CN105198139A - Hydrometallurgy industry raffinate waste water COD removal method - Google Patents
Hydrometallurgy industry raffinate waste water COD removal method Download PDFInfo
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- CN105198139A CN105198139A CN201510684466.2A CN201510684466A CN105198139A CN 105198139 A CN105198139 A CN 105198139A CN 201510684466 A CN201510684466 A CN 201510684466A CN 105198139 A CN105198139 A CN 105198139A
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Abstract
The invention discloses a hydrometallurgy industry raffinate waste water COD removal method. According to the method, lime is added into waste water, and is combined with sulfate radical, phosphate radical, carbonate radical, fluorinions, metal ions and the like to generate defecation mud, the defecation mud is taken as an adsorber to remove dispersed oil in the waste water, filter liquor generated after filtering is subjected to pH regulation, then fenton oxidation is performed to degrade macromolecular organic compounds, further pH regulation is performed, then low molecular weight organic matters are deeply degraded by photo-catalytic oxidation, finally solid-liquid separation is performed to obtain a solid catalyst and waste water with the COD content smaller than 100mg/L, and the solid catalyst is returned to photo-catalytic oxidation reaction for cyclic utilization. The method is good in COD removal effect, free of adsorber regeneration and low in operation cost, and has industry application prospect.
Description
Technical field
The invention belongs to metallurgy waste water treatment field, particularly relate to a kind of minimizing technology of hydrometallurgy industry raffinate waste water COD.
Background technology
Industry metallurgy method mainly contains two kinds, i.e. pyrogenic process and wet method, and wherein hydrometallurgical technology is most widely used.Hydrometallurgical technology refers to first transfers to liquid phase by various valuable element from solid phase by extract technology, and then by various effective ways Separation and Recovery valuable component from leach liquor.The most general a kind of technique of hydrometallurgy sector application with extraction process Separation and Recovery non-ferrous metal and rare earth element from leach liquor.But when while Footwall drift element, also can produce a large amount of raffinate waste water with extraction process from leach liquor thereupon.Organic components in raffinate waste water is complicated, and COD content is high, and toxicity is large, pre-treatment must remove COD before discharge.
In hydrometallurgy industry, conventional metal extraction agent mainly contains acidic extractant, Neutral-neutral Extractants, basic extractant and oxime type extraction agent.Wherein acidic extractant is usually used in the non-ferrous metal elements such as extracting and separating nickel cobalt as P204, P507 etc.; Neutral-neutral Extractants such as TBP etc. is usually used in extracting and separating rear earth element; Basic extractant such as primary amine N235, N1923 etc. are then usually used in extraction and recovery vanadium chromium tungsten etc.; Oximes extraction agent such as LIX984 etc. is widely used in the extraction and recovery of copper.
In actual production, above-mentioned various extraction agent all needs to be made into certain density extracted organic phase with sulphonated coal wet goods thinner and uses.Like this, be presented as in raffinate waste water that the composition of COD just mainly comprises extraction agent, thinner and the metal extracted species etc. that are dissolved in aqueous phase.For the molybdenum extraction process of certain enterprise, the raffinate Organic substance in water that gives up comprises a small amount of dispersed oil, extraction agent N235, solvability sulfonated kerosene and molybdenum extracted species.Except COD, the salts contg in general raffinate waste water is usually higher, and negatively charged ion mainly comprises sulfate radical, phosphate radical, nitrate radical, carbonate, chlorion, fluorion and other heavy metal acid ions etc., is not suitable for using biological process degradation treatment.Inventor's early-stage Study finds, the removal to the various raffinate waste water CODs of hydrometallurgy industry of oil removal, air supporting, resin and active carbon adsorption technology does not all have positive effect; Use the multiple high-level oxidation technologies such as Fenton, electric Fenton, electrolytic oxidation, ozone oxidation the COD in raffinate waste water can be removed to about 200mg/L at most, utilize gac or activated coke absorption still cannot remove below COD to 100mg/L further.This illustrates, the organism in the waste water after the high-level oxidation technology process such as Fenton is mainly the very strong small molecules of polarity, extremely difficult degraded further.
