CN102633326A - Ion exchange membrane electrolysis method for treating acid waste water containing chloride in copper metallurgy process - Google Patents
Ion exchange membrane electrolysis method for treating acid waste water containing chloride in copper metallurgy process Download PDFInfo
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- CN102633326A CN102633326A CN2012101302480A CN201210130248A CN102633326A CN 102633326 A CN102633326 A CN 102633326A CN 2012101302480 A CN2012101302480 A CN 2012101302480A CN 201210130248 A CN201210130248 A CN 201210130248A CN 102633326 A CN102633326 A CN 102633326A
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- electrolysis
- copper
- wastewater
- chloracid
- exchange membrane
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- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002351 wastewater Substances 0.000 title claims abstract description 28
- 239000003014 ion exchange membrane Substances 0.000 title claims abstract description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title abstract description 8
- 239000002253 acid Substances 0.000 title abstract description 5
- 238000009867 copper metallurgy Methods 0.000 title abstract 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000010949 copper Substances 0.000 claims abstract description 28
- 229910052802 copper Inorganic materials 0.000 claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000460 chlorine Substances 0.000 claims abstract description 8
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 8
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 6
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 6
- 239000011669 selenium Substances 0.000 claims abstract description 6
- 229910052709 silver Inorganic materials 0.000 claims abstract description 6
- 239000004332 silver Substances 0.000 claims abstract description 6
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 5
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052737 gold Inorganic materials 0.000 claims abstract description 5
- 239000010931 gold Substances 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- ZHLKXBJTJHRTTE-UHFFFAOYSA-N Chlorobenside Chemical compound C1=CC(Cl)=CC=C1CSC1=CC=C(Cl)C=C1 ZHLKXBJTJHRTTE-UHFFFAOYSA-N 0.000 claims description 18
- 238000005272 metallurgy Methods 0.000 claims description 14
- 125000002091 cationic group Chemical group 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005342 ion exchange Methods 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 5
- 229910001385 heavy metal Inorganic materials 0.000 claims description 4
- CJTCBBYSPFAVFL-UHFFFAOYSA-N iridium ruthenium Chemical compound [Ru].[Ir] CJTCBBYSPFAVFL-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims 1
- 239000001117 sulphuric acid Substances 0.000 claims 1
- 150000002739 metals Chemical class 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000005341 cation exchange Methods 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 46
- 239000000203 mixture Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 12
- 230000003292 diminished effect Effects 0.000 description 7
- 239000004519 grease Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 copper wherein Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 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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- Electrolytic Production Of Metals (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses an ion exchange membrane electrolysis method for treating acid waste water containing chloride in a copper metallurgy process. Solutions in a cathode chamber and an anode chamber are separated by virtue of a heterogeneous cation exchange membrane, an anode is one of noble electrodes such as a ruthenium-iridium-series coating titanium net (plate) or a graphite electrode, a cathode is one of a graphite electrode, a copper electrode, a titanium electrode or a stainless steel electrode, the electrolysis temperature ranges from 25 DEG C to 65 DEG C, and the current density is 100A/m<2> and 1000A/m<2>. By virtue of the electrolysis, valuable metals such as copper, selenium, tellurium, antimony, bismuth, lead, arsenic, silver and gold in the acid waste water containing chloride are all enriched in cathode sediment, and the gross recovery of the valuable metals is more than or equal to 80%; and chloride ions are anodized to chlorine so as to be removed and recovered, treating fluid is recovered in a high-concentration sulfuric acid way, the recovery rate of sulfuric acid is more than or equal to 95%, and the content of the chloride ions in the recovered sulfuric acid is less than or equal to 500mg/L.
Description
Technical field
The present invention is a kind of realize chloracid wastewater resource utilization and innoxious electrolysis with ion-exchange film technology in the metallurgy of copper flow process, more particularly, is a kind of valuable metal, chlorine and vitriolic method that can comprehensively reclaim in the chloracid wastewater.
Background technology
The chloracid wastewater has characteristics such as acidity height, chloride height, heavy metal complicated component, corrodibility be strong in the metallurgy of copper flow process.Adopt traditional waste water treatment process, not only the quantity of slag is big, cl ions can't remove, and the waste water chloride ion-containing of output is high and can't reuse; And comprehensive recovery such as valuable element such as tellurium, selenium, copper, silver, sulfuric acid, cl ions is low.From stopping to pollute the angle with comprehensive utilization of resources, research is low-cost, to reclaim novel process be to realize that resource utilization reduces discharging the most reasonably technological approaches for high efficiency spent acid and heavy metal.
