CN102838233A - Method for recycling acidic vanadium deposit wastewater - Google Patents
Method for recycling acidic vanadium deposit wastewater Download PDFInfo
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- CN102838233A CN102838233A CN2012103341850A CN201210334185A CN102838233A CN 102838233 A CN102838233 A CN 102838233A CN 2012103341850 A CN2012103341850 A CN 2012103341850A CN 201210334185 A CN201210334185 A CN 201210334185A CN 102838233 A CN102838233 A CN 102838233A
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- decalcifying agent
- waste water
- vanadium
- acid
- acid waste
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Abstract
The invention provides a method for recycling acidic vanadium deposit wastewater. The method comprises the following steps: adjusting the acidic vanadium deposit wastewater to be alkaline by lime milk, then carrying out solid-liquid separation to obtain an alkaline solution and a gypsum residue; adding a decalcifying agent into the alkaline solution for decalcifying, then carrying out solid-liquid separation to obtain a supernatant liquor and a decalcified residue; and adjusting the pH of the supernatant liquor to be 3-7 by sulfuric acid, then returning the supernatant liquor to the leaching step for recycling. Due to the adoption of the method for recycling the acidic vanadium deposit wastewater, concentration of calcium ions in the solution returned to the leaching step can be effectively controlled, calcium sulfate deposit is prevented from being formed, a pipeline and a water outlet are prevented from being blocked due to calcium sulfate scale, and the production equipment is guaranteed to run normally.
Description
Technical field
The present invention relates to a kind of treatment process of vanadium wastewater, especially relate to a kind of treatment process of acid waste water for depositing vanadium recycle.
Background technology
The vanadium wastewater that industry is at present gone up producing for the raw material production vanadium oxide with the vanadium slag mainly contains two kinds of treatment processs:
A kind of is to be main flow technology with vanadium slag sodium roasting-water logging vanadium extraction, and the waste water that this technology produces generally adopts waste water reduction vanadium chromium-neutralization, filtration-evaporation concentration, and this technology is than maturation but cost for wastewater treatment is high;
Another kind is to be main flow with vanadium slag calcification baking-acid-leaching vanadium-extracted; The vanadium wastewater that this technology produces is returned leaching operation washing residue after adopting lime neutralization, filtration-adjusting pH at present, and this technology is fairly simple and cost is low, and is simultaneously effective; But; In returning the residual washing-out operation, occur calcium sulfate scaling easily, cause pipeline and washing water water outlet seriously to stop up, production unit can not normally be moved.
Summary of the invention
The objective of the invention is to overcome the deficiency of aforesaid method; A kind of acid waste water for depositing vanadium cyclic utilization method is provided; This method has effectively been controlled the calcium ion concn that returns in the solution that leaches operation, has avoided the pickling vanadium wastewater in the process of recycle, to produce calcium sulfate and the problem of blocking pipe and washing water water outlet.
In order to realize the foregoing invention purpose,, said method comprising the steps of according to acid waste water for depositing vanadium cyclic utilization method of the present invention:
Adopt milk of lime adjustment of acidity vanadium wastewater to alkalescence, carry out solid-liquid separation then, obtain basic soln and gypsum tailings; In said basic soln, add decalcifying agent and carry out decalcification, carry out solid-liquid separation then, obtain supernatant liquid and decalcification slag; With sulfuric acid the pH value of said supernatant liquid is adjusted to 3～7, then supernatant liquid is returned and leach operation and carry out recycle.
According to acid waste water for depositing vanadium cyclic utilization method of the present invention, the pH value of acid waste water for depositing vanadium is adjusted to 9～11 with milk of lime.
According to acid waste water for depositing vanadium cyclic utilization method of the present invention, in the said decalcification step, add decalcifying agent so that the Ca in the said basic soln
2+Concentration is reduced to below the 0.62g/L, and wherein, said decalcifying agent is volatile salt, bicarbonate of ammonia, oxalic acid, ammonium oxalate, hydrofluoric acid or Neutral ammonium fluoride, is preferably volatile salt or bicarbonate of ammonia; When said decalcifying agent is volatile salt or bicarbonate of ammonia, press the CO in the decalcifying agent
3 2-With the Ca in the said basic soln
2+And Mn
2+The mol ratio of sum is that 1.0～1.2 ratio is added said decalcifying agent; When said decalcifying agent is oxalic acid or ammonium oxalate, press the C in the decalcifying agent
2O
4 2-With the Ca in the said basic soln
2+Mol ratio be that 0.7～1.2 ratio is added said decalcifying agent; When decalcifying agent is hydrofluoric acid or Neutral ammonium fluoride, press the F in the decalcifying agent
-With the Ca in the said basic soln
2+And Mg
2+The mol ratio of sum is that 1.8～2.2 ratio is added said decalcifying agent; Said decalcification step stirs when in addition, also can comprise the adding decalcifying agent.
Embodiment
The invention provides a kind of acid waste water for depositing vanadium cyclic utilization method, may further comprise the steps:
Adopt milk of lime adjustment of acidity vanadium wastewater to alkalescence, carry out solid-liquid separation then, obtain basic soln and gypsum tailings; In said basic soln, add decalcifying agent and carry out decalcification, carry out solid-liquid separation then, obtain supernatant liquid and decalcification slag; With sulfuric acid the pH value of said supernatant liquid is adjusted to 3～7, then supernatant liquid is returned and leach operation and carry out recycle.
Carry out bright specifically to above-mentioned steps and description below in conjunction with principle of the present invention:
It is pointed out that pickling vanadium wastewater according to the invention is in the process of vanadium slag calcification baking process for extracting vanadium by acid leaching production vanadium oxide, to obtain, it mainly contains Fe
3+, Al
3+, Mg
2+, Mn
2+, SiO
3 2-, SO
4 2-, the P plasma; Said milk of lime is the saturated solution of calcium hydroxide, and the preparation of milk of lime is known in those skilled in the art, generally by water dissolution lime or quicklime and form.
At first, under condition of stirring, adopt pH value to 9～11 of milk of lime adjustment of acidity vanadium wastewater, can make Fe
3+, Al
3+, Mg
2+, Mn
2+Form corresponding precipitation of hydroxide, SiO
3 2-, SO
4 2-, P forms corresponding calcium precipitation; Carry out solid-liquid separation through methods commonly used such as filtrations; Impurity element is got in the gypsum tailings discharge circulating system, leach operation and carry out the concentration of impurity element in the supernatant liquid of recycle and be in lower level to guarantee to return.
Acid waste water for depositing vanadium is transferred pH through milk of lime, and the basic soln that obtains after the solid-liquid separation then is the saturated solution of calcium hydroxide, Ca
2+Pressure, Concentration, Temperature has relation, is generally 0.75～0.90g/L, after directly with sulfuric acid said basic soln being regulated the pH value, will return the leaching operation, so portion C a
2+Can crystallize out with the form of calcium sulfate, in the solution course of conveying, form calcium sulfate scaling blocking pipe and water outlet; For fear of the formation of calcium sulfate scaling, the present invention adds decalcifying agent so that the Ca in the basic soln before regulating pH with sulfuric acid
2+Concentration is reduced to below the 0.62g/L, promptly basic soln is carried out decalcification and handles, and avoiding forming the saturated solution of calcium sulfate, thereby avoids calcium sulfate scaling blocking pipe and water outlet; Here, for the reaction that makes the decalcification operation more is tending towards fully, can under stirring condition, carry out decalcification; Consider the effect of decalcification; Select for use volatile salt, bicarbonate of ammonia, oxalic acid, ammonium oxalate, hydrofluoric acid or Neutral ammonium fluoride as decalcifying agent, promptly can add wherein one or more, for easy to operate; General a kind of the getting final product that only adds wherein; Add when multiple, guarantee to add for a kind of anionic decalcifying agent solubility product difference can cause certain negatively charged ion ineffective when adding different anions because mix; Preferably adopting volatile salt or bicarbonate of ammonia is decalcifying agent.
When said decalcifying agent was volatile salt or bicarbonate of ammonia, because the solubility product of manganous carbonate is littler than lime carbonate, the deliming ionic also can be removed mn ion simultaneously, so press
Mol ratio is that 1.0～1.2 ratio is added said decalcifying agent, and promptly the add-on of decalcifying agent is according to the CO that contains in the decalcifying agent
3 2-, with the Ca that contains in the basic soln
2+And Mn
2+Mol ratio be that 1.0～1.2 ratio is added.
When said decalcifying agent was oxalic acid or ammonium oxalate, because the solubility product of caoxalate is all littler than the solubility product of manganous oxalate, magnesium oxalate, and calcium ion removed more than 50% and gets final product, so press C
2O
4 2-/ Ca
2+Mol ratio is that 0.7～1.2 ratio is added said decalcifying agent, and promptly the add-on of decalcifying agent is by the C that contains in the decalcifying agent
2O
4 2-With the Ca that contains in the basic soln
2+Mol ratio be that 0.7～1.2 ratio is added.
When decalcifying agent is hydrofluoric acid or Neutral ammonium fluoride; Because the solubility product of Calcium Fluoride (Fluorspan), Sellaite is more or less the same; But much smaller than manganous fluoride, so be that 1.8～2.2 ratio is added said decalcifying agent in
mol ratio.
At last; With sulfuric acid the pH value of said supernatant liquid is adjusted to 3～7; To satisfy the requirement of cleaning solution for removing residue in the extract technology, when adjust pH, the acid substitution sulfuric acid that does not adopt other is can bring the negatively charged ion that is difficult for removing into because of common hydrochloric acid, nitric acid etc.; Meeting enrichment in the water cycle process, and sulfate radical can be removed the balance of partly keeping sulfate radical in the solution in the milk of lime regulate process of next round; Behind the adjusting pH supernatant liquid is returned the leaching operation and carry out recycle.
Below in conjunction with embodiment the present invention is further described.
Embodiment 1
The 500mL acid waste water for depositing vanadium (is contained Ca
2+0.486g/L, Mn
2+8.32g/L, Mg
2+1.49g/L), under stirring condition, regulate pH value to 9 with milk of lime, carry out solid-liquid separation then, obtain gypsum tailings and the 492mL basic soln (contains Ca
2+0.772g/L, Mn
2+0.75g/L, Mg
2+0.51g/L); In the basic soln of gained, add the 1.70g volatile salt, leave standstill, filter out the decalcification slag behind the stirring 10min, obtain supernatant liquid (Ca
2+0.144g/L, Mn
2+0.08g/L, Mg
2+0.46g/L); With sulfuric acid the pH value of supernatant liquid is adjusted to 3.2, and leaves standstill, find not have deposition and produce, at last supernatant liquid is returned and leach operation and carry out recycle.
Embodiment 2
The 500mL acid waste water for depositing vanadium (is contained Ca
2+0.486g/L, Mn
2+8.32g/L, Mg
2+1.49g/L), under stirring condition, regulate pH value to 10 with milk of lime, carry out solid-liquid separation then, obtain gypsum tailings and the 495mL basic soln (contains Ca
2+0.847g/L, Mn
2+0.38g/L, Mg
2+0.34g/L); In the basic soln of gained, add 1.20g bicarbonate of ammonia, leave standstill, filter out the decalcification slag behind the stirring 10min, obtain supernatant liquid (Ca
2+0.152g/L, Mn
2+0.08g/L, Mg
2+0.31g/L); With sulfuric acid the pH value of supernatant liquid is adjusted to 4.5, and leaves standstill, find not have deposition and produce, at last supernatant liquid is returned and leach operation and carry out recycle.
Embodiment 3
The 500mL acid waste water for depositing vanadium (is contained Ca
2+0.486g/L, Mn
2+8.32g/L, Mg
2+1.49g/L), under stirring condition, regulate pH value to 11 with milk of lime, carry out solid-liquid separation then, obtain gypsum tailings and the 495mL basic soln (contains Ca
2+0.847g/L, Mn
2+0.38g/L, Mg
2+0.34g/L); In the basic soln of gained, add 1.00g oxalic acid, leave standstill, filter out the decalcification slag behind the stirring 10min, obtain supernatant liquid (Ca
2+0.092g/L, Mn
2+0.37g/L, Mg
2+0.30g/L); With sulfuric acid the pH value of supernatant liquid is adjusted to 6, and leaves standstill, find not have deposition and produce, at last supernatant liquid is returned and leach operation and carry out recycle.
Embodiment 4
The 500mL acid waste water for depositing vanadium (is contained Ca
2+0.486g/L, Mn
2+8.32g/L, Mg
2+1.49g/L), under stirring condition, regulate pH value to 9.5 with milk of lime, carry out solid-liquid separation then, obtain gypsum tailings and the 492mL basic soln (contains Ca
2+0.772g/L, Mn
2+0.75g/L, Mg
2+0.51g/L); In the basic soln of gained, add the 1.20g ammonium oxalate, leave standstill, filter out the decalcification slag behind the stirring 10min, obtain supernatant liquid (Ca
2+0.089g/L, Mn
2+0.73g/L, Mg
2+0.47g/L); With sulfuric acid the pH value of supernatant liquid is adjusted to 4, and leaves standstill, find not have deposition and produce, at last supernatant liquid is returned and leach operation and carry out recycle.
Embodiment 5
The 500mL acid waste water for depositing vanadium (is contained Ca
2+0.486g/L, Mn
2+8.32g/L, M
G2+1.49g/L), under stirring condition, regulate pH value to 10 with milk of lime, carry out solid-liquid separation then, obtain gypsum tailings and the 492mL basic soln (contains Ca
2+0.772g/L, Mn
2+0.75g/L, Mg
2+0.51g/L); In the basic soln of gained, add the 1.50g Neutral ammonium fluoride, leave standstill, filter out the decalcification slag behind the stirring 10min, obtain supernatant liquid (Ca
2+0.156g/L, Mn
2+0.69g/L, Mg
2+0.08g/L); With sulfuric acid the pH value of supernatant liquid is adjusted to 7, and leaves standstill, find not have deposition and produce, at last supernatant liquid is returned and leach operation and carry out recycle.
Embodiment 6
The 500mL acid waste water for depositing vanadium (is contained Ca
2+0.486g/L, Mn
2+8.32g/L, Mg
2+1.49g/L), under stirring condition, regulate pH value to 10.5 with milk of lime, carry out solid-liquid separation then, obtain gypsum tailings and the 495mL basic soln (contains Ca
2+0.847g/L, Mn
2+0.38g/L, Mg
2+0.34g/L); Adding quality percentage composition is 40% hydrofluoric acid 1.6mL in the basic soln of gained, leaves standstill, filters out the decalcification slag behind the stirring 10min, obtains supernatant liquid (Ca
2+0.152g/L, Mn
2+0.35g/L, Mg
2+0.08g/L); With sulfuric acid the pH value of supernatant liquid is adjusted to 5, and leaves standstill, find not have deposition and produce, at last supernatant liquid is returned and leach operation and carry out recycle.
In sum; Acid waste water for depositing vanadium cyclic utilization method of the present invention can effectively have been controlled the calcium ion concn that returns in the solution that leaches operation; Avoid the formation of calcium sulfate precipitation, prevent because calcium sulfate scaling blocking pipe and water outlet ensure the normal operation of production unit.
Claims (9)
1. an acid waste water for depositing vanadium cyclic utilization method is characterized in that, said working method may further comprise the steps:
Adopt milk of lime adjustment of acidity vanadium wastewater to alkalescence, carry out solid-liquid separation then, obtain basic soln and gypsum tailings;
In said basic soln, add decalcifying agent and carry out decalcification, carry out solid-liquid separation then, obtain supernatant liquid and decalcification slag;
With sulfuric acid the pH value of said supernatant liquid is adjusted to 3～7, then supernatant liquid is returned and leach operation and carry out recycle.
2. acid waste water for depositing vanadium cyclic utilization method as claimed in claim 1 is characterized in that, in the said decalcification step, adds decalcifying agent so that the Ca in the said basic soln
2+Concentration is reduced to below the 0.62g/L.
3. according to claim 1 or claim 2 acid waste water for depositing vanadium cyclic utilization method is characterized in that said decalcifying agent is volatile salt, bicarbonate of ammonia, oxalic acid, ammonium oxalate, hydrofluoric acid or Neutral ammonium fluoride.
4. acid waste water for depositing vanadium cyclic utilization method as claimed in claim 3 is characterized in that, said decalcifying agent is volatile salt or bicarbonate of ammonia.
5. acid waste water for depositing vanadium cyclic utilization method as claimed in claim 4 is characterized in that, presses the CO in the decalcifying agent
3 2-With the Ca in the said basic soln
2+And Mn
2+The mol ratio of sum is that 1.0～1.2 ratio is added said decalcifying agent.
6. acid waste water for depositing vanadium cyclic utilization method as claimed in claim 3 is characterized in that, when said decalcifying agent is oxalic acid or ammonium oxalate, presses the C in the decalcifying agent
2O
4 2-With the Ca in the said basic soln
2+Mol ratio be that 0.7～1.2 ratio is added said decalcifying agent.
7. acid waste water for depositing vanadium cyclic utilization method as claimed in claim 3 is characterized in that, when decalcifying agent is hydrofluoric acid or Neutral ammonium fluoride, presses the F in the decalcifying agent
-With the Ca in the said basic soln
2+And Mg
2+The mol ratio of sum is that 1.8～2.2 ratio is added said decalcifying agent.
8. acid waste water for depositing vanadium cyclic utilization method as claimed in claim 1 is characterized in that, the step of said employing milk of lime adjustment of acidity vanadium wastewater to alkalescence is adjusted to 9～11 with milk of lime with the pH value of acid waste water for depositing vanadium.
9. acid waste water for depositing vanadium cyclic utilization method as claimed in claim 1 is characterized in that, said decalcification step stirs when also comprising the adding decalcifying agent.
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|---|---|---|---|
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| CN102838233B CN102838233B (en) | 2014-05-21 |
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| CN103145267A (en) * | 2013-03-20 | 2013-06-12 | 李杨 | Method for recovering copper sulfide and ferric hydroxide in auricupride acid wastewater through sulfidization method |
| CN103922454A (en) * | 2014-04-15 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing manganese from acidic molybdenum precipitation wastewater |
| CN103964624A (en) * | 2014-05-13 | 2014-08-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Recycling method of ammonium salt precipitating vanadium wastewater |
| CN105330050A (en) * | 2014-08-11 | 2016-02-17 | 司明丽 | Integrated waste water treatment and resource recycle method of crystal processing |
| CN105567976A (en) * | 2016-01-13 | 2016-05-11 | 晟通亿和（天津）企业管理咨询有限公司 | Method for treating vanadium extracting industrial acid wastewater and comprehensively recycling valuable metal |
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| CN107381754A (en) * | 2017-09-19 | 2017-11-24 | 攀钢集团研究院有限公司 | Processing method for calcification vanadium extracting waste water |
| CN107541599A (en) * | 2017-10-27 | 2018-01-05 | 成都先进金属材料产业技术研究院有限公司 | Use the preparation method of acid high manganese high purity containing vanadium leachate vanadium |
| CN109161695A (en) * | 2018-09-29 | 2019-01-08 | 成都先进金属材料产业技术研究院有限公司 | The method of calcification vanadium slag sintering Selectively leaching vanadium |
| CN112811660A (en) * | 2021-01-05 | 2021-05-18 | 长沙有色冶金设计研究院有限公司 | Treatment process for waste gas and alum precipitation wastewater generated in integration of stone coal navajoite and navajoite |
| CN113860376A (en) * | 2021-11-04 | 2021-12-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity manganese carbonate by using vanadium extraction wastewater |
| CN113929247A (en) * | 2021-11-15 | 2022-01-14 | 国网山东省电力公司电力科学研究院 | Vanadium-containing wastewater treatment method, vanadium-containing catalyst, preparation method and application |
| CN114350952A (en) * | 2021-11-29 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for recycling gypsum slag in calcification vanadium extraction process |
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| CN103145267A (en) * | 2013-03-20 | 2013-06-12 | 李杨 | Method for recovering copper sulfide and ferric hydroxide in auricupride acid wastewater through sulfidization method |
| CN103922454A (en) * | 2014-04-15 | 2014-07-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for removing manganese from acidic molybdenum precipitation wastewater |
| CN103922454B (en) * | 2014-04-15 | 2016-03-30 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of acid waste water for depositing vanadium demanganization |
| CN103964624A (en) * | 2014-05-13 | 2014-08-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Recycling method of ammonium salt precipitating vanadium wastewater |
| CN103964624B (en) * | 2014-05-13 | 2016-04-27 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method that ammonium salt vanadium wastewater recycles |
| CN105330050A (en) * | 2014-08-11 | 2016-02-17 | 司明丽 | Integrated waste water treatment and resource recycle method of crystal processing |
| CN105567976A (en) * | 2016-01-13 | 2016-05-11 | 晟通亿和（天津）企业管理咨询有限公司 | Method for treating vanadium extracting industrial acid wastewater and comprehensively recycling valuable metal |
| CN107055872A (en) * | 2017-05-04 | 2017-08-18 | 长沙华时捷环保科技发展股份有限公司 | A kind of desulfurization absorbing liquid purifying processing device and method |
| CN107381754A (en) * | 2017-09-19 | 2017-11-24 | 攀钢集团研究院有限公司 | Processing method for calcification vanadium extracting waste water |
| CN107541599A (en) * | 2017-10-27 | 2018-01-05 | 成都先进金属材料产业技术研究院有限公司 | Use the preparation method of acid high manganese high purity containing vanadium leachate vanadium |
| CN107541599B (en) * | 2017-10-27 | 2019-07-26 | 成都先进金属材料产业技术研究院有限公司 | Use the preparation method of acid high manganese high purity containing vanadium leachate vanadium |
| CN109161695A (en) * | 2018-09-29 | 2019-01-08 | 成都先进金属材料产业技术研究院有限公司 | The method of calcification vanadium slag sintering Selectively leaching vanadium |
| CN109161695B (en) * | 2018-09-29 | 2020-06-09 | 成都先进金属材料产业技术研究院有限公司 | Method for selectively leaching vanadium from calcified roasted vanadium slag |
| CN112811660A (en) * | 2021-01-05 | 2021-05-18 | 长沙有色冶金设计研究院有限公司 | Treatment process for waste gas and alum precipitation wastewater generated in integration of stone coal navajoite and navajoite |
| CN113860376A (en) * | 2021-11-04 | 2021-12-31 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing high-purity manganese carbonate by using vanadium extraction wastewater |
| CN113929247A (en) * | 2021-11-15 | 2022-01-14 | 国网山东省电力公司电力科学研究院 | Vanadium-containing wastewater treatment method, vanadium-containing catalyst, preparation method and application |
| CN113929247B (en) * | 2021-11-15 | 2023-11-21 | 国网山东省电力公司电力科学研究院 | Vanadium-containing wastewater treatment method, vanadium-containing catalyst, preparation method and application |
| CN114350952A (en) * | 2021-11-29 | 2022-04-15 | 攀钢集团研究院有限公司 | Method for recycling gypsum slag in calcification vanadium extraction process |
| CN114350952B (en) * | 2021-11-29 | 2024-02-23 | 攀钢集团研究院有限公司 | Method for recycling gypsum slag in calcified vanadium extraction process |
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