COD in order to ensure hydrometallurgy industry raffinate waste water is up to standard, and reduces processing cost, is badly in need of a kind of method this kind of waste water COD can removed to below 100mg/L.
Summary of the invention
For the feature containing sulfate radical, phosphate radical, carbonate and fluorion etc. in above-mentioned hydrometallurgy industry raffinate waste water, the present invention proposes a kind of method effectively can removing COD in raffinate waste water, first the method utilizes lime and sulfate radical, phosphate radical, carbonate and fluorion etc. to be obtained by reacting calcium deposit slag, Adsorption dispersed oil, reach the double effects of desalination and reduction COD, follow-up through Fenton oxidation degraded larger molecular organics, further photochemical catalytic oxidation depth degradation small organic molecule, finally obtains the waste water that COD content is less than 100mg/L.
For reaching this object, the present invention by the following technical solutions:
A kind of minimizing technology of hydrometallurgy industry raffinate waste water COD, in waste water, feeding lime is precipitated slag, Adsorption dispersed oil, filter, the filtrate obtained enters Fenton oxidation reaction degraded larger molecular organics after pH regulator, further pH regulator laggard enter photocatalysis oxidation reaction depth degradation small organic molecule, the waste water COD content finally obtained is less than 100mg/L.
Heterogeneous solid catalyzer in photocatalysis oxidation reaction can without any process direct reuse.
Described Lime-Injecting amount is for removing 1% ~ 200% of theoretical amount needed for whole negatively charged ion.
The filtrate optimal pH scope entering Fenton oxidation reaction is 1 ~ 12.
Fenton oxidation reaction is with divalent iron salt and hydrogen peroxide for Fenton reagent, and the reaction times is 20 ~ 60min, and temperature is 20 ~ 60 DEG C.
Hydrogen peroxide dosage is 1 ~ 10 times of influent COD mass concentration, and the ferrous ion added and the mol ratio of hydrogen peroxide are 1:2 ~ 6.
The waste water optimal pH entering photocatalysis oxidation reaction is 4 ~ 9.
Photocatalysis oxidation reaction catalyzer is can be used as a certain metal oxide of photocatalyst material or a certain metallic sulfide, or certain several metal oxide, or certain several metallic sulfide, or the mixture of one or more metal oxides and metallic sulfide, the conventional photocatalyst material according to recording in common practise includes but not limited to ZnO, ZnS, SnO
2, SnS
2, ZrO
2, ZrS
2, TiO
2, TiS
2, CdO and CdS etc., oxygenant is hydrogen peroxide, is under the rayed of 190 ~ 780nm at wavelength, and the reaction times is 1 ~ 8min, and temperature is 20 ~ 80 DEG C.
Catalyst amounts is 0.1 ~ 10g/L, and oxygenant adds 1 ~ 10 times that concentration is influent COD mass concentration.
Waste water COD content after photocatalysis oxidation reaction is down to below 100mg/L.
Compared with prior art scheme, the present invention has following beneficial effect:
1, the invention provides a kind of minimizing technology of hydrometallurgy industry raffinate waste water COD;
2, the present invention passes through to feeding lime in waste water, combine with sulfate radical, phosphate radical, carbonate and fluorion etc. and generate calcium deposit slag as sorbent material, not only can remove dispersed oil in waste water by active adsorption, reduce COD, and successfully anionic part is removed, serve desalting, without the need to initial adsorbent material manipulation of regeneration;
3, the heterogeneous solid catalyzer reusable edible in photocatalysis oxidation reaction of the present invention, lossless;
4, the lime low price used in the present invention, Fenton reagent and photocatalyst dosage is little, power consumption is few, integrated operation cost is low;
5, COD successfully can be down to below 100mg/L by the present invention, is applicable to the little smelter of raffinate wastewater flow rate and promotes.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the method for the invention.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, and do not represent or limit the scope of the present invention, protection scope of the present invention is as the criterion with claims.
Embodiment
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
The copper of certain enterprise, molybdenum extraction and recovery system composite waste, pH=0.69, COD1240mg/L, SO
4 2-content is 109.5g/L, Cl
-content is 7.8g/L, NO
3 -content is 210.5g/L.COD main component is a small amount of dispersed oil, extraction agent N235 and LIX984, sulfonated kerosene and copper molybdenum extracted species.
(1) get the above-mentioned waste water of 5000mL, add dry hydrate, stirring reaction 30min by 1% of the theoretical amount removing whole sulfate radical, then leave standstill 20min, filter the calcium sulfate slag removed and produce;
(2) filtrate of step (1) gained regulates pH=1, COD content to be 1010mg/L, SO with 10% dilute hydrochloric acid solution
4 2-content is 108.5g/L;
(3) step (2) gained solution first adds the hydrogen peroxide of 30%, wherein H
2o
2add-on is 1 times of COD mass concentration, i.e. and then 1.01g/L adds rapidly the copperas solution of 30%, Fe
2+with H
2o
2mol ratio be 1:2.Stirring reaction 60min, temperature of reaction is 20 DEG C;
(4) step (3) gained solution 10%NaOH solution regulates pH=7, COD content to be 450mg/L;
(5) ZnO or ZnS that step (4) gained solution first adds 0.1g/L makes catalyzer, then adds 30%H
2o
2, wherein H
2o
2dosage is 1 times of influent COD mass concentration, i.e. 450mg/L, then at wavelength is to carry out catalyzed oxidation under the illumination of 190nm, and oxidizing reaction temperature is 20 DEG C, and the reaction times is 8min;
(6) step (5) water outlet is filtered.Gained filter residue returns step (5) and uses as catalyst recirculation, and liquor C OD is 79mg/L.
Embodiment 2
The cobalt raffinate waste water of Zhejiang smelter, pH=9.80, COD4580mg/L, SO
4 2-content is 158.4g/L.COD main component is a small amount of dispersed oil, extraction agent P204, a small amount of emulsification and deliquescent sulfonated kerosene and the cobalt extracted species in blueness.
(1) get the above-mentioned waste water of 5000mL, add dry hydrate, stirring reaction 30min by 50% of the theoretical amount removing whole sulfate radical, then leave standstill 20min, filter the calcium sulfate slag removed and produce;
(2) filtrate of step (1) gained regulates pH=8, COD content to be 2540mg/L, SO with 10% dilute hydrochloric acid solution
4 2-content is 82.3g/L;
(3) step (2) gained solution first adds the hydrogen peroxide of 30%, wherein H
2o
2add-on is 2 times of COD mass concentration, i.e. and then 5.08g/L adds rapidly the copperas solution of 30%, Fe
2+with H
2o
2mol ratio be 1:3, stirring reaction 40min, temperature of reaction is 60 DEG C;
(4) step (3) gained solution 10%NaOH solution regulates pH=9, COD content to be 372.3mg/L;
(5) step (4) gained solution first adds the SnO of 2g/L
2+ ZnO dual-component catalyst (SnO
2be 1:1 with ZnO mass ratio), then add 30%H
2o
2, wherein H
2o
2dosage is 3 times of influent COD mass concentration, i.e. 1.117g/L, then at wavelength is to carry out catalyzed oxidation under the illumination of 400nm, and oxidizing reaction temperature is 50 DEG C, and the reaction times is 5min;
(6) centrifugation is carried out in step (5) water outlet, and gained precipitation returns step (5) and uses as catalyst recirculation, and supernatant C OD is 75.2mg/L.
Embodiment 3
Jiangxi Rare Earth Company raffinate waste water, pH=6.58, COD960mg/L, PO
4 3-content is 78.2g/L, Cl
-content is 18.3g/L, NO
3 -content is 165.2.5g/L.COD main component is a small amount of dispersed oil, extraction agent TBP, sulfonated kerosene and rare earth extracted species.