Summary of the invention
Deficiency to above-mentioned existence; The present invention proposes a kind of electrolysis with ion-exchange film method of handling chloracid wastewater in the metallurgy of copper flow process; Adopt the cationic exchange membrane electrolysis tech to handle the chloracid wastewater of output in the metallurgy of copper flow process; Valuable metals such as copper wherein, selenium, tellurium, antimony, bismuth, lead, arsenic, silver and gold obtain enrichment at cathode deposit; Cl ions is oxidized to chlorine and removes and reclaim, and treatment solution has been realized the comprehensive utilization of resources of chloracid wastewater finally with the reuse of high-concentration sulfuric acid form.
Realize that step of the present invention is: 1. adopt cationic exchange membrane to separate the solution of cathode compartment and anolyte compartment; 2. the chloracid wastewater is as cathode chamber solution, and valuable metal ions such as copper wherein, tellurium are enriched in settling through cathodic reduction; 3. the waste water that has deposited valuable metal at cathode compartment is behind filtration under diminished pressure, and filtrating is as anolyte compartment's solution, and cl ions wherein removes with the chlorine form through anodic oxidation; 4. the solution of anolyte compartment is discharged as handling qualifying liquid after the electrolysis.
Described ion-exchange membrane is heterogeneous cationic exchange membranes such as Ionac MC-3470 cationic exchange membrane or ULTREX CMI-7000 cationic exchange membrane.
The anode that said anolyte compartment adopts is that to analyse the low and ruthenium iridium that overpotential for oxygen evolution is higher of chlorine overpotential be a kind of in the noble electrodes such as coated titanium net/plate or Graphite Electrodes; The negative electrode that said cathode compartment adopts is a kind of in Graphite Electrodes, copper electrode, titanium electrode or the stainless steel electrode.
Handled chloracid wastewater is one or more the heavy metal wastewater thereby that contains in copper, selenium, tellurium, lead, arsenic, antimony, bismuth, silver or the gold, and wherein cl concn is not less than 0.1g/L, and sulfuric acid concentration is 0～400g/L.
The above-mentioned steps 4. current density of electrolytic process employing is 100～1000A/m
2, temperature is 25～65 ℃.
Beneficial effect of the present invention is: liquid and dirty acid etc. are after treatment behind chloracid wastewater in the metallurgy of copper flow process such as beneficiation wastewater, the deselenization; Through electrolysis; Valuable metal in the chloracid wastewater such as copper, selenium, tellurium, antimony, bismuth, lead, arsenic, silver and gold etc. all are enriched in the cathode deposit total yield>=80%; Cl ions changes into chlorine in anodic oxygen and removes and reclaim, and treatment solution is finally realized reuse, the sulfuric acid recovery>=95%, chloride ion content≤500mg/L in the sulfuric acid of reuse with the high-concentration sulfuric acid form.
Description of drawings
Fig. 1 is a principle schematic of the present invention.
Embodiment
Be described further below in conjunction with embodiment and Fig. 1 specific embodiments of the invention:
In embodiment 1, the metallurgy of copper flow process behind the deselenization of output the liquid composition as shown in table 1.Adopt the ULTREXCMI-7000 cationic exchange membrane that liquid pool and electrolyzer are divided into cathode compartment and anolyte compartment respectively.The electrolysis temperature of liquid pool and electrolyzer is 25 ℃ of room temperatures, and current density is 625A/m
2, electrolysing period is 4 hours, and it is the coated titanium net that anode all adopts ruthenium iridium, and negative electrode all adopts Graphite Electrodes.Liquid is as the catholyte of liquid pool behind the deselenization, and anolyte is for containing 10g/L Cu
2+With 273g/L H
2SO
4Solution, carry out the electrolysis dosing.After the liquid pool electrolysis 4 hours, liquid is removed the copper sponge of concentration of valuable metals through filtration under diminished pressure after the electrolysis of cathode compartment, and supernatant is a liquid and for use as the anolyte of electrolyzer after the demetalization electrolysis.The cathode compartment of electrolyzer is allocated liquid behind the fresh deselenization into, and the anolyte compartment allocates liquid after the demetalization electrolysis into.Through electrolysis after 4 hours; Liquid is analyzed composition as handling qualifying liquid after anolyte compartment's electrolysis; Liquid is removed sea copper after the cathode compartment electrolysis behind filtration under diminished pressure, and the supernatant that obtains is that liquid is as follow-up electrolytic anolyte behind the demetalization ion, and the sponge grease that deposits washs dry post analysis composition.
Handle the composition of qualifying liquid and see table 1.The sponge grease composition is seen table 2.
Liquid and the composition of handling qualifying liquid behind table 1 deselenization
The composition of table 2 copper sponge
In embodiment 2, the metallurgy of copper flow process behind the deselenization of output the liquid composition as shown in table 3.Adopt the ULTREXCMI-7000 cationic exchange membrane that liquid pool and electrolyzer are divided into cathode compartment and anolyte compartment respectively.The electrolysis temperature of liquid pool and electrolyzer is 25 ℃ of room temperatures, and current density is 625A/m
2, electrolysing period is 4 hours, and it is the coated titanium net that anode all adopts ruthenium iridium, and negative electrode all adopts Graphite Electrodes.The catholyte of liquid pool and anolyte all are liquid behind the fresh deselenization, carry out the electrolysis dosing.After the liquid pool electrolysis 4 hours, liquid is removed the copper sponge of concentration of valuable metals through filtration under diminished pressure after the electrolysis of cathode compartment, and supernatant (being liquid after the demetalization electrolysis) is for use as the anolyte of electrolyzer.The cathode compartment of electrolyzer is allocated liquid behind the fresh deselenization into, and the anolyte compartment allocates liquid after the demetalization electrolysis into.After 4 hours, anolyte compartment's solution is analyzed composition as handling qualifying liquid through electrolysis, and the cathode chamber solution filtration under diminished pressure is removed copper sponge, and liquid is as follow-up electrolytic anolyte after the demetalization electrolysis, and the sponge grease that deposits washs dry post analysis composition.Handle the composition of qualifying liquid and see table 3.The sponge grease composition is seen table 4.
Liquid and the composition of handling qualifying liquid behind table 3 deselenization
The composition of table 4 copper sponge
Liquid mixing in 4: 3 by volume behind the beneficiation wastewater of output and the deselenization in embodiment 3, the metallurgy of copper flow process, the mixed solution composition that obtains is as shown in table 5.Adopt Ionac MC-3470 cationic exchange membrane that liquid pool and electrolyzer are divided into cathode compartment and anolyte compartment respectively.The electrolysis temperature of liquid pool and electrolyzer is water-bath (30 ℃), and current density is 825A/m
2, electrolysing period is 2.5 hours, and anode all adopts Graphite Electrodes, and negative electrode all adopts the 316L stainless steel electrode.Mixed solution is as the catholyte of liquid pool, and anolyte is for containing 10g/L Cu
2+With 273g/L H
2SO
4Solution, carry out the electrolysis dosing.After the liquid pool electrolysis 2.5 hours, liquid is removed the copper sponge of concentration of valuable metals through filtration under diminished pressure after the electrolysis of cathode compartment, and supernatant (being liquid after the demetalization electrolysis) is for use as the anolyte of electrolyzer.The cathode compartment of electrolyzer is allocated fresh mixed solution into, and the anolyte compartment allocates liquid after the demetalization electrolysis into.After 2.5 hours, anolyte compartment's solution is analyzed composition as handling qualifying liquid through electrolysis, and cathode chamber solution is removed copper sponge through filtration under diminished pressure, and liquid send follow-up electrolytic anolyte compartment after the demetalization electrolysis, and the sponge grease that deposits washs dry post analysis composition.Handle the composition of qualifying liquid and see table 5.The sponge grease composition is seen table 6.
Table 5 mixed solution and the composition of handling qualifying liquid
The composition of table 6 copper sponge
Claims (5)
1. an electrolysis with ion-exchange film method of handling chloracid wastewater in the metallurgy of copper flow process is characterized in that step is following: 1. adopt ion-exchange membrane to separate the solution of cathode compartment and anolyte compartment; 2. the chloracid wastewater is as cathode chamber solution, and valuable metal ions such as copper wherein, tellurium are enriched in settling through cathodic reduction; 3. after cathode compartment has deposited the waste water filtering of valuable metal as anolyte compartment's solution, cl ions wherein removes with the chlorine form through anodic oxidation; 4. the anolyte compartment's solution after the electrolysis is the sulphuric acid soln of final output.
2. the electrolysis with ion-exchange film method of chloracid wastewater in the processing metallurgy of copper flow process according to claim 1 is characterized in that: described ion-exchange membrane is heterogeneous cationic exchange membranes such as Ionac MC-3470 cationic exchange membrane or ULTREX CMI-7000 cationic exchange membrane.
3. the electrolysis with ion-exchange film method of chloracid wastewater in the processing metallurgy of copper flow process according to claim 1 is characterized in that: the anode that said anolyte compartment adopts is that to analyse the low and ruthenium iridium that overpotential for oxygen evolution is higher of chlorine overpotential be a kind of in the noble electrodes such as coated titanium net/plate or Graphite Electrodes; The negative electrode that said cathode compartment adopts is a kind of in Graphite Electrodes, copper electrode, titanium electrode or the stainless steel electrode.
4. the electrolysis with ion-exchange film method of chloracid wastewater in the processing metallurgy of copper flow process according to claim 1; It is characterized in that: handled chloracid wastewater is one or more the heavy metal wastewater thereby that contains in copper, selenium, tellurium, lead, arsenic, antimony, bismuth, silver or the gold; Wherein cl concn is not less than 0.1g/L, and sulfuric acid concentration is 0 ~ 400g/L.
5. the electrolysis with ion-exchange film method of chloracid wastewater in the processing metallurgy of copper flow process according to claim 1 is characterized in that: the current density that 4. step adopts in the electrolytic process is 100 ~ 1000A/m
2, temperature is 25 ~ 65 ℃.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399187A (en) * | 2015-11-20 | 2016-03-16 | 扬州祥发资源综合利用有限公司 | Method for resource utilization of steel wire rope pickling waste liquor |
| CN106587452A (en) * | 2016-12-30 | 2017-04-26 | 云南省环境科学研究院(中国昆明高原湖泊国际研究中心) | Method for treating arsenic-containing wastewater by ionic membrane electrolysis |
| CN108101163A (en) * | 2017-12-21 | 2018-06-01 | 衢州华友钴新材料有限公司 | It is a kind of that valuable metal is recycled from industrial wastewater and drops ammonia nitrogen and the method for COD |
| CN108531914A (en) * | 2018-06-15 | 2018-09-14 | 哈尔滨工业大学深圳研究生院 | A kind of H2SO4/S2O82-The copper of microetch waste liquid recycles and synchronizing regeneration micro etching solution system and method |
| CN108726740A (en) * | 2018-06-11 | 2018-11-02 | 山东龙安泰环保科技有限公司 | A kind of high sodium chloride waste water Zero discharge treatment method |
| CN108823420A (en) * | 2018-07-06 | 2018-11-16 | 陕西瑞凯环保科技有限公司 | The method of chlorine is removed in a kind of metallurgical slag |
| CN110182908A (en) * | 2019-05-13 | 2019-08-30 | 浙江大学 | A kind of expanded graphite electrode and its preparation method and application for the removal of heavy metal ions in wastewater electrochemistry |
| CN110872651A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院过程工程研究所 | Method for removing chloride ions in chlorine-containing sulfuric acid solution by adopting fluidized bed electrode |
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| CN105399187A (en) * | 2015-11-20 | 2016-03-16 | 扬州祥发资源综合利用有限公司 | Method for resource utilization of steel wire rope pickling waste liquor |
| CN105399187B (en) * | 2015-11-20 | 2018-06-15 | 扬州祥发资源综合利用有限公司 | A kind of method of recycling steel wire rope pickle liquor |
| CN106587452A (en) * | 2016-12-30 | 2017-04-26 | 云南省环境科学研究院(中国昆明高原湖泊国际研究中心) | Method for treating arsenic-containing wastewater by ionic membrane electrolysis |
| CN108101163A (en) * | 2017-12-21 | 2018-06-01 | 衢州华友钴新材料有限公司 | It is a kind of that valuable metal is recycled from industrial wastewater and drops ammonia nitrogen and the method for COD |
| CN108101163B (en) * | 2017-12-21 | 2020-11-03 | 衢州华友钴新材料有限公司 | Method for recovering valuable metals and reducing ammonia nitrogen and COD (chemical oxygen demand) from industrial wastewater |
| CN108726740A (en) * | 2018-06-11 | 2018-11-02 | 山东龙安泰环保科技有限公司 | A kind of high sodium chloride waste water Zero discharge treatment method |
| CN108531914A (en) * | 2018-06-15 | 2018-09-14 | 哈尔滨工业大学深圳研究生院 | A kind of H2SO4/S2O82-The copper of microetch waste liquid recycles and synchronizing regeneration micro etching solution system and method |
| CN108823420A (en) * | 2018-07-06 | 2018-11-16 | 陕西瑞凯环保科技有限公司 | The method of chlorine is removed in a kind of metallurgical slag |
| CN110872651A (en) * | 2018-09-04 | 2020-03-10 | 中国科学院过程工程研究所 | Method for removing chloride ions in chlorine-containing sulfuric acid solution by adopting fluidized bed electrode |
| CN110182908A (en) * | 2019-05-13 | 2019-08-30 | 浙江大学 | A kind of expanded graphite electrode and its preparation method and application for the removal of heavy metal ions in wastewater electrochemistry |
| CN110182908B (en) * | 2019-05-13 | 2021-04-06 | 浙江大学 | Expanded graphite electrode for electrochemically removing heavy metal ions in wastewater and preparation method and application thereof |
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