CN113754122B - Process for removing sodium by returning electroplating heavy metal ions to tank - Google Patents

Process for removing sodium by returning electroplating heavy metal ions to tank Download PDF

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Publication number
CN113754122B
CN113754122B CN202111101839.0A CN202111101839A CN113754122B CN 113754122 B CN113754122 B CN 113754122B CN 202111101839 A CN202111101839 A CN 202111101839A CN 113754122 B CN113754122 B CN 113754122B
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heavy metal
electroplating
metal ions
column
volume
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CN113754122A (en
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袁华
周保学
袁玥文
李金花
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Nanjing Kunteng Chemical Technology Co ltd
Shanghai Jiaotong University
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Nanjing Kunteng Chemical Technology Co ltd
Shanghai Jiaotong University
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/16—Regeneration of process solutions
    • C25D21/18—Regeneration of process solutions of electrolytes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
    • C02F2001/425—Treatment of water, waste water, or sewage by ion-exchange using cation exchangers
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/14—Maintenance of water treatment installations
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/16—Regeneration of sorbents, filters
    • 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

Abstract

A process for removing sodium from the plated heavy metal ions in a tank includes collecting the waste water containing plated heavy metal ions, coarse filtering, fine filtering, passing the solution of heavy metal ions through a sodium-type weakly acidic cation exchange resin column, and exchanging and adsorbing heavy metal ions; after adsorption saturation, eluting the cation exchange column by dilute acid and concentrated acid respectively, collecting the effluent liquid of heavy metal ions, and returning the effluent liquid to an electroplating process line for use after concentration. The invention can greatly reduce the concentration of sodium ions and free acid in the bath solution, and meets the requirement of the stability of the use of the electroplating heavy metal ions in the bath.

Description

Process for removing sodium by returning electroplating heavy metal ions to tank
Technical Field
The invention relates to a technology in the field of electroplating heavy metal and water recovery, in particular to a process for removing sodium by returning electroplating heavy metal ions to a tank.
Background
The electroplating industry is one of industries with serious environmental pollution, in particular to the pollution of heavy metal wastewater. The existing electroplating heavy metal wastewater is mainly treated at the tail end of an electroplating line by adopting modes such as flocculation precipitation and the like, so that a large amount of hazardous waste sludge is generated, and the problems of great resource waste and high treatment cost are caused; the effluent of the end treatment technology contains particles and higher salt concentration, and membrane pollution is easily caused, so that the recovery efficiency of subsequent membrane separation water is low and the service life of the membrane is reduced.
Various electroplating wastewater heavy metal recycling technologies are developed in the prior art, but the purpose of the technologies is only to recycle the heavy metal ions at the tail end of the electroplating line, and the heavy metal ions are not directly recycled to the electroplating line, so the recovered heavy metal ions generally need to be further separated and purified to be made into inorganic salts, metals and other materials, and the process involves new energy consumption and chemical substance consumption, and can generate new environmental pollution problems. For example, in the prior art, the process for recovering heavy metal and water by an ion exchange-nanofiltration membrane-electrolysis combined process is complex, but the process for recovering heavy metal ions by an electrochemical deposition method is also limited by the problems of low concentration of heavy metal ions in wastewater, high energy consumption, serious side reaction, low recovery rate of heavy metal ions, difficulty in standard-reaching discharge of the treated wastewater and the like. The in-situ separation and on-line recycling of heavy metal ions and water are realized on an electroplating production line, the pollution of electroplating wastewater can be fundamentally eliminated with the lowest energy consumption and the lowest material consumption, the resource utilization of the electroplating wastewater is realized, and the method is the best way for realizing the pollution control of the electroplating wastewater. In the prior art, heavy metal ions and water in electroplating wastewater can be recovered through ion exchange, the water can be directly reused for an electroplating line, the heavy metal ions are further concentrated for reusing the electroplating line, but the heavy metal ion solution separated by the prior ion exchange technology contains sodium ions with higher concentration and free acid; as the recycling time is prolonged, sodium ions and free acid are accumulated in the electroplating bath continuously, the excessive sodium ions can cause the loosening of the plating layer and the deterioration of corrosion resistance, and the excessive free acid can influence the pH value of the electroplating solution and the like, thereby seriously influencing the quality of the electroplating layer. Therefore, the problem of sodium ions and free acid in the recycled heavy metal ion solution is solved, and the problem is the key problem of stable recycling of the heavy metal ions of the electroplating line.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a process for removing sodium by returning electroplating heavy metal ions to a tank, which can greatly reduce the concentration of sodium ions and free acid in the liquid returning to the tank and meet the requirement of the stability of the use of the electroplating heavy metal ions returning to the tank.
The invention is realized by the following technical scheme:
the invention relates toA process for removing sodium from the plated heavy metal ions in a tank includes collecting the waste water containing plated heavy metal ions, coarse filtering, fine filtering, passing the solution of heavy metal ions through a sodium-type weakly acidic cation exchange resin column, and exchanging and adsorbing heavy metal ions; after saturation, dilute H of 0.5-1% is used 2 SO 4 Eluting cation exchange column with eluent in countercurrent at elution rate of 0.5-0.75 times column volume/h and volume of 1.5-2 times column volume; then using 8-12% of 2 SO 4 And (3) performing countercurrent elution for an eluent at an elution rate of 2-3 times the column volume/h, collecting the effluent of the heavy metal ions, and returning the effluent to the electroplating process line for use after concentration.
The heavy metal ion includes but is not limited to Cu 2+ 、Ni 2+ 、Zn 2+ And (3) plasma.
Technical effects
Compared with the prior art, the method collects the effluent of heavy metal ions, has low sodium ion content and free acid content, does not influence the stability of the electroplating process, and can be directly recycled in a production line after evaporation and concentration.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention.
Detailed Description
Example 1
The embodiment relates to a process for removing sodium by returning electroplating heavy metal ions to a tank, which comprises the following steps: collecting copper-containing rinsing wastewater and Cu in electroplating production line 2+ The concentration is 102mg/L, after filtration, cu < 2+ > wastewater ions enter a 110 sodium type weak acid cation exchange resin column for ion exchange, and the sodium type weak acid cation exchange resin column adsorbs Cu in a saturated mode 2+ After ionization, washing, first with 0.75% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 1.75 times of the column volume, and the elution rate is 0.65 times of the column volume/h; thereafter adopting 10% of 2 SO 4 Eluting with eluent in countercurrent at flow rate of 2.5 times of column volume/h, and collecting the eluate containing Cu 2+ The ion effluent is concentrated and then returns to the electroplating process line for use.
Example Cu 2+ Ion effluent, cu 2+ The concentration of the mixed solution is 28g/L,Na + ＜1mg/L，pH 6.0。
comparative example 1
The comparative example includes the following steps: collecting copper-containing rinsing wastewater and Cu in electroplating production line 2+ The concentration is 102mg/L, after filtration, the wastewater enters an ion exchange column system for adsorption exchange, wherein Cu in the wastewater 2+ Ion exchange with 110 sodium type weakly acidic cation exchange resin, washing, and directly adopting 10% H 2 SO 4 Eluting with eluent at flow rate and volume 2.5 times of column volume/h, and collecting Cu-containing solution 2+ And (4) ion effluent.
Comparative example Cu 2+ Ion effluent, cu 2+ The concentration of Na is 28.5g/L + 350mg/L，pH＜2.0。
Comparative example 2
The comparative example includes the following steps: collecting copper-containing rinsing wastewater and Cu in electroplating production line 2+ The concentration is 102mg/L, after filtration, the wastewater enters an ion exchange column system for adsorption exchange, wherein Cu in the wastewater 2+ Ion exchange is carried out between ions and 110 sodium type weak acid cation exchange resin, and Cu is adsorbed by saturation of a sodium type weak acid cation exchange resin column 2+ After ionization, washing, first with 3% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 1.75 times of the column volume, and the elution rate is 0.65 times of the column volume/h, so as to obtain an effluent A; thereafter adopt 10% H 2 SO 4 Eluting with eluent at flow rate and volume 2.5 times of column volume/h, and collecting Cu-containing solution 2+ And (6) ion effluent liquid B.
The control example flowed out Cu in the solution A 2+ The concentration is more than or equal to 6g/L; cu in effluent B 2+ Concentration 24g/L, na + 150mg/L，pH＜3.0。
Comparative example 3
The comparative example comprises the following steps: collecting copper-containing rinsing wastewater and Cu in electroplating production line 2+ The concentration is 102mg/L, after filtration, the wastewater enters an ion exchange column system for adsorption exchange, wherein the Cu in the wastewater 2+ Ion exchange with 110 sodium type weak acidic cation exchange resin, sodium type weak acidic cation exchangeSaturated adsorption of Cu by resin column 2+ After ionization, washing, first with 0.75% dilute H 2 SO 4 Carrying out countercurrent elution for an eluent, wherein the elution volume is 1.75 times of the column volume, and the elution rate is 3 times of the column volume/h, so as to obtain an effluent liquid A; thereafter adopt 10% H 2 SO 4 Eluting with eluent at flow rate and volume 2.5 times of column volume/h, and collecting Cu-containing solution 2+ And (4) ion effluent liquid B.
Cu in effluent B of this control example 2+ Concentration 27g/L, na + 70mg/L，pH 6.0。
Example 2
The embodiment specifically comprises the following steps: collecting nickel-containing rinsing wastewater, ni, of electroplating production line 2+ Concentration 118mg/L, after filtration, ni 2+ The wastewater enters a 116 sodium type weak acid cation exchange resin column for ion exchange, and the 116 sodium type weak acid cation exchange resin column adsorbs Ni in a saturated way 2+ After ionization, washing, first with 0.5% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 1.5 times of the column volume, and the elution rate is 0.5 times of the column volume/h; thereafter adopting 10% of 2 SO 4 Eluting with eluent at flow rate 2 times of column volume/h, and collecting Ni-containing solution 2+ And concentrating the ion effluent liquid and returning the concentrated ion effluent liquid to an electroplating process line for use.
Example Ni 2+ Ion effluent, ni 2+ Concentration 30g/L, na + ＜1mg/L，pH 6.5。
Comparative example 4
The comparative example includes the following steps: collecting nickel-containