according to Ca/F=0.7
The concentration of waste water fluorine ion 20mg/L be can be dropped to, state sewage emission standard, but calcirm-fluoride purity obtained by the method do not reached
Height, is conducive to the recycling of fluorine in wastewater.
Chinese patent (A of CN 102276034) reports a kind of technique for removing fluorine in thermal power plant's high-concentration fluorine-containing waste water
Method, the process employs chemical precipitation method and coagulation sedimentation combined fluorine removing, adds chlorine in high-concentration fluorine-containing waste water first
Change calcium, carry out first of fluorine removal, after by the fluoride waste pH value regulation to 5.5~6.5 or so addition coagulant and flocculant enter
Fluorinion concentration in fluoride waste effectively can be reduced to 10mg/L by second of fluorine removal of row, this method.But in this method,
The factors such as raw water fluorinated volume, basicity, salinity, coagulation mixing time all have certain influence on defluorination effect；And apply coagulating sedimentation
Method fluorine removal, the coagulation dosage that need to be added is larger, and processing cost is big, while producing more reluctant waste residue, defluorination effect is not
It is very stable, sulfate ion concentration is higher in water quality after fluorine removal, substantial amounts of dissolving aluminium is contained in the water after particularly handling, this
Cause worry of the people to health.
The content of the invention
To overcome the problems of existing process technology, the invention provides a kind of recovery of high-concentration fluorine-containing waste water profit
With method, it is intended to the technique being combined by chemical precipitation method and electrodialytic technique, secondary fluorine removal, so that high-concentration fluorine-containing waste water
In fluorine can recycle, while being reduced to the content of fluoride ion in fluoride waste reaches discharging standards.
To achieve the above object, the present invention is adopted the following technical scheme that：
The recoverying and utilizing method of high-concentration fluorine-containing waste water of the present invention, its feature is：First in high-concentration fluorine-containing waste water
Calcium chloride is added in raw water, chemical precipitation processing is carried out, then separation of solid and liquid, calcirm-fluoride solid is collected, fluorine is reclaimed；Simultaneously by institute
It is introduced into after obtaining supernatant liquor pretreatment in the diluting compartment and enriched chamber of electrodialysis plant, carries out electrodialysis process, realize electrodialysis
Fresh water in the concentration of fluorine ion reach below 10mg/L, then using electrodialytic concentrated water as the high-concentration fluorine-containing waste water original
Water is handled.Specifically include following steps：
(1) according to Ca：F=1：1.2~2 mol ratio, into the raw water of high-concentration fluorine-containing waste water, addition mass concentration is
5% calcium chloride solution, stirs 20~40min, stands 10~30min, then carries out separation of solid and liquid, collects gained calcirm-fluoride and consolidates
Body simultaneously reclaims fluorine, while collecting supernatant liquor and carrying out step (2)；
(2) supernatant liquor of gained in step (1) is pre-processed, including filter organics removal and suspension, it is soft
Change is handled；
(3) diluting compartment and the enriched chamber of electrodialysis plant will be passed into through step (2) pretreated supernatant liquor, and
Electrolyte solution is passed through in pole room, electrodialysis is carried out；
When fluorinion concentration is less than 10mg/L in electrodialytic fresh water, stop electrodialysis, while by electrodialytic concentrated water
Handled as the raw water of the high-concentration fluorine-containing waste water in step (1).
It is preferred that, the speed of stirring is maintained at 300rpm~500rpm in step (1).
It is preferred that, electrolyte solution described in step (3) is metabisulfite solution, sodium chloride solution or sodium nitrate solution；Institute
The concentration for stating electrolyte solution is 0.05-0.3mol/L.
It is preferred that, it is constant voltage mode processing that the operating condition of electrodialysis process is carried out in step (3), and film is controlled voltage
0.8-1V。
It is preferred that, in step (3), high value is reached for the content of fluoride ion that makes electrodialysis concentrated water, in favor of chemical precipitation,
It is 5~10 to set electrodialysis diluting compartment and enriched chamber's input material volume ratio：1.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) method of the present invention combines the sediment fluorination of chemical precipitation method and electrodialytic technique, wherein chemical precipitation method
Calcium purity is high, is conducive to recycling fluorine, is arrived while can effectively reduce the fluorine ion in fluoride waste by electrodialytic technique
Below 10mg/L, reaches discharging standards, improves the comprehensive utilization value of waste water.
