CN102079534A - Method for producing cryolite by using fluorine-containing waste residues of electrolytic aluminium - Google Patents
Method for producing cryolite by using fluorine-containing waste residues of electrolytic aluminium Download PDFInfo
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- CN102079534A CN102079534A CN2010105919048A CN201010591904A CN102079534A CN 102079534 A CN102079534 A CN 102079534A CN 2010105919048 A CN2010105919048 A CN 2010105919048A CN 201010591904 A CN201010591904 A CN 201010591904A CN 102079534 A CN102079534 A CN 102079534A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention belongs to the technical field of aluminum industry smelting, and relates to a method for producing cryolite by using fluorine-containing waste residues of electrolytic aluminium. The technical scheme adopted by the invention is as follows: the fluorine-containing waste residues of the electrolytic aluminium and concentrated sulfuric acid are taken as raw materials to produce the cryolite. The method provided by the invention is used to improve the use ratio of the cryolite, prevent the waste of fluorine resources, and reduce the environmental pollution.
Description
Technical field
The invention belongs to the aluminum metal technical field of smelting, relate to the method that a kind of electrolytic aluminium containing waste slag of fluorine is produced sodium aluminum fluoride.
Background technology
At present, Jue Daduoshuo fluoride salt product all is with fluorite (main component CaF
2) be raw material production; the standing stock of fluorite are very limited; grand strategy resource as the development nuclear industry; each state all pays much attention to the protection to fluorite resource; along with deficient day by day, the continuous of price of fluorite resource in the world wide are risen, causing the inorganic fluorine chemical industry to seek other fluorine resources becomes inexorable trend.
Sodium aluminum fluoride is a kind of fluoaluminate, also claims sodium fluoroaluminate, and its molecular formula is Na
3AIF
6, natural cryolite is monoclinic prismatic crystallization, and is colourless, because the influence of impurity often is canescence, faint yellow or incarnadine, is black sometimes.The indivisible compact block of normal one-tenth has vitreous luster.Be slightly soluble in water, react acid, meet sulfuric acid and promptly decompose.As a kind of Chemicals, be mainly used in the fusing assistant of metal smelting aluminium, also can make the sterilant of farm crop, the enamel opacifier, the opalizer and the fusing assistant of glass and enamel production usefulness, the wear-resistant filler of resin rubber also can be used for the production of iron alloy and rimming steel.Along with the fast development of aluminium industry, its potential market share progressively increases, and is also more and more higher to the requirement of quality.
In the Aluminum Electrolysis Production process, for guaranteeing normal production, must make the electrolytic solution in the electrolyzer keep reasonably height and cleanliness factor, therefore need to extract and salvage too much electrolytic solution out swim in electrolytic solution top solid, these solids are just becoming fluorine-containing waste residue through after the condensation.Fluorine-containing waste residue according to 10.2 kilograms of one ton of aluminium meeting of measuring and calculating production outputs wherein contains the sodium aluminum fluoride more than 30%, 60%～70% breeze.For these fluorine-containing waste residue, at present by simple purification processes, do not reach the standard that is used for electrolytic aluminum of returning, the mode that can only take to pile up is handled, and has both caused environmental pollution, has wasted the fluorine resource again.
Summary of the invention
The purpose of this invention is to provide a kind of electrolytic aluminium containing waste slag of fluorine and produce the method for sodium aluminum fluoride.This method is to be raw material with the electrolytic aluminium containing waste slag of fluorine and the vitriol oil, may further comprise the steps:
(1) be that 98% the vitriol oil reacted 5～12 hours under 150 ℃～450 ℃ temperature with fluorine-containing waste residue and 1～4 times of concentration of its quality;
(2) gas that generates in the reaction process is treated, recycle;
(3) reacted solid sodium sulfate and Tai-Ace S 150 and concentration be 20%～40% hydrofluoric acid at 20 ℃～40 ℃ following stirring reaction 0.3～1.5h, make cryolite slurry;
(4) with above-mentioned slurry filtration, filter cake washing, drying promptly get the high purity sodium aluminum fluoride; Gained filtrate and washing water are collected respectively, and circulation is used to absorb sulphur trioxide and hydrogen fluoride.