(1) get the above-mentioned waste water of 5000mL, add dry hydrate, stirring reaction 30min by 100% of the theoretical amount removing whole phosphate radical, then leave standstill 20min, filter the calcium phosphate slag removed and produce.
(2) the filtrate pH=12 of step (1) gained, COD content is 752mg/L, PO
4 3-content is 1.7g/L;
(3) step (2) gained solution first adds the hydrogen peroxide of 30%, wherein H
2o
2add-on is 5 times of COD mass concentration, i.e. and then 3.76g/L adds rapidly the copperas solution of 30%, Fe
2+with H
2o
2mol ratio be 1:6, stirring reaction 20min, temperature of reaction is 30 DEG C;
(4) step (3) gained solution 10%NaOH solution regulates pH=6, COD content to be 582.3mg/L;
(5) step (4) gained solution first adds the ZnS+ZrS of 5g/L
2dual-component catalyst (ZnS and ZrS
2mass ratio is 3:2), then add 30%H
2o
2, wherein H
2o
2dosage is 5 times of influent COD mass concentration, i.e. 2.912g/L, then at wavelength is to carry out catalyzed oxidation under the illumination of 600nm, and oxidizing reaction temperature is 80 DEG C, and the reaction times is 3min;
(6) centrifugation is carried out in step (5) water outlet.Gained precipitation returns step (5) and uses as catalyst recirculation, and liquor C OD is 58.5mg/L.
Embodiment 4
Certain Rare Earth Enterprises raffinate composite waste, pH=4.53, COD4870mg/L, SO
4 2-content is 38.6g/L, Cl
-content is 82.3g/L, F
-content is 8.5g/L.COD main component is a small amount of dispersed oil and oil in water emulsion, N1923, TBP, P507, LIX984, sulfonated kerosene and various metal extracted species.
(1) get the above-mentioned waste water of 5000mL, add dry hydrate, stirring reaction 30min by 200% of the theoretical amount removing whole sulfate radical and fluorion, then leave standstill 20min, filter the calcium deposit slag removed and produce;
(2) filtrate of step (1) gained regulates pH=4, COD content to be 3258mg/L, SO with 10% dilute hydrochloric acid solution
4 2-content is 0.7g/L, F
-ion is 25.2mg/L;
(3) step (2) gained solution first adds the hydrogen peroxide of 30%, wherein H
2o
2add-on is 10 times of COD mass concentration, i.e. and then 32.58g/L adds rapidly the copperas solution of 30%, Fe
2+with H
2o
2mol ratio be 1:3, stirring reaction 50min, temperature of reaction is 25 DEG C;
(4) step (3) gained solution 10%NaOH solution regulates pH=4, COD content to be 767.3mg/L;
(5) step (4) gained solution first adds the TiO of 10g/L
2+ TiS
2dual-component catalyst (TiO
2with TiS
2mass ratio is 2:1), then add H
2o
2, wherein H
2o
2add-on is 10 times of influent COD mass concentration, i.e. 7.67g/L, then at wavelength is to carry out catalyzed oxidation under the illumination of 780nm, and oxidizing reaction temperature is 40 DEG C, and the reaction times is 1min;
(6) step (5) water outlet is filtered.Gained filter residue returns step (5) and uses as catalyst recirculation, and liquor C OD is 68.9mg/L.
Embodiment 5
Certain hydrometallurgy enterprise raffinate composite waste, pH=4.53, COD3840mg/L, CO
3 2-content is 18.6g/L, Cl
-content is 22.8g/L, SO
4 2-content is 6.7g/L.COD main component is a small amount of dispersed oil and oil in water emulsion, P507, LIX984, sulfonated kerosene and various metal extracted species.