(2) handling process of the present invention is simple, workable, and effluent characteristics are stable, can be widely used for high-concentration fluorine-contained useless
The recycling of water.
(3) method of the present invention can preferably control the hardness of fluorinated volume in water, salt content and water, and can increase beneficial
In the trace element of health, while the cleannes of water are improved, the mouthfeel of water is improved.
(4) method that this high-concentration fluorine-containing waste water of the invention is recycled, energy comprehensive reutilization fluoride waste becomes useless
It is a kind of ideal technology method of suitable popularization and application for treasured.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Electrodialysis plant used by following embodiments is by diluting compartment, enriched chamber, pole room, membrane module, circulating pump, flowmeter, straight
Flow power supply and assembling framework composition；Electrodialysis plant is the CJED- that Hefei Ke Jia macromolecular materials Science and Technology Ltd. produces
2040-20 equipment, used electrodialysis cation-exchange membrane and anion-exchange membrane are respectively the good macromolecular material of Hefei section
CJMC the and CJMA films of Science and Technology Ltd.'s production, film logarithm is 20 pairs.
Embodiment 1
The desulfurization wastewater of Anhui power plant is taken as high-concentration fluorine-containing waste water raw water, its F-Ion concentration be 200mg/L~
300mg/L, pH are 5.5 or so.It is handled by the method for the present invention, it specifically includes following steps：
(1) high-concentration fluorine-containing waste water raw water is flowed into precipitation reaction pond, according to Ca：F=1：1.2 mol ratio, to
The calcium chloride solution that mass concentration is 5% is added in raw water, with 300rpm rotating speed stirring reaction 20min, is then stood
20min, separation of solid and liquid collects gained calcirm-fluoride solid and reclaims fluorine, while collecting supernatant liquor and carrying out step (2)；Through inspection
The content for surveying fluorine ion in supernatant liquor is 43mg/L.
(2) supernatant liquor of gained in step (1) is pre-processed, including filter organics removal and suspension, it is soft
Change processing and remove Ca and Mg etc.；
(3) diluting compartment and the enriched chamber of electrodialysis plant will be passed into through step (2) pretreated supernatant liquor, and
0.1mol/L metabisulfite solutions are passed through in pole room, electrodialysis is carried out；To improve the F contents in the final concentrate in enriched chamber, desalination
Room processing waste water 15L, enriched chamber add waste water 2L.Experimentation uses constant voltage mode, and voltage is fixed as 20V, and experimental temperature is
Room temperature, the F ion content of fluoride waste in detection diluting compartment is sampled every 5min, when F ion content is less than 10mg/L, is terminated
This time test, the F ion content in detection enriched chamber's fluoride waste is 282mg/L, and it is real that replacing diluting compartment feed liquid carries out next group
Test, while concentrated water is incorporated into precipitation reaction pond by step (1)~(3) circular treatment.
Embodiment 2
The desulfurization wastewater of Anhui power plant is taken as high-concentration fluorine-containing waste water raw water, its F-Ion concentration be 200mg/L~
300mg/L, pH are 5.5 or so.It is handled by the method for the present invention, it specifically includes following steps：
(1) high-concentration fluorine-containing waste water raw water is flowed into precipitation reaction pond, according to Ca：F=1：1.8 mol ratio, to
The calcium chloride solution that mass concentration is 5% is added in raw water, with 400rpm rotating speed stirring reaction 20min, is then stood
20min, separation of solid and liquid collects gained calcirm-fluoride solid and reclaims fluorine, while collecting supernatant liquor and carrying out step (2)；Through inspection
The content for surveying fluorine ion in supernatant liquor is 56mg/L.
