CN112458310A - Method for extracting zinc salt from zinc-containing wastewater - Google Patents

Method for extracting zinc salt from zinc-containing wastewater Download PDF

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Publication number
CN112458310A
CN112458310A CN202011340590.4A CN202011340590A CN112458310A CN 112458310 A CN112458310 A CN 112458310A CN 202011340590 A CN202011340590 A CN 202011340590A CN 112458310 A CN112458310 A CN 112458310A
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zinc
solution
extracting
leaching
cobalt
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CN202011340590.4A
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Inventor
唐烷家
王兵
姜术丹
兰伟宝
熊丁丁
高磊
付敏波
彭善俊
张文涛
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Sateri Jiujiang Fiber Co ltd
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Sateri Jiujiang Fiber Co ltd
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Priority to CN202011340590.4A priority Critical patent/CN112458310A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/30Obtaining zinc or zinc oxide from metallic residues or scraps
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00Obtaining zinc or zinc oxide
    • C22B19/20Obtaining zinc otherwise than by distilling
    • C22B19/26Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Water Supply & Treatment (AREA)
  • Hydrology & Water Resources (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention aims to provide a method for extracting zinc salt from zinc-containing wastewater, which comprises the following steps: (1) adding a sodium polyacrylate mixture into the zinc-containing wastewater, and stirring to obtain a first solution; (2) adding caustic soda into the first solution, and stirring to obtain a second solution; (3) adding sodium carbonate and hydrogen peroxide into the second solution to obtain a third solution; (4) carrying out biological adsorption on the third solution, and filtering to obtain filter residue; (5) mixing the filter residue leaching agents, and standing for 5 hours to obtain a zinc-containing leaching solution; the method comprises the steps of firstly obtaining filter residues containing zinc through multi-stage treatment and filtration, then further treating the filter residues, and extracting the zinc-containing composition from the filter residues through extraction, thereby extracting the zinc-containing extract under the condition of ensuring that pollutants are cleaned by waste water.

Description

Method for extracting zinc salt from zinc-containing wastewater
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to a method for extracting zinc salt from zinc-containing wastewater.
Background
Zinc is a heavy metal resource which is abundant on the earth. The reserves of zinc ore resources in China are the second place in the world, and the zinc resources are widely applied to modern industrial production, such as smelting, pharmacy and food industries. Zinc is an indispensable element for human health, widely exists in human muscles and bones, but the content of zinc is very small, and serious consequences can occur if the zinc is in excess. The discharge of the zinc-containing wastewater has serious harm to human health and industrial and agricultural activities, has the characteristics of persistence, high toxicity, serious pollution and the like, once the wastewater enters the environment, the wastewater cannot be biodegraded, most of the wastewater participates in food chain circulation, and finally is accumulated in organisms to destroy normal physiological metabolic activities of the organisms, so that the human health is harmed.
The inventor finds that when the zinc-containing wastewater is treated, waste residues are obtained by treatment, and then the waste residues containing zinc are directly discarded, so that an effective method for recovering the zinc is not available.
Disclosure of Invention
In view of the problems in the prior art, the present invention is directed to one of the problems set forth above. The method for extracting zinc salt from zinc-containing wastewater comprises the following steps: (1) adding a sodium polyacrylate mixture into the zinc-containing wastewater, and stirring to obtain a first solution; (2) adding caustic soda into the first solution, and stirring to obtain a second solution; (3) adding sodium carbonate and hydrogen peroxide into the second solution to obtain a third solution; (4) carrying out biological adsorption on the third solution, and filtering to obtain filter residue; (5) mixing the filter residue leaching agents, and standing for 5 hours to obtain a zinc-containing leaching solution; (6) extracting zinc from the leaching solution obtained in the step (5) to obtain zinc salt andextracting zinc mixed liquor, wherein the zinc extraction comprises the following steps: mixing the organic phase with the leaching solution, adding NaCl and CaCl2Standing for 2h, and after layering, separating the liquid from the organic phase to obtain a zinc extraction mixed solution; (7) extracting nickel, cobalt and copper from the zinc extraction mixed solution obtained in the step (6) to obtain corresponding nickel, cobalt and copper salt and raffinate; (8) and (3) using the raffinate obtained in the step (7) as a leaching agent and the extraction method for extracting zinc in the step (6) to obtain the zinc-containing composition.
Preferably, the leaching agent is one or more of formic acid, acetic acid and citric acid.
Preferably, the biosorbent used in the bioadsorbent of step (4) is a mixture of Aspergillus, Penicillium, Trichoderma and sodium polyaminosaccharide phosphate.
Preferably, the organic phase is 15% to 55% by volume: 45-85% of extractant and solvent oil.
Preferably, the solvent oil is one or two of kerosene and sulfonated kerosene.
Preferably, sodium carbonate, hydrogen peroxide and sodium bicarbonate are added into the second solution in the step (3).
Preferably, the extracting agent used for extracting nickel, cobalt and copper in the step (7) is one or more of P204, P507 or Cyanex 272.
Preferably, the weight part ratio of the filter residue to the leaching agent in the step (5) is 1: 10.
p204: p204, Chinese name: bis (2-ethylhexyl) phosphate; bis (2-ethylhexyl) phosphate; diisooctyl phosphate; dioctyl phosphate, national CAS accession number: 298-07-7, is a colorless, transparent, and viscous liquid. Freezing point-60 deg.C, relative density 0.973(25/25 deg.C), refractive index 1.4420(25 deg.C), boiling point 209 deg.C (1.33 kPa). The product is used as an organic solvent, is an acidic extracting agent and is an organic synthesis intermediate. In kerosene, hydrogen-bonded dimer structure is adopted to cover polar phosphate group, and when being complexed with metal ions, the kerosene usually takes part in reaction in dimeric form
Cyanex 272: bis (2,4, 4-trimethylpentyl) phosphonic acid (disooctylphosphinic acid), CAS number: 83411-71-6, EINECS No.: 280-445-7, which is sold as Cyanex272, is an acidic phosphinic acid extractant, originally developed for separating nickel and cobalt, but has excellent extraction performance, and the application range of the extractant is continuously expanded, so that the extractant is used for separating other metal systems.
P507: p-507 chemical name: 2-ethylhexyl phosphate mono-2-ethylhexyl ester, of the formula [ CH3(CH2)3CH (C2H5) CH2O ] [ CH3(CH2)3CH (C2H5) CH2] HPO is a colorless or pale yellow transparent oily liquid.
Has the advantages that: the method comprises the steps of firstly obtaining filter residues containing zinc through multi-stage treatment and filtration, then further treating the filter residues, and extracting the zinc-containing composition from the filter residues through extraction, thereby extracting the zinc-containing extract under the condition of ensuring that pollutants are cleaned by waste water.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for extracting zinc salt from zinc-containing wastewater, which is characterized by comprising the following steps:
(1) adding a sodium polyacrylate mixture into the zinc-containing wastewater, and stirring to obtain a first solution;
(2) adding caustic soda into the first solution, and stirring to obtain a second solution;
(3) adding sodium carbonate and hydrogen peroxide into the second solution to obtain a third solution;
(4) carrying out biological adsorption on the third solution, and filtering to obtain filter residue;
(5) mixing the filter residue leaching agents, and standing for 5 hours to obtain a zinc-containing leaching solution;
(6) extracting zinc from the leaching solution obtained in the step (5) to obtain zinc salt and zinc extraction mixed solution,
the zinc extraction comprises the following steps: mixing the organic phase with the leaching solution, adding NaCl and CaCl2Standing for 2h, and after layering, separating the liquid from the organic phase to obtain a zinc extraction mixed solution;
(7) extracting nickel, cobalt and copper from the zinc extraction mixed solution obtained in the step (6), wherein an organic phase is used for extracting nickel, cobalt and copper to obtain corresponding nickel, cobalt and copper salt and raffinate;
(8) and (3) using the raffinate obtained in the step (7) as a leaching agent and the extraction method for extracting zinc in the step (6) to obtain the zinc-containing composition.
The leaching agent is formic acid, and the organic phase is 15% by volume: 85% of extractant and solvent oil, and the extractant used for extracting the nickel, cobalt and copper in the step (7) is P204.
Example 2
A method for extracting zinc salt from zinc-containing wastewater, which is characterized by comprising the following steps:
(1) adding a sodium polyacrylate mixture into the zinc-containing wastewater, and stirring to obtain a first solution;
(2) adding caustic soda into the first solution, and stirring to obtain a second solution;
(3) adding sodium carbonate, hydrogen peroxide and sodium bicarbonate into the second solution to obtain a third solution;
(4) carrying out biological adsorption on the third solution, and filtering to obtain filter residue;
(5) mixing the filter residue leaching agents, and standing for 5 hours to obtain a zinc-containing leaching solution;
(6) extracting zinc from the leaching solution obtained in the step (5) to obtain zinc salt and zinc extraction mixed solution,
the zinc extraction comprises the following steps: mixing the organic phase with the leaching solution, adding NaCl and CaCl2Standing for 2h, and after layering, separating the liquid from the organic phase to obtain a zinc extraction mixed solution;
(7) extracting nickel, cobalt and copper from the zinc extraction mixed solution obtained in the step (6), wherein an organic phase is used for extracting nickel, cobalt and copper to obtain corresponding nickel, cobalt and copper salt and raffinate;
(8) and (3) using the raffinate obtained in the step (7) as a leaching agent and the extraction method for extracting zinc in the step (6) to obtain the zinc-containing composition.
The leaching agent is citric acid, and the organic phase is a mixture of the following components in a volume ratio of 55%: 45% of extracting agent and solvent oil, wherein the extracting agent used for extracting the nickel, cobalt and copper in the step (7) is P204 and P507. .
Example 3
A method for extracting zinc salt from zinc-containing wastewater, which is characterized by comprising the following steps:
(1) adding a sodium polyacrylate mixture into the zinc-containing wastewater, and stirring to obtain a first solution;
(2) adding caustic soda into the first solution, and stirring to obtain a second solution;
(3) adding sodium carbonate and hydrogen peroxide into the second solution to obtain a third solution;
(4) carrying out biological adsorption on the third solution, and filtering to obtain filter residue;
(5) mixing the filter residue leaching agents, and standing for 5 hours to obtain a zinc-containing leaching solution;
(6) extracting zinc from the leaching solution obtained in the step (5) to obtain zinc salt and zinc extraction mixed solution,
the zinc extraction comprises the following steps: mixing the organic phase with the leaching solution, adding NaCl and CaCl2Standing for 2h, and after layering, separating the liquid from the organic phase to obtain a zinc extraction mixed solution;
(7) extracting nickel, cobalt and copper from the zinc extraction mixed solution obtained in the step (6), wherein an organic phase is used for extracting nickel, cobalt and copper to obtain corresponding nickel, cobalt and copper salt and raffinate;
(8) and (3) using the raffinate obtained in the step (7) as a leaching agent and the extraction method for extracting zinc in the step (6) to obtain the zinc-containing composition.
The leaching agent is citric acid, and the organic phase is a mixture of the following components in a volume ratio of 55%: 85 percent of extractant and solvent oil, and the extractant used for extracting the nickel, cobalt and copper in the step (7) is Cyanex 272. .
Example 4
A method for extracting zinc salt from zinc-containing wastewater, which is characterized by comprising the following steps:
(1) adding a sodium polyacrylate mixture into the zinc-containing wastewater, and stirring to obtain a first solution;
(2) adding caustic soda into the first solution, and stirring to obtain a second solution;
(3) adding sodium carbonate and hydrogen peroxide into the second solution to obtain a third solution;
(4) carrying out biological adsorption on the third solution, and filtering to obtain filter residue;
(5) mixing the filter residue leaching agents, and standing for 5 hours to obtain a zinc-containing leaching solution;
(6) extracting zinc from the leaching solution obtained in the step (5) to obtain zinc salt and zinc extraction mixed solution,
the zinc extraction comprises the following steps: mixing the organic phase with the leaching solution, adding NaCl and CaCl2Standing for 2h, and after layering, separating the liquid from the organic phase to obtain a zinc extraction mixed solution;
(7) extracting nickel, cobalt and copper from the zinc extraction mixed solution obtained in the step (6), wherein an organic phase is used for extracting nickel, cobalt and copper to obtain corresponding nickel, cobalt and copper salt and raffinate;
(8) and (3) using the raffinate obtained in the step (7) as a leaching agent and the extraction method for extracting zinc in the step (6) to obtain the zinc-containing composition.
The leaching agent is formic acid, and the organic phase is 15-55% by volume: 45% -85% of an extracting agent and solvent oil, wherein the extracting agent used for extracting the nickel, cobalt and copper in the step (7) is P204. .
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (8)

1. A method for extracting zinc salt from zinc-containing wastewater, which is characterized by comprising the following steps:
(1) adding a sodium polyacrylate mixture into the zinc-containing wastewater, and stirring to obtain a first solution;
(2) adding caustic soda into the first solution, and stirring to obtain a second solution;
(3) adding sodium carbonate and hydrogen peroxide into the second solution to obtain a third solution;
(4) carrying out biological adsorption on the third solution, and filtering to obtain filter residue;
(5) mixing the filter residue leaching agents, and standing for 5 hours to obtain a zinc-containing leaching solution;
(6) extracting zinc from the leaching solution obtained in the step (5) to obtain zinc salt and zinc extraction mixed solution,
the zinc extraction comprises the following steps: mixing the organic phase with the leaching solution, adding NaCl and CaCl2Standing for 2h, and after layering, separating the liquid from the organic phase to obtain a zinc extraction mixed solution;
(7) extracting nickel, cobalt and copper from the zinc extraction mixed solution obtained in the step (6), wherein an organic phase is used for extracting nickel, cobalt and copper to obtain corresponding nickel, cobalt and copper salt and raffinate;
(8) and (3) using the raffinate obtained in the step (7) as a leaching agent and the extraction method for extracting zinc in the step (6) to obtain the zinc-containing composition.
2. The method of claim 1, wherein the leaching agent is one or more of formic acid, acetic acid, and citric acid.
3. The method according to claim 1, wherein the biosorbent used in the bioadsorbent of step (4) is a mixture of Aspergillus, Penicillium, Trichoderma and sodium polyaminosaccharide phosphate.
4. The process according to claim 1, characterized in that the organic phase is 15-55% by volume: 45-85% of extractant and solvent oil.
5. The method of claim 4, wherein the mineral spirit is one or both of kerosene and sulfonated kerosene.
6. The method of claim 1, wherein step (3) adds sodium carbonate, hydrogen peroxide, and sodium bicarbonate to the second solution.
7. The method according to claim 1, wherein the extracting agent used in the step (7) for extracting nickel, cobalt and copper is one or more of P204, P507 or Cyanex 272.
8. The method according to claim 1, wherein the weight part ratio of the filter residue to the leaching agent in the step (5) is 1: 10.
CN202011340590.4A 2020-11-25 2020-11-25 Method for extracting zinc salt from zinc-containing wastewater Pending CN112458310A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113373309A (en) * 2021-05-13 2021-09-10 浙江省遂昌金矿有限公司 Process for recovering zinc from gold cyanide mud acid pickling waste liquid

Citations (5)

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Publication number Priority date Publication date Assignee Title
CN1148999A (en) * 1995-10-20 1997-05-07 东国制药株式会社 Biosorbent for heavy metals prepared from biomass
CN101130158A (en) * 2006-08-21 2008-02-27 中国科学院生态环境研究中心 Biological adsorption agent, producing method and use of the same
EP1997919A1 (en) * 2007-05-24 2008-12-03 Paul Wurth S.A. Method of recovering zinc- and sulphate-rich residue
CN107151744A (en) * 2017-04-15 2017-09-12 桂林理工大学 It is a kind of to clean the method for extracting zinc
CN109809622A (en) * 2019-03-28 2019-05-28 长沙埃比林环保科技有限公司 A kind of processing method of zinc-containing water

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1148999A (en) * 1995-10-20 1997-05-07 东国制药株式会社 Biosorbent for heavy metals prepared from biomass
CN101130158A (en) * 2006-08-21 2008-02-27 中国科学院生态环境研究中心 Biological adsorption agent, producing method and use of the same
EP1997919A1 (en) * 2007-05-24 2008-12-03 Paul Wurth S.A. Method of recovering zinc- and sulphate-rich residue
CN107151744A (en) * 2017-04-15 2017-09-12 桂林理工大学 It is a kind of to clean the method for extracting zinc
CN109809622A (en) * 2019-03-28 2019-05-28 长沙埃比林环保科技有限公司 A kind of processing method of zinc-containing water

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Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113373309A (en) * 2021-05-13 2021-09-10 浙江省遂昌金矿有限公司 Process for recovering zinc from gold cyanide mud acid pickling waste liquid

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