The treatment process of the gas that generates in the reaction process is:
(1) sulfurous gas that generates in the reaction process, carbonic acid gas, hydrogen fluoride gas are through condenser condenses;
(2) after condensation finishes, the hydrogen fluoride liquid of condenser through absorb to concentration be 20%～40%, be used for subsequent reactions;
(3) sulfurous gas, the carbon dioxide that come out of condenser top isolated the carbonic acid gas more than 90% by dry purification equipment (tornado dust collector, electrostatic precipitator);
(4) sulfur dioxide gas that will isolate carbonic acid gas purifies through the wet purification system; After purifying end, sulfurous gas enters in the convertor, carries out catalytic oxidation in the presence of vanadium catalyst, is converted into sulphur trioxide, concentrates after absorbing again, makes the vitriol oil, is used for the circular treatment waste residue;
(5) separate the carbon dioxide that obtains and after purifying, get the technical grade carbonic acid gas.
Hydrogen fluoride liquid water in the first set reaction absorbs, and absorbs with washing water in the circulating reaction; After Sulphur Dioxide was sulphur trioxide, water absorbed in the first set reaction, absorbs with filtrate in the circulating reaction.
Reaction equation of the present invention is as follows:
Reaction 1:H
2SO
4+ 2C=CO
2+ 2SO
2+ 2H
2O;
6H
2SO
4+2Na
3AlF
6=?3Na
2SO
4?+Al
2(SO
4)
3+12HF
Reaction 2:3Na
2SO
4+ Al
2(SO
4)
3+ 12HF=6H
2SO
4+ 2Na
3AlF
6
Method advantage provided by the present invention is: (1) is the high-purity sodium aluminum fluoride of raw material production with the waste slag of electrolytic aluminium of cheapness, and production cost is low, remarkable in economical benefits; (2) sodium aluminum fluoride that the inventive method is produced, its quality is better than national standard, can return aluminum electrolysis industry and continue to use; (3) sulfur dioxide gas that produces in the reaction becomes the sulfuric acid circulation to be used to handle waste residue through purifying, transform post-absorption, reduces cost; (4) the present invention is converted into carbonic acid gas with the carbon in the fluorine-containing carbon slag, has both carried out the trans-utilization of carbon, has carried out the fluorine resource circulation utilization again simultaneously, has followed " 3R " principle of recycling economy; (5) the present invention produces " three wastes " all recycles, does not produce secondary pollution, and environmental benefit is remarkable; (6) the invention solves the bottleneck that the restriction aluminum electrolysis industry develops, impel its sound development.
Description of drawings
Fig. 1 produces the sodium aluminum fluoride process flow sheet for utilizing the vitriol oil and electrolytic aluminium containing waste slag of fluorine.
Embodiment
Embodiment 1
The method that present embodiment utilizes the fluorine-containing waste residue of the vitriol oil and electrolytic aluminum to produce sodium aluminum fluoride may further comprise the steps:
(1) with fluorine-containing waste residue and 4 times of concentration of its quality is 98% the vitriol oil, under 450 ℃ temperature, reacts 5h;
(2) sulfurous gas that generates in the reaction process, carbonic acid gas, hydrogen fluoride gas are through condenser condenses (boiling point of HF is 19.54 ℃);
(3) after condensation finishes, the hydrogen fluoride liquid of condenser add water absorb to concentration be 40%, be used for subsequent reactions;
(4) sulfurous gas, the carbon dioxide that come out of condenser top isolated 90% carbonic acid gas by dry purification equipment tornado dust collector;
(5) sulfur dioxide gas that will isolate carbonic acid gas purifies through the wet purification system; Purify end back sulfurous gas and enter in the convertor, in the presence of vanadium catalyst, carry out catalytic oxidation, be converted into sulphur trioxide, after water absorbs, concentrate again, make the vitriol oil, be used for the circular treatment waste residue;
(6) separate the carbon dioxide that obtains and after purifying, get the technical grade carbonic acid gas;
(7) reacted solid sodium sulfate and Tai-Ace S 150 and concentration be 40% hydrofluoric acid at 20 ℃ of following stirring reaction 1h, make cryolite slurry;
(8) with above-mentioned slurry filtration, filter cake washing, drying promptly get high-purity sodium aluminum fluoride; Filtrate and washing water are collected respectively, and circulation is used to absorb sulphur trioxide and hydrogen fluoride.
