CN101195511A - Method for processing, using and formulating fluorine containing wastewater of naluminum fluoride industry - Google Patents
Method for processing, using and formulating fluorine containing wastewater of naluminum fluoride industry Download PDFInfo
- Publication number
- CN101195511A CN101195511A CNA200710168535XA CN200710168535A CN101195511A CN 101195511 A CN101195511 A CN 101195511A CN A200710168535X A CNA200710168535X A CN A200710168535XA CN 200710168535 A CN200710168535 A CN 200710168535A CN 101195511 A CN101195511 A CN 101195511A
- Authority
- CN
- China
- Prior art keywords
- aluminum fluoride
- reaction
- fluoride
- stop
- calcium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002351 wastewater Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 19
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 18
- 239000011737 fluorine Substances 0.000 title claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 11
- 238000012545 processing Methods 0.000 title claims description 6
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims abstract description 21
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims abstract description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 11
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000292 calcium oxide Substances 0.000 claims abstract description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000001110 calcium chloride Substances 0.000 claims abstract description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 239000011734 sodium Substances 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 9
- -1 sodium aluminum fluoride Chemical compound 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 235000017550 sodium carbonate Nutrition 0.000 claims description 7
- 235000021050 feed intake Nutrition 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 159000000007 calcium salts Chemical class 0.000 claims description 2
- 235000011089 carbon dioxide Nutrition 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000012452 mother liquor Substances 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 239000010842 industrial wastewater Substances 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 abstract description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 abstract description 2
- 229910001610 cryolite Inorganic materials 0.000 abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910004261 CaF 2 Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000247 postprecipitation Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
The invention relates to treatment of industrial wastewater of aluminum fluoride, utilization and a process of preparation. The components of the invention are fluoride wastewater, sodium carbonate, calcium oxide and calcium chloride. The process of preparation is that sodium carbonate is added in the industrial wastewater of aluminum fluoride to produce cryolite products which absorb the fluorine in the wastewater, then calcium oxide is added in cryolite wastewater, calcium fluoride generated by the calcium chloride further absorbs the fluorine in the wastewater, thereby the fluorine content and acidity of the industrial fluoride wastewater reach the national discharging standard.
Description
Technical field:
The present invention relates to domain of inorganic chemistry, produce processing, utilization and the compound method thereof of the industrial fluoride waste of aluminum fluoride especially for the silicofluoric acid method.
Background technology:
Produce the novel industry that aluminum fluoride is the rise in latter stage of China's the eighties in last century with silicofluoric acid, institute's effluent fluorine content and pH value respectively between 4000～8500mg/L and 1.6～3, the problem that to solve this Industrial Wastewater Treatment problem be the sector research always.Known silicofluoric acid method is produced the Industrial Wastewater Treatment behind the aluminum fluoride, the comprehensive precipitator method of the lime that is adopted, and its cost is high and not easily separated, and outer draining fluorine content does not reach discharging standards, has caused the waste and the loss of fluorine raw material yet.Existing enterprise with hydrofluoric acid dry production aluminum fluoride adopts soda ash (Na
2CO
3) or sodium hydroxide (NaOH) with heat after fluoride waste carry out neutralization reaction and generate sodium aluminum fluoride (Na
3AIF
6) precipitation, its investment is big, consumption is high, and environmental pollution is serious, and technology is difficult for grasping, and handled waste water fluorine content does not reach national emission request yet.
, handling in the discharging and can not defective up to standard never have the solution of good technical scheme with the trade effluent behind the silicofluoric acid method production aluminum fluoride for above-mentioned.
Summary of the invention:
Purpose of the present invention, be to produce the Industrial Wastewater Treatment of aluminum fluoride with the silicofluoric acid method, a kind of processing, utilization and compound method thereof of aluminum fluoride industry fluoride waste are provided, it obtains the product sodium aluminum fluoride with easy pharmaceutical chemicals compound method and Technology, reclaim the fluorine raw material, and this trade effluent fluorine (F) content is reduced to below the 10mg/L, pH value reaches 6～9, thereby reaches the discharged wastewater met the national standard purpose.Its raw material is easy to get, and technology is simple and easy, invests for a short time, also can obtain considerable economic.