(2) supernatant liquor of gained in step (1) is pre-processed, including filter organics removal and suspension, it is soft
Change processing and remove Ca and Mg etc.；
(3) diluting compartment and the enriched chamber of electrodialysis plant will be passed into through step (2) pretreated supernatant liquor, and
0.05mol/L metabisulfite solutions are passed through in pole room, electrodialysis is carried out；To improve the F contents in the final concentrate in enriched chamber, desalination
Room processing waste water 15L, enriched chamber add waste water 2L.Experimentation uses constant voltage mode, and voltage is fixed as 20V, and experimental temperature is
Room temperature, the F ion content of fluoride waste in detection diluting compartment is sampled every 5min, when F ion content is less than 10mg/L, is terminated
This time test, the F ion content in detection enriched chamber's fluoride waste is 322mg/L, and it is real that replacing diluting compartment feed liquid carries out next group
Test, while concentrated water is incorporated into precipitation reaction pond by step (1)~(3) circular treatment.
Embodiment 3
Waste water same as Example 1 is handled by the identical method of embodiment 1, step (1) is differed only in and adds
Enter after calcium chloride solution, the pH=7 of fluoride waste is adjusted using ammoniacal liquor, other steps are same as Example 1.After testing, this reality
The content for applying fluorine ion in supernatant liquor obtained by example is 21mg/L；After electrodialysis process, when the F ion of fluoride waste in diluting compartment
When content is less than 10mg/L, the F ion content of enriched chamber's fluoride waste is 162mg/L.
The exemplary embodiment of the present invention is the foregoing is only, is not intended to limit the invention, it is all the present invention's
Any modification, equivalent and improvement made within spirit and principle etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of recoverying and utilizing method of high-concentration fluorine-containing waste water, it is characterised in that：First in the raw water of high-concentration fluorine-containing waste water
Middle addition calcium chloride, carries out chemical precipitation processing, then separation of solid and liquid, collects calcirm-fluoride solid, reclaims fluorine；Simultaneously by gained
It is introduced into after layer clear liquid pretreatment in the diluting compartment and enriched chamber of electrodialysis plant, carries out electrodialysis process, realize electrodialytic light
The concentration of fluorine ion reaches below 10mg/L in water, then enters electrodialytic concentrated water as the raw water of the high-concentration fluorine-containing waste water
Row processing.
2. the recoverying and utilizing method of high-concentration fluorine-containing waste water according to claim 1, it is characterised in that including following step
Suddenly：
(1) according to Ca：F=1：1.2~2 mol ratio, it is 5% that mass concentration is added into the raw water of high-concentration fluorine-containing waste water
Calcium chloride solution, stirs 20~40min, stands 10~30min, then carries out separation of solid and liquid, collects gained calcirm-fluoride solid simultaneously
Fluorine is reclaimed, while collecting supernatant liquor and carrying out step (2)；
(2) supernatant liquor of gained in step (1) is pre-processed, including at filtering organics removal and suspension, softening
Reason；
(3) diluting compartment and the enriched chamber of electrodialysis plant will be passed into through step (2) pretreated supernatant liquor, and in pole room
In be passed through electrolyte solution, carry out electrodialysis；
When in electrodialytic fresh water fluorinion concentration be less than 10mg/L when, stop electrodialysis, while using electrodialytic concentrated water as
The raw water of the high-concentration fluorine-containing waste water in step (1) is handled.
3. the recoverying and utilizing method of high-concentration fluorine-containing waste water according to claim 2, it is characterised in that：Step is stirred in (1)
The speed mixed is maintained at 300rpm~500rpm.
4. the recoverying and utilizing method of high-concentration fluorine-containing waste water according to claim 2, it is characterised in that：Institute in step (3)
Electrolyte solution is stated for metabisulfite solution, sodium chloride solution or sodium nitrate solution；The concentration of the electrolyte solution is 0.05-
0.3mol/L。
5. the recoverying and utilizing method of high-concentration fluorine-containing waste water according to claim 2, it is characterised in that：Step is entered in (3)
The operating condition of row electrodialysis process is constant voltage mode processing, and film is controlled in 0.8-1V voltage.
6. the recoverying and utilizing method of high-concentration fluorine-containing waste water according to claim 2, it is characterised in that：In step (3), electricity
Dialysis diluting compartment and enriched chamber's input material volume ratio are 5~10：1.