Embodiment 2
The method that present embodiment utilizes the fluorine-containing waste residue of the vitriol oil and electrolytic aluminum to produce sodium aluminum fluoride may further comprise the steps:
(1) with fluorine-containing waste residue and 3 times of concentration of its quality 98% the vitriol oil at 250 ℃ of reaction 8h down;
(2) sulfurous gas that generates in the reaction process, carbonic acid gas, hydrogen fluoride gas are through condenser condenses (boiling point of HF is 19.54 ℃);
(3) after condensation finishes, the hydrogen fluoride liquid of condenser add washing water absorb to concentration be 30%, be used for subsequent reactions;
(4) sulfurous gas, the carbon dioxide that come out of condenser top isolated 90% carbonic acid gas by dry purification equipment electrostatic precipitator;
(5) sulfur dioxide gas that will isolate carbonic acid gas purifies through the wet purification system; Purify end back sulfurous gas and enter in the convertor, in the presence of vanadium catalyst, carry out catalytic oxidation, be converted into sulphur trioxide, after filtrate absorbs, concentrate again, make the vitriol oil, be used for the circular treatment waste residue;
(6) separate the carbon dioxide that obtains and after purifying, get the technical grade carbonic acid gas;
(7) reacted solid sodium sulfate and Tai-Ace S 150 and concentration be 30% hydrofluoric acid at 25 ℃ of following stirring reaction 0.5h, make cryolite slurry;
(8) with above-mentioned slurry filtration, filter cake washing, drying promptly get high-purity sodium aluminum fluoride; Filtrate and washing water are collected respectively, and circulation is used to absorb sulphur trioxide and hydrogen fluoride.
Embodiment 3
The method that present embodiment utilizes the fluorine-containing waste residue of the vitriol oil and electrolytic aluminum to produce sodium aluminum fluoride may further comprise the steps:
(1) be that 98% the vitriol oil reacts 12h with fluorine-containing waste residue and 2 times of concentration of its quality under 150 ℃ temperature;
(2) sulfurous gas that generates in the reaction process, carbonic acid gas, hydrogen fluoride gas are through condenser condenses (boiling point of HF is 19.54 ℃);
(3) after condensation finishes, the hydrogen fluoride liquid of condenser add washing water absorb to concentration be 25%, be used for subsequent reactions;
(4) sulfurous gas, the carbon dioxide that come out of condenser top isolated 90% carbonic acid gas by dry purification equipment tornado dust collector;
(5) sulfur dioxide gas that will isolate carbonic acid gas purifies through the wet purification system; Purify end back sulfurous gas and enter in the convertor, in the presence of vanadium catalyst, carry out catalytic oxidation, be converted into sulphur trioxide, after filtrate absorbs, concentrate again, make the vitriol oil, be used for the circular treatment waste residue;
(6) separate the carbon dioxide that obtains and after purifying, get the technical grade carbonic acid gas;
(7) reacted solid sodium sulfate and Tai-Ace S 150 and concentration be 25% hydrofluoric acid at 40 ℃ of following stirring reaction 1.5h, make cryolite slurry;
(8) with above-mentioned slurry filtration, filter cake washing, drying promptly get high-purity sodium aluminum fluoride; Filtrate and washing water are collected respectively, and circulation is used to absorb sulphur trioxide and hydrogen fluoride.
The mass analysis result of the sodium aluminum fluoride that table 1 embodiment 1～3 produces
Claims (7)
1. the method that electrolytic aluminium containing waste slag of fluorine is produced sodium aluminum fluoride is characterized in that, is raw material with the electrolytic aluminium containing waste slag of fluorine and the vitriol oil, may further comprise the steps:
(1) be that 98% the vitriol oil reacted 5～12 hours under 150 ℃～450 ℃ temperature with fluorine-containing waste residue and 1～4 times of concentration of its quality;
(2) gas that generates in the reaction process is treated, recycle;
(3) reacted solid sodium sulfate and Tai-Ace S 150 and concentration be 20%～40% hydrofluoric acid at 20 ℃～40 ℃ following stirring reaction 0.3～1.5h, make cryolite slurry;
(4) with above-mentioned slurry filtration, filter cake washing, drying promptly get the high purity sodium aluminum fluoride; Gained filtrate and washing water are collected respectively, and circulation is used to absorb sulphur trioxide and hydrogen fluoride.
