CN101565775A - Method for recovering medium-concentration and low-concentration vanadium in industrial sewage resulted from stone coal vanadium extraction - Google Patents
Method for recovering medium-concentration and low-concentration vanadium in industrial sewage resulted from stone coal vanadium extraction Download PDFInfo
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- CN101565775A CN101565775A CNA2009100941004A CN200910094100A CN101565775A CN 101565775 A CN101565775 A CN 101565775A CN A2009100941004 A CNA2009100941004 A CN A2009100941004A CN 200910094100 A CN200910094100 A CN 200910094100A CN 101565775 A CN101565775 A CN 101565775A
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- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 85
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000000605 extraction Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000003245 coal Substances 0.000 title claims abstract description 27
- 239000004575 stone Substances 0.000 title claims abstract description 25
- 239000010865 sewage Substances 0.000 title abstract 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- IDOQDZANRZQBTP-UHFFFAOYSA-N 2-[2-(2,4,4-trimethylpentan-2-yl)phenoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=CC=C1OCCO IDOQDZANRZQBTP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920004929 Triton X-114 Polymers 0.000 claims abstract description 6
- 239000002351 wastewater Substances 0.000 claims description 27
- 239000013543 active substance Substances 0.000 claims description 26
- 229910001456 vanadium ion Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000693 micelle Substances 0.000 claims description 14
- 238000011084 recovery Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 235000011149 sulphuric acid Nutrition 0.000 claims description 12
- 239000001117 sulphuric acid Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 5
- 235000010265 sodium sulphite Nutrition 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004513 sizing Methods 0.000 claims description 2
- ANFIEGWCRSNVFS-UHFFFAOYSA-N [Na].OCl(=O)=O Chemical compound [Na].OCl(=O)=O ANFIEGWCRSNVFS-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000002736 nonionic surfactant Substances 0.000 abstract 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 230000002209 hydrophobic effect Effects 0.000 abstract 1
- 230000003165 hydrotropic effect Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention relates to a new method for recovering medium-concentration and low-concentration vanadium in industrial sewage resulted from stone coal vanadium extraction, belonging to the technical field of metallurgy and engineering chemistry. The method comprises the steps of oxidization, pH value adjustment, extraction of non-ionic surfactant Triton X-114, back extraction of sulfuric acid solution, and the like. The method is mainly and technically characterized in that the non-ionic surfactant Triton X-114 is used for extraction, the cloud point phenomenon of the surfactant is taken as the basis, hydrophobic substances are separated from hydrotropic substances by changing technical parameters (such as pH value of the solution, temperature, and the like), the vanadium in the sewage can be effectively recovered, and the surfactant after the back extraction can be cyclically used. The method has the advantages of small use amount of reagent, fast extraction and separation, low cost, no secondary pollution, and the like, and can be widely used for treating vanadium-containing industrial sewage.
Description
Technical field
The invention belongs to the chemical metallurgy technical field, in particular, relate to the recovery method of lower concentration vanadium in a kind of extracting vanadium from stone coal trade effluent.
Background technology
Bone coal acidleach wet method process for extracting vanadium adopts the vanadium in the sulphuric acid soln leaching bone coal, contains the vanadic acid leach liquor after purifying, neutralize, extracting, and produces the waste water that contains the lower concentration vanadium in a large number.As an acidleach-extraction wet method vanadium extraction factory that produces 1200 tons per year, the annual waste water about 3.2 * 10 that contains the lower concentration vanadium of discharging
6m
3If these waste water directly discharge, both serious environment pollution was wasted a large amount of callable vanadium resources again.Along with the progressively expansion of vanadium industry, vanadium-containing water flows into underground water more, enters human body with food and water behind the pollution animals and plants, influences human health.
The side that handles vanadium-containing water mostly adopts absorption method, chemical precipitation method and ion exchange method at present, wherein mainly comprises iron filings (or ferrous sulfate) precipitator method, the sulfurous gas precipitator method and ion exchange method.Though absorption method can reclaim the vanadium in the waste water, but still there are shortcomings such as treatment effect is undesirable, running cost height; Chemical precipitation method is necessarily used on engineering at present, but this kind method of wastewater treatment easily produces the phenomenon of corrosion and passivation, thereby influences the stability of purifying water effect.There is the treatment effect instability when this method is handled the high density vanadium-containing water in addition, causes secondary pollution, the working cost height, the vanadium in the waste water can not obtain effective recycling etc.; Though the recyclable vanadium of ion-exchange, treatment effect is also more stable, and its shortcoming is the ion exchange resin large usage quantity, and regeneration is frequent, and processing cost is higher.
Summary of the invention
The objective of the invention is to overcome the existing shortcoming and defect that contains the vanadium technology for treating industrial waste water, a kind of efficient height is provided, the method for non-secondary pollution, easy to operate processing vanadium-containing water.
Realize that the technical scheme that above-mentioned purpose of the present invention is taked is:
Make extraction agent with nonionogenic tenside Triton X-114, sulphuric acid soln is made strippant, extracts more than the solution cloud point temperature and strips, and it comprises the steps:
(1) adopt oxygenant that the tetravalent vanadium ion in the solution is oxidized to pentavalent vanadium ion;
(2) adopt neutralizing agent that the resulting waste water of step (1) is adjusted to the required pH value of extracting vanadium ion;
(3) add nonionogenic tenside Triton X-114 in the solution that step (2) obtains, heating in water bath extracts, with the vanadium ion in the waste water be enriched in the tensio-active agent micelle mutually in;
(4) do reverse-extraction agent with sulphuric acid soln, the tensio-active agent micelle that obtains with step (3) mixes, heating in water bath once more, strip, obtain containing vanadium enrichment liquid and tensio-active agent mutually, contain vanadium enrichment liquid and return extracting vanadium from stone coal and leach the operation of sizing mixing, tensio-active agent can return as the extraction agent recycle.
Concrete processing parameter of the present invention is as follows:
(1) optimum range of neutralizing agent adjusting waste water ph is 3.0~6.5;
(2) Cui Qu tensio-active agent volume integral number is 3%~10% of a wastewater volume.The temperature of extraction is 45 ℃~90 ℃, centrifugal while hot phase-splitting 10min~25min after the extraction;
(3) during back extraction, the shared massfraction of reverse-extraction agent sulphuric acid soln is 5%~15%, and the temperature of reextraction is 45 ℃~90 ℃, centrifugal while hot phase-splitting 10min~25min after the reextraction.
In being suitable for extracting vanadium from stone coal trade effluent of the present invention, vanadium ion concentration is 1.0~50.0mg/L, and waste water ph is 0.5~3.0.
The above-mentioned used oxygenant of adjusting waste water of the present invention can adopt any of sodium chlorate, clorox or sodium sulphite, and the add-on of sodium chlorate, clorox or sodium sulphite is respectively 35%~45%, 30%~40% or 20%~30% of vanadium quality in the waste water.
The present invention adopts a kind of environment-friendly type liquid-liquid technique, does not use volatile organic solvent, does not influence environment.It is based on the cloud point phenomenon of tensio-active agent, by changing experiment parameter (as the pH value of solution, temperature etc.) lyophobic dust is separated with hydroaropic substance, and the vanadium in the energy efficient recovery waste water, the extracting and enriching rate reaches as high as 100%.And operating between two waters of extraction and separation technology of the present invention carried out, and avoids using harmful organic solvent, also avoided the pollution of volatile organic solvent to environment.It has advantages such as economy, safe, efficient, easy and simple to handle and applied range.
Adopt the effectively vanadium of lower concentration in the enrichment extracting vanadium from stone coal trade effluent of extraction and separation technology of the present invention, not only reduce vanadium ion concentration in the waste water, alleviate environmental pollution, the vanadium resource in again can comprehensive reutilization waste water.
Advantage of the present invention:
1. the invention provides a kind of method that reclaims lower concentration vanadium in the extracting vanadium from stone coal trade effluent, present method rate of recovery height, technology is simple, and dosage of surfactant is little, and extracting and separating speed is fast.
2. the concentration of vanadium ion reduces greatly in the waste water of extraction back, alleviates environmental pollution.
3. liquid-liquid technique of the present invention does not use volatile organic solvent, does not influence environment, non-secondary pollution, environmental friendliness.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment technology contents of the present invention is further elaborated.
Example one
Getting vanadium ion concentration is the extracting vanadium from stone coal waste water 100ml of 1mg/L, adds the 0.05mg sodium chlorate low price vanadium in the solution is oxidized to the pentavalent vanadium.Adopting massfraction is that 18~25% ammoniacal liquor regulator solution pH value is 3.0, and adding 3mlTritonX-114 places 45 ℃ of water-baths to heat 10min, it is fully dissolved after.While hot with the centrifugal phase-splitting 10min of whizzer, the micelle that vanadium ion is enriched in tensio-active agent mutually in.Add massfraction in the tensio-active agent micelle that comes out and be 10% sulphuric acid soln 5ml after phase-splitting, heating in water bath to 45 ℃ fully dissolves it once more.Centrifugal while hot phase-splitting 10min.The rate of recovery of vanadium is 91.6%.Back extraction obtains contains vanadium enrichment liquid and can return extracting vanadium from stone coal and leach operation, isolated tensio-active agent reusable edible.
Example two
Get the extracting vanadium from stone coal waste water 100ml that contains vanadium 5mg/L, add the 0.17mg sodium chlorate low price vanadium in the solution is oxidized to the pentavalent vanadium.Adopting massfraction is that 18~25% regulator solution pH values are 3.0, and adding 4mlTritonX-114 places 50 ℃ of water-baths to heat 15min, it is fully dissolved after.While hot with the centrifugal phase-splitting 15min of whizzer, the micelle that vanadium ion is enriched in tensio-active agent mutually in.Add massfraction in the tensio-active agent micelle that comes out and be 10% sulphuric acid soln 5ml after phase-splitting, heating in water bath to 50 ℃ fully dissolves it once more.Centrifugal while hot phase-splitting 15min.The rate of recovery of vanadium is 82.1%.Back extraction obtains contains vanadium enrichment liquid and can return extracting vanadium from stone coal and leach operation, isolated tensio-active agent reusable edible.
Example three
Get the extracting vanadium from stone coal waste water 100ml that contains vanadium 10mg/L, add the 0.40mg clorox low price vanadium in the solution is oxidized to the pentavalent vanadium.Adopting massfraction is that 18~25% ammoniacal liquor regulator solution pH values are 3.5, and adding 5ml TritonX-114 places 60 ℃ of water-baths to heat 20min, it is fully dissolved after.While hot with the centrifugal phase-splitting 15min of whizzer, the micelle that vanadium ion is enriched in tensio-active agent mutually in.Add massfraction in the tensio-active agent micelle that comes out and be 10% sulphuric acid soln 5ml after phase-splitting, heating in water bath to 60 ℃ fully dissolves it once more.Centrifugal while hot phase-splitting 15min.The rate of recovery of vanadium is 76.1.3%.Back extraction obtains contains vanadium enrichment liquid and can return extracting vanadium from stone coal and leach operation, isolated tensio-active agent reusable edible.
Example four
Get the extracting vanadium from stone coal waste water 100ml that contains vanadium 20mg/L, add the 0.60mg clorox low price vanadium in the solution is oxidized to the pentavalent vanadium.Adopting massfraction is that 18~25% ammoniacal liquor regulator solution pH values are 4.0, and adding 6ml TritonX-114 places 70 ℃ of water-baths to heat 25min, it is fully dissolved after.While hot with the centrifugal phase-splitting 20min of whizzer, the micelle that vanadium ion is enriched in tensio-active agent mutually in.Add massfraction in the tensio-active agent micelle that comes out and be 15% sulphuric acid soln 6ml after phase-splitting, heating in water bath to 70 ℃ fully dissolves it once more.Centrifugal while hot phase-splitting 20min.The rate of recovery of vanadium is 65.2%.Back extraction obtains contains vanadium enrichment liquid and can return extracting vanadium from stone coal and leach operation, isolated tensio-active agent reusable edible.
Example five
Get the extracting vanadium from stone coal waste water 100ml that contains vanadium 50mg/L, add 1.25mg sodium sulphite the low price vanadium in the solution is oxidized to the pentavalent vanadium.Adopting massfraction is that 18~25% ammoniacal liquor regulator solution pH values are 6.5, and adding 10ml TritonX-114 places 90 ℃ of water-baths to heat 30min, it is fully dissolved after.While hot with the centrifugal phase-splitting 25min of whizzer, the micelle that vanadium ion is enriched in tensio-active agent mutually in.Add massfraction in the tensio-active agent micelle that comes out and be 15% sulphuric acid soln 10ml after phase-splitting, heating in water bath to 90 ℃ fully dissolves it once more.Centrifugal while hot phase-splitting 25min.The rate of recovery of vanadium is 61.0%.Back extraction obtains contains vanadium enrichment liquid and can return extracting vanadium from stone coal and leach operation, isolated tensio-active agent reusable edible.
Claims (5)
1. the recovery method of lower concentration vanadium in the extracting vanadium from stone coal trade effluent, it is characterized in that: make extraction agent with nonionogenic tenside Triton X-114, sulphuric acid soln is made strippant, extracts more than the solution cloud point temperature and strips, and it comprises the steps:
(1) adopt oxygenant that the tetravalent vanadium ion in the solution is oxidized to pentavalent vanadium ion;
(2) adopt neutralizing agent that the resulting waste water of step (1) is adjusted to the required pH value of extracting vanadium ion;
(3) add nonionogenic tenside Triton X-114 in the solution that step (2) obtains, heating in water bath extracts, with the vanadium ion in the waste water be enriched in the tensio-active agent micelle mutually in;
(4) do reverse-extraction agent with sulphuric acid soln, the tensio-active agent micelle that obtains with step (3) mixes, heating in water bath once more, strip, obtain containing vanadium enrichment liquid and tensio-active agent mutually, contain vanadium enrichment liquid and return extracting vanadium from stone coal and leach the operation of sizing mixing, tensio-active agent can return as the extraction agent recycle.
2. the recovery method of lower concentration vanadium in the extracting vanadium from stone coal trade effluent according to claim 1 is characterized in that:
(1) optimum range of neutralizing agent adjusting waste water ph is 3.0~6.5;
(2) Cui Qu tensio-active agent volume integral number is 3%~10% of a wastewater volume.The temperature of extraction is 45 ℃~90 ℃, centrifugal while hot phase-splitting 10min~25min after the extraction;
(3) during back extraction, the shared massfraction of reverse-extraction agent sulphuric acid soln is 5%~15%, and the temperature of reextraction is 45 ℃~90 ℃, centrifugal while hot phase-splitting 10min~25min after the reextraction.
3. the recovery method of lower concentration vanadium in the extracting vanadium from stone coal trade effluent according to claim 2 is characterized in that: the vanadium ion concentration in the extracting vanadium from stone coal trade effluent is 1.0~50.0mg/L, and waste water ph is 0.5~3.0.
4. the recovery method of lower concentration vanadium in a kind of extracting vanadium from stone coal trade effluent according to claim 2 is characterized in that: oxygenant adopts any of sodium chlorate, clorox or sodium sulphite.
5. the recovery method of lower concentration vanadium in the extracting vanadium from stone coal trade effluent according to claim 4, it is characterized in that: the add-on of oxygenant chloric acid sodium, clorox or sodium sulphite is respectively 35%~45%, 30%~40% or 20%~30% of vanadium quality in the waste water.
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Cited By (7)
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CN103555962A (en) * | 2013-10-23 | 2014-02-05 | 北京矿冶研究总院 | Method for comprehensively recovering selenium, vanadium and silver from vanadium-silver-selenium polymetallic ore by wet method |
CN106282607A (en) * | 2016-08-30 | 2017-01-04 | 陕西福盛钒业科技有限公司 | One utilizes V5+the extracting and enriching method containing vanadium solution |
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CN111020193A (en) * | 2019-11-06 | 2020-04-17 | 北京华电光大环境股份有限公司 | Method for recovering vanadium, tungsten and titanium elements from waste SCR denitration catalyst |
CN111020193B (en) * | 2019-11-06 | 2022-05-03 | 北京华电光大环境股份有限公司 | Method for recovering vanadium, tungsten and titanium elements from waste SCR denitration catalyst |
CN112575207A (en) * | 2020-12-04 | 2021-03-30 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide by low-concentration acidic vanadium liquid extraction |
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