(1) get the above-mentioned waste water of 5000mL, add dry hydrate, stirring reaction 40min by 100% of the theoretical amount removing whole sulfate radical and carbonate, then leave standstill 30min, filter the calcium deposit slag removed and produce;
(2) filtrate of step (1) gained regulates pH=3, COD content to be 3158mg/L, SO with 10% dilute hydrochloric acid solution
4 2-content is 1.7g/L, CO
3 2-ion is 114mg/L;
(3) step (2) gained solution first adds the hydrogen peroxide of 30%, wherein H
2o
2add-on is 2 times of COD mass concentration, i.e. and then 6.316g/L adds rapidly the copperas solution of 30%, Fe
2+with H
2o
2mol ratio be 1:4, stirring reaction 60min, temperature of reaction is 40 DEG C;
(4) step (3) gained solution 10%NaOH solution regulates pH=8.5, COD content to be 800mg/L;
(5) step (4) gained solution first adds the CdO+CdS+ZnO+ZrO of 2.5g/L
2catalyzer (CdO, CdS, ZnO and ZrO
2mass ratio is 1:1:2:1), then add H
2o
2, wherein H
2o
2add-on is 3 times of influent COD mass concentration, i.e. 2.4g/L.Then be carry out catalyzed oxidation under the illumination of 550nm at wavelength, oxidizing reaction temperature is 30 DEG C, and the reaction times is 2min;
(6) step (5) water outlet is filtered.Gained filter residue returns step (5) and uses as catalyst recirculation, and liquor C OD is 17.9mg/L.
Applicant states, the present invention illustrates method of the present invention by above-described embodiment, but the present invention is not limited to aforesaid operations step, does not namely mean that the present invention must rely on aforesaid operations step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. the minimizing technology of a hydrometallurgy industry raffinate waste water COD, it is characterized in that, in waste water, feeding lime is precipitated slag, Adsorption dispersed oil, filter, the filtrate obtained enter after pH regulator Fenton oxidation reaction degraded larger molecular organics, further pH regulator laggard enter photocatalysis oxidation reaction depth degradation small organic molecule, the waste water COD finally obtained is less than 100mg/L.
2. treatment process as claimed in claim 1, it is characterized in that, the heterogeneous catalyst in photocatalysis oxidation reaction can without any process direct reuse.
3. treatment process as claimed in claim 1 or 2, is characterized in that, described Lime-Injecting amount is for removing 1% ~ 200% of theoretical amount needed for whole negatively charged ion.
4. treatment process as claimed in claim 1, is characterized in that, the filtrate optimal pH scope entering Fenton oxidation reaction is 1 ~ 12.
5. treatment process as claimed in claim 4, is characterized in that, Fenton oxidation reaction is with divalent iron salt and hydrogen peroxide for Fenton reagent, and the reaction times is 20 ~ 60min, and temperature is 20 ~ 60 DEG C.
6. treatment process as claimed in claim 5, it is characterized in that, hydrogen peroxide dosage is 1 ~ 10 times of influent COD mass concentration, and the ferrous ion added and the mol ratio of hydrogen peroxide are 1:2 ~ 6.
7. treatment process as claimed in claim 1, it is characterized in that, the waste water optimal pH entering photocatalysis oxidation reaction is 4 ~ 9.
8. treatment process as claimed in claim 7, it is characterized in that, photocatalysis oxidation reaction catalyzer is can be used as a certain metal oxide of photocatalyst material or a certain metallic sulfide, or certain several metal oxide, or certain several metallic sulfide, the mixture of a certain or several metal oxide and metallic sulfide, oxygenant is hydrogen peroxide, be under the rayed of 190 ~ 780nm at wavelength, the reaction times is 1 ~ 8min, and temperature is 20 ~ 80 DEG C.
9. treatment process as claimed in claim 8, it is characterized in that, catalyst amounts is 0.1 ~ 10g/L, and oxygenant adds 1 ~ 10 times that concentration is influent COD mass concentration.
10. treatment process as claimed in claim 9, it is characterized in that, after photocatalysis oxidation reaction, the waste water COD content obtained through solid-liquid separation is down to below 100mg/L.