In order to realize the object of the invention, the contriver handles aluminum fluoride industry fluoride waste and has carried out secular analysis, test, at normal temperatures, adopts three grades of neutralization reaction treatment process, succeeds.
First step reaction: utilize in the waste water remaining aluminum fluoride AIF
3With hydrofluoric acid HF composition, with soda ash NaCO
3Or caustic soda NaOH reacts generation sodium aluminum fluoride Na with it
3AIF
6And precipitate, its throw out is made the sodium aluminum fluoride production marketing after separating, and its waste water pH value transfers to 5～6, and fluorine content reaches below the 1000mg/L.Its main chemical reactions formula is:
2AIF
3+6HF+3Na
2CO
3→2Na
3AIF
6+3CO
2+3H
2O
3HF+AIF
3+3NaOH→Na
3AIF
6+3H
2O
Second stage reaction: reclaim residual fluorine F with lime CaO, to generate Calcium Fluoride (Fluorspan) CaF
2Precipitation, throw out is made byproduct after separating, and its waste water pH value transfers to 7～9, and fluorine content reaches below the 10mg/L, and its main chemical reactions formula is:
2HF+CaO→CaF
2+2H
2O
Third stage reaction: with small amount of calcium chloride CaCI
2Reclaim the residual fluorine F in the waste water, and adjust pH value to 6～8, waste water fluorine content is reduced to below the 5mg/L, and its main chemical reactions formula is:
2HF+CaCI
2→CaF
2+2HCI
The present invention one is respectively (weight fraction) to the feed composition of third order reaction:
First step reaction: aluminum fluoride industry fluoride waste 10～15
Sodium carbonate or caustic soda 0.15～0.5
Second stage reaction: waste water 10～15 after the first step reaction treatment
Calcium oxide or calcium hydroxide 0.05～0.15
Third stage reaction: waste water 10～15 after the reaction treatment of the second stage
Calcium chloride 0.001～0.005
Description of drawings:
Fig. 1 is processing, utilization and the compound method process flow sheet thereof of aluminum fluoride industry fluoride waste of the present invention.
Embodiment:
Below the specific embodiment of the present invention is described in further detail, but the present invention is not limited to following embodiment.
Embodiment 1:
Proportioning raw materials:
First step reaction: aluminum fluoride trade effluent 10
Sodium carbonate (Na
2CO
3) 0.2
Second stage reaction: the postindustrial waste water 10 of first step reaction treatment
Calcium oxide (CaO) 0.08
Third stage reaction: the postindustrial waste water 10 of second stage reaction treatment
Calcium chloride 0.001
The mother liquor of producing aluminum fluoride with the silicofluoric acid method is after crystalline aluminophosphate is fluoridized in separation, and its aluminum fluoride trade effluent is squeezed into one-level metering retort through the naturally cooling post precipitation with pump, starts stirrer, in proportion with yellow soda ash Na
2CO
3Slowly drop into retort and waste water and carry out neutralization reaction, treat that pH value reaches 5.5, when the carbonic acid gas bubble obviously reduces in the jar, stop to feed intake, after 3～5 minutes, stop to stir, left standstill 3 hours, to be crystallized separate out sedimentation after, carry out solid-liquid separation, the crystalline deposit thing promptly gets the sodium aluminum fluoride product after separating drying.It divides dried uply squeezes into the second order reaction jar through settling tank with pump again, and second order reaction jar trade effluent drops into calcium oxide CaO after metering in proportion, starts stirrer, slowly feed intake while stirring, adjusting pH value is 8, and expanding, form calcium salt in a large number with calcium Ca is reaction end, stop to feed intake this moment, react after 1 hour, stop to stir, left standstill 2 hours, after treating abundant precipitated and separated, carry out solid-liquid separation, it divides dried uply squeezes into the third order reaction jar through settling tank with pump again, adds CaCI in proportion
2React, adjusting pH value is 7, and fluorine content reaches below the 10mg/L, discharges after precipitate and separate.
Press GB/T4291-1999 " natural and cryolith chemical analysis method " and Hubei Province's environmental protection tests junction centre detects through national light metal quality test center, the sodium aluminum fluoride fluorine content is 53.61%, aluminum content is 16.79, and containing the sodium amount is 22.63%, meets sodium aluminum fluoride first grade standard; The waste water fluorine content is 2.2mg/L, and pH value is 7, reaches the industrial wastewater discharge standard of national requirements.
Claims (1)
1. processing, utilization and the compound method thereof of aluminum fluoride industry fluoride waste, its special component is (weight fraction):
First step reaction: aluminum fluoride trade effluent 10
Yellow soda ash (Na
2CO
3) 0.2
Second stage reaction: the postindustrial waste water 10 of first step reaction treatment
Calcium oxide (CaO) 0.08
Third stage reaction: the postindustrial waste water 10 of second stage reaction treatment
Calcium chloride 0.001
Its special compound method, the mother liquor of producing aluminum fluoride with the silicofluoric acid method is after crystalline aluminophosphate is fluoridized in separation, and its aluminum fluoride trade effluent precipitates through naturally cooling, squeezes into one-level metering retort with pump, starts stirrer, in proportion with yellow soda ash Na
2CO
3Slowly drop into retort and waste water and carry out neutralization reaction, treat that pH value reaches 5.5, when the carbonic acid gas bubble obviously reduces in the jar, stop to feed intake, after 3～5 minutes, stop to stir, left standstill 3 hours, to be crystallized separate out sedimentation after, carry out solid-liquid separation, the crystalline deposit thing promptly gets the sodium aluminum fluoride product after separating drying; It divides dried uply squeezes into the second order reaction jar through settling tank with pump again, and second order reaction jar trade effluent drops into calcium oxide CaO after metering in proportion, starts stirrer, slowly feed intake while stirring, adjusting pH value is 8, and expanding, form calcium salt in a large number with calcium Ca is reaction end, stop to feed intake this moment, react after 1 hour, stop to stir, left standstill 2 hours, after treating abundant precipitated and separated, carry out solid-liquid separation, it divides dried uply squeezes into the third order reaction jar through settling tank with pump again, adds CaCI in proportion
2React, adjusting pH value is 7, and fluorine content reaches below the 10mg/L, discharges after precipitate and separate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710168535XA CN100551847C (en) | 2007-11-30 | 2007-11-30 | Processing, utilization and the compound method thereof of aluminum fluoride industry fluoride waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200710168535XA CN100551847C (en) | 2007-11-30 | 2007-11-30 | Processing, utilization and the compound method thereof of aluminum fluoride industry fluoride waste |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101195511A true CN101195511A (en) | 2008-06-11 |
| CN100551847C CN100551847C (en) | 2009-10-21 |
Family
ID=39546169
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200710168535XA Active CN100551847C (en) | 2007-11-30 | 2007-11-30 | Processing, utilization and the compound method thereof of aluminum fluoride industry fluoride waste |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100551847C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159342A (en) * | 2011-12-15 | 2013-06-19 | 诺发光电股份有限公司 | Hydrofluoric acid wastewater treatment method |
| CN105753211A (en) * | 2016-03-24 | 2016-07-13 | 北京国环清华环境工程设计研究院有限公司 | Method and system for recovering fluorine from waste acid produced in thinning production of solar cells or glass |