2. electrolytic aluminium containing waste slag of fluorine according to claim 1 is produced the method for sodium aluminum fluoride, it is characterized in that, the sulfurous gas that generates in step (2) reaction, carbonic acid gas, hydrogen fluoride gas are through condenser condenses; The hydrogen fluoride liquid of condenser again through absorb to concentration be 20%～40%, be used for subsequent reactions.
3. electrolytic aluminium containing waste slag of fluorine according to claim 2 is produced the method for sodium aluminum fluoride, it is characterized in that, and the absorption of hydrogen fluoride liquid, water absorbs in the first set reaction, absorbs with washing water in the circulating reaction.
4. electrolytic aluminium containing waste slag of fluorine according to claim 2 is produced the method for sodium aluminum fluoride, it is characterized in that the sulfurous gas that comes out in condenser top, carbon dioxide gas mixture go out 90% carbonic acid gas by the dry purification device separates; Carbonic acid gas gets the technical grade carbonic acid gas after purifying.
5. electrolytic aluminium containing waste slag of fluorine according to claim 4 is produced the method for sodium aluminum fluoride, it is characterized in that, the sulfur dioxide gas of isolating carbonic acid gas is purified through the wet purification system; Purify end back sulfurous gas and enter in the convertor, in the presence of vanadium catalyst, carry out catalytic oxidation, be converted into sulphur trioxide, after absorbing, concentrate again, make the vitriol oil, be used for the circular treatment waste residue.
6. electrolytic aluminium containing waste slag of fluorine according to claim 4 is produced the method for sodium aluminum fluoride, it is characterized in that described dry purification equipment is tornado dust collector, electrostatic precipitator.
7. electrolytic aluminium containing waste slag of fluorine according to claim 5 is produced the method for sodium aluminum fluoride, it is characterized in that, and the absorption of sulphur trioxide, water absorbs in the first set reaction, absorbs with filtrate in the circulating reaction.
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| CN201010591904A CN102079534B (en) | 2010-12-16 | 2010-12-16 | Method for producing cryolite by using fluorine-containing waste residues of electrolytic aluminium |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293536A (en) * | 2015-12-01 | 2016-02-03 | 多氟多化工股份有限公司 | Method of extracting lithium from electrolytic aluminium waste residues |
| CN105502452A (en) * | 2015-12-08 | 2016-04-20 | 北京京碧蓝环保科技有限公司 | Method for recovering cryolite and carrying out tail gas treatment during heat treatment of waste aluminum electrolysis bath liners |
| RU2643675C1 (en) * | 2016-12-16 | 2018-02-05 | федеральное государственное бюджетное образовательное учреждение высшего образования "Иркутский национальный исследовательский технический университет" (ФГБОУ ВО "ИРНИТУ") | Method for processing spent thermal insulation lining of aluminium electrolyser |
| CN108941167A (en) * | 2018-08-01 | 2018-12-07 | 湘潭大学 | Mechanochemistry conversion and recovery method in a kind of waste cathode of aluminum electrolytic cell carbon block containing sodium, fluorochemical |
| CN109437271A (en) * | 2018-12-10 | 2019-03-08 | 湖南绿脉环保科技有限公司 | A method of recycling electrolytic aluminium fluorine-containing resource |
| CN109721090A (en) * | 2019-03-06 | 2019-05-07 | 山东聚科源铝业科技有限公司 | A method of reducing ice crystal molecular proportion |
| CN114031099A (en) * | 2021-11-19 | 2022-02-11 | 东北大学 | Acidification roasting method for efficiently treating aluminum electrolysis solid waste |
| CN114797449A (en) * | 2022-04-13 | 2022-07-29 | 中南大学 | Based on theta-Al 2 O 3 Catalyst for high-efficiency catalytic decomposition of CF in electrolytic aluminum flue gas 4 And HF by-product resource recovery method |
| CN115156238A (en) * | 2022-07-12 | 2022-10-11 | 华南理工大学 | Comprehensive recycling method for aluminum electrolysis waste cathode carbon blocks and application thereof |
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| US4355017A (en) * | 1981-05-14 | 1982-10-19 | Martin Marietta Corporation | Aluminum electrolytic cell cathode waste recovery |
| CN101239731A (en) * | 2008-03-11 | 2008-08-13 | 中南大学 | Method for producing cryolite from aluminum electrolysis waste slag |
| CN101734701A (en) * | 2009-12-30 | 2010-06-16 | 朱彦青 | Method for producing cryolite by using fluorine-containing slag of electrolytic aluminum |
-
2010
- 2010-12-16 CN CN201010591904A patent/CN102079534B/en active Active
Patent Citations (3)
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| US4355017A (en) * | 1981-05-14 | 1982-10-19 | Martin Marietta Corporation | Aluminum electrolytic cell cathode waste recovery |
| CN101239731A (en) * | 2008-03-11 | 2008-08-13 | 中南大学 | Method for producing cryolite from aluminum electrolysis waste slag |
| CN101734701A (en) * | 2009-12-30 | 2010-06-16 | 朱彦青 | Method for producing cryolite by using fluorine-containing slag of electrolytic aluminum |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293536A (en) * | 2015-12-01 | 2016-02-03 | 多氟多化工股份有限公司 | Method of extracting lithium from electrolytic aluminium waste residues |
| CN105502452A (en) * | 2015-12-08 | 2016-04-20 | 北京京碧蓝环保科技有限公司 | Method for recovering cryolite and carrying out tail gas treatment during heat treatment of waste aluminum electrolysis bath liners |
| CN105502452B (en) * | 2015-12-08 | 2017-11-24 | 北京京碧蓝环保科技有限公司 | Ice crystal is reclaimed in aluminium electroloysis waste lining heat treatment process to go forward side by side the method for end of line gas disposal |
| RU2643675C1 (en) * | 2016-12-16 | 2018-02-05 | федеральное государственное бюджетное образовательное учреждение высшего образования "Иркутский национальный исследовательский технический университет" (ФГБОУ ВО "ИРНИТУ") | Method for processing spent thermal insulation lining of aluminium electrolyser |
| CN108941167B9 (en) * | 2018-08-01 | 2021-04-09 | 湘潭大学 | Mechanochemical conversion and recovery method of sodium-containing and fluorine-containing compounds in waste cathode carbon blocks of aluminum electrolytic cell |
| CN108941167B (en) * | 2018-08-01 | 2021-01-22 | 湘潭大学 | Mechanochemical conversion and recovery method of sodium-containing and fluorine-containing compounds in waste cathode carbon blocks of aluminum electrolytic cell |
| CN108941167A (en) * | 2018-08-01 | 2018-12-07 | 湘潭大学 | Mechanochemistry conversion and recovery method in a kind of waste cathode of aluminum electrolytic cell carbon block containing sodium, fluorochemical |
| CN109437271A (en) * | 2018-12-10 | 2019-03-08 | 湖南绿脉环保科技有限公司 | A method of recycling electrolytic aluminium fluorine-containing resource |
| CN109437271B (en) * | 2018-12-10 | 2021-11-23 | 湖南绿脉环保科技股份有限公司 | Method for recycling fluorine-containing resources of electrolytic aluminum |
| CN109721090A (en) * | 2019-03-06 | 2019-05-07 | 山东聚科源铝业科技有限公司 | A method of reducing ice crystal molecular proportion |
| CN109721090B (en) * | 2019-03-06 | 2021-03-23 | 山东绿脉铝业科技有限公司 | Method for reducing cryolite molecular ratio |
| CN114031099A (en) * | 2021-11-19 | 2022-02-11 | 东北大学 | Acidification roasting method for efficiently treating aluminum electrolysis solid waste |
| CN114797449A (en) * | 2022-04-13 | 2022-07-29 | 中南大学 | Based on theta-Al 2 O 3 Catalyst for high-efficiency catalytic decomposition of CF in electrolytic aluminum flue gas 4 And HF by-product resource recovery method |
| CN115156238A (en) * | 2022-07-12 | 2022-10-11 | 华南理工大学 | Comprehensive recycling method for aluminum electrolysis waste cathode carbon blocks and application thereof |
| CN115156238B (en) * | 2022-07-12 | 2023-05-30 | 华南理工大学 | Comprehensive recycling method for aluminum electrolysis waste cathode carbon blocks and application thereof |
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| CN102079534B (en) | 2012-09-26 |
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Effective date of registration: 20160118 Address after: 730621 No. 850 East Main Street, Jingyuan County, Gansu, Baiyin Patentee after: Baiyin Zhongtian Chemical Co., Ltd. Address before: The station area 454191 Henan province Jiaozuo City West Feng Feng Industrial Zone Patentee before: Duo-fluoride Chemicals Co., Ltd. |