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| CN105601020A (en) * | 2016-03-30 | 2016-05-25 | 北京赛科康仑环保科技有限公司 | Treatment technology of raffinate wastewater of nickel, cobalt and manganese |
| CN106315756A (en) * | 2016-10-18 | 2017-01-11 | 南昌航空大学 | Device for advanced treatment of organic wastewater through coordination of photocatalysis and fenton oxidation |
| CN106582711A (en) * | 2016-11-25 | 2017-04-26 | 南宁市黑晶信息技术有限公司 | Wastewater precipitation and purification method |
| CN108529791A (en) * | 2018-05-02 | 2018-09-14 | 北京赛科康仑环保科技有限公司 | The processing method of deep removal COD in a kind of raffinate from nickel cobalt |
| CN108947016A (en) * | 2018-08-10 | 2018-12-07 | 湖南艾森尼克环保科技有限公司 | A method of removing hydrometallurgy industry raffinate waste water COD |
| CN109970135A (en) * | 2019-04-09 | 2019-07-05 | 中南大学 | The application of the TOC of calcium sulfate and/or calcium phosphate in removal hydrometallurgy raffinate |
| CN111747560A (en) * | 2020-06-04 | 2020-10-09 | 广东益诺欧环保股份有限公司 | System and method for treating and recycling J acid |
| CN113979579A (en) * | 2021-11-23 | 2022-01-28 | 浙江解氏新材料股份有限公司 | Method for efficiently removing fluorine-containing compounds in wastewater |
| CN114394693A (en) * | 2022-01-22 | 2022-04-26 | 安徽科技学院 | Clarification treatment method for industrial oily wastewater |
| CN114656078A (en) * | 2022-01-25 | 2022-06-24 | 昆明理工大学 | Method for removing organic matters in solution through spray catalysis in multi-field coupling high-energy field |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105601020A (en) * | 2016-03-30 | 2016-05-25 | 北京赛科康仑环保科技有限公司 | Treatment technology of raffinate wastewater of nickel, cobalt and manganese |
| CN106315756A (en) * | 2016-10-18 | 2017-01-11 | 南昌航空大学 | Device for advanced treatment of organic wastewater through coordination of photocatalysis and fenton oxidation |
| CN106582711A (en) * | 2016-11-25 | 2017-04-26 | 南宁市黑晶信息技术有限公司 | Wastewater precipitation and purification method |
| CN108529791A (en) * | 2018-05-02 | 2018-09-14 | 北京赛科康仑环保科技有限公司 | The processing method of deep removal COD in a kind of raffinate from nickel cobalt |
| CN108947016A (en) * | 2018-08-10 | 2018-12-07 | 湖南艾森尼克环保科技有限公司 | A method of removing hydrometallurgy industry raffinate waste water COD |
| CN108947016B (en) * | 2018-08-10 | 2021-06-18 | 湖南艾森尼克环保科技有限公司 | Method for removing COD (chemical oxygen demand) in raffinate wastewater in hydrometallurgy industry |
| CN109970135A (en) * | 2019-04-09 | 2019-07-05 | 中南大学 | The application of the TOC of calcium sulfate and/or calcium phosphate in removal hydrometallurgy raffinate |
| CN111747560A (en) * | 2020-06-04 | 2020-10-09 | 广东益诺欧环保股份有限公司 | System and method for treating and recycling J acid |
| CN113979579A (en) * | 2021-11-23 | 2022-01-28 | 浙江解氏新材料股份有限公司 | Method for efficiently removing fluorine-containing compounds in wastewater |
| CN113979579B (en) * | 2021-11-23 | 2023-04-07 | 浙江解氏新材料股份有限公司 | Method for efficiently removing fluorine-containing compounds in wastewater |
| CN114394693A (en) * | 2022-01-22 | 2022-04-26 | 安徽科技学院 | Clarification treatment method for industrial oily wastewater |
| CN114656078A (en) * | 2022-01-25 | 2022-06-24 | 昆明理工大学 | Method for removing organic matters in solution through spray catalysis in multi-field coupling high-energy field |
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