7. the recoverying and utilizing method of high-concentration fluorine-containing waste water according to claim 2, it is characterised in that：In step (3), institute
Electrodialysis plant is stated to be made up of diluting compartment, enriched chamber, pole room, membrane module, circulating pump, flowmeter, dc source and assembling framework；
Amberplex, electrode and filter are housed in the membrane module；The amberplex is homogeneous ion-exchange membrane, film logarithm
For 5-1000 pairs.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109105586A (en) * | 2018-09-05 | 2019-01-01 | 安徽农业大学 | A method of preparing low fluorine instant tea powder |
| CN110817924A (en) * | 2019-10-09 | 2020-02-21 | 江西理工大学 | Method for treating fluorine-containing waste gas |
| CN112028296A (en) * | 2020-07-22 | 2020-12-04 | 兆德（南通）电子科技有限公司 | Recovery treatment process of fluorine-containing waste liquid |
| CN113321226A (en) * | 2021-06-30 | 2021-08-31 | 攀钢集团研究院有限公司 | Method for removing fluorine in ionic membrane caustic soda by using brine prepared from chlorination residues |
| CN115259482A (en) * | 2021-04-29 | 2022-11-01 | 中国石油化工股份有限公司 | Treatment method of fluorine-containing boron-containing wastewater |
| CN115259483A (en) * | 2021-04-29 | 2022-11-01 | 中国石油化工股份有限公司 | Treatment method and treatment device for fluorine-containing boron-containing wastewater |
| CN117228871A (en) * | 2023-09-08 | 2023-12-15 | 北京神舟茂华环保科技有限公司 | Method for selectively separating fluoride ions from fluoride-containing wastewater and recycling full components |
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| CN101941752A (en) * | 2010-09-05 | 2011-01-12 | 中南大学 | Method and device for treating fluorine-containing waste water |
| CN102659277A (en) * | 2012-05-10 | 2012-09-12 | 杭州蓝然环境技术有限公司 | Ammonium fluoride wastewater treatment technique |
| CN105347574A (en) * | 2015-12-10 | 2016-02-24 | 浙江奇彩环境科技有限公司 | Fluoride removal method of graphite purification waste water and processing system |
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Patent Citations (3)
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| CN101941752A (en) * | 2010-09-05 | 2011-01-12 | 中南大学 | Method and device for treating fluorine-containing waste water |
| CN102659277A (en) * | 2012-05-10 | 2012-09-12 | 杭州蓝然环境技术有限公司 | Ammonium fluoride wastewater treatment technique |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109105586A (en) * | 2018-09-05 | 2019-01-01 | 安徽农业大学 | A method of preparing low fluorine instant tea powder |
| CN110817924A (en) * | 2019-10-09 | 2020-02-21 | 江西理工大学 | Method for treating fluorine-containing waste gas |
| CN112028296A (en) * | 2020-07-22 | 2020-12-04 | 兆德（南通）电子科技有限公司 | Recovery treatment process of fluorine-containing waste liquid |
| CN115259482A (en) * | 2021-04-29 | 2022-11-01 | 中国石油化工股份有限公司 | Treatment method of fluorine-containing boron-containing wastewater |
| CN115259483A (en) * | 2021-04-29 | 2022-11-01 | 中国石油化工股份有限公司 | Treatment method and treatment device for fluorine-containing boron-containing wastewater |
| CN115259482B (en) * | 2021-04-29 | 2023-12-12 | 中国石油化工股份有限公司 | Treatment method of fluorine-containing and boron-containing wastewater |
| CN115259483B (en) * | 2021-04-29 | 2023-12-12 | 中国石油化工股份有限公司 | Treatment method and treatment device for fluorine-containing and boron-containing wastewater |
| CN113321226A (en) * | 2021-06-30 | 2021-08-31 | 攀钢集团研究院有限公司 | Method for removing fluorine in ionic membrane caustic soda by using brine prepared from chlorination residues |
| CN117228871A (en) * | 2023-09-08 | 2023-12-15 | 北京神舟茂华环保科技有限公司 | Method for selectively separating fluoride ions from fluoride-containing wastewater and recycling full components |
| CN117228871B (en) * | 2023-09-08 | 2024-04-16 | 北京神舟茂华环保科技有限公司 | Method for selectively separating fluoride ions from fluoride-containing wastewater and recycling full components |
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