| CN106348328A (en) * | 2016-10-25 | 2017-01-25 | 嘉善蓝欣涂料有限公司 | Method for recycling acid liquor by utilizing aluminum-containing electric cast liquid and fluorine-containing wastewater |
| CN106745138A (en) * | 2017-02-27 | 2017-05-31 | 中南大学 | A kind of use HCl HF mixed gas production hexafluoro sodium aluminate and the method for reclaiming HCl |
| CN106830034A (en) * | 2017-02-09 | 2017-06-13 | 武汉工程大学 | A kind of utilization fluoride waste prepares the method and device of sand like synthetic cryolite |
-
2007
- 2007-11-30 CN CNB200710168535XA patent/CN100551847C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159342A (en) * | 2011-12-15 | 2013-06-19 | 诺发光电股份有限公司 | Hydrofluoric acid wastewater treatment method |
| CN103159342B (en) * | 2011-12-15 | 2014-12-17 | 诺发光电股份有限公司 | Hydrofluoric acid wastewater treatment method |
| CN105753211A (en) * | 2016-03-24 | 2016-07-13 | 北京国环清华环境工程设计研究院有限公司 | Method and system for recovering fluorine from waste acid produced in thinning production of solar cells or glass |
| CN106348328A (en) * | 2016-10-25 | 2017-01-25 | 嘉善蓝欣涂料有限公司 | Method for recycling acid liquor by utilizing aluminum-containing electric cast liquid and fluorine-containing wastewater |
| CN106830034A (en) * | 2017-02-09 | 2017-06-13 | 武汉工程大学 | A kind of utilization fluoride waste prepares the method and device of sand like synthetic cryolite |
| CN106745138A (en) * | 2017-02-27 | 2017-05-31 | 中南大学 | A kind of use HCl HF mixed gas production hexafluoro sodium aluminate and the method for reclaiming HCl |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100551847C (en) | 2009-10-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Free format text: FORMER OWNER: GUO ZHONGCHENG PENG XIAOMAN Owner name: HUBEI YONGSHAO TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: WANG YONGJIN Effective date: 20100519 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
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| CB03 | Change of inventor or designer information |
Inventor after: Wang Yongjin Inventor after: Guo Zhongcheng Inventor after: Peng Xiaoman Inventor after: Wang Xiaohe Inventor after: Zou Jing Inventor before: Wang Yongjin Inventor before: Guo Zhongcheng Inventor before: Peng Xiaoman |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 433100 ROAD 1, HONGQI AVENUE, WANGCHANG TOWN, QIANJIANG CITY, HUBEI PROVINCE TO: 433122 HONGQI AVENUE, WANGCHANG TOWN, QIANJIANG CITY, HUBEI PROVINCE Free format text: CORRECT: INVENTOR; FROM: WANG YONGJIN GUO ZHONGCHENG PENG XIAOMAN TO: WANG YONGJIN GUO ZHONGCHENG PENG XIAOMAN WANG XIAOHE ZOU JING |
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| TR01 | Transfer of patent right |
Effective date of registration: 20100519 Address after: 433122 Hongqi Road, Qianjiang Town, Hubei, China Patentee after: Hubei Yongshao Technology Co.,Ltd. Address before: 433100, Hongqi Road, King Town, Qianjiang, Hubei Co-patentee before: Guo Zhongcheng Patentee before: Wang Yongjin Co-patentee before: Peng Xiaoman |
|
| CP03 | Change of name, title or address |
Address after: 433100 Hongqi Avenue, Jianghan Salt Chemical Industrial Park, Qianjiang City, Hubei Province Patentee after: HUBEI YONG SHAO POLYTRON TECHNOLOGIES Inc. Address before: 433122 Hongqi Avenue, Wangchang Town, Qianjiang City, Hubei Province Patentee before: Hubei Yongshao Technology Co.,Ltd. |
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| CP03 | Change of name, title or address | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Treatment, utilization, and preparation methods of fluoride containing wastewater from aluminum fluoride industry Effective date of registration: 20230913 Granted publication date: 20091021 Pledgee: Agricultural Bank of China Limited Qianjiang Branch Pledgor: HUBEI YONG SHAO POLYTRON TECHNOLOGIES Inc. Registration number: Y2023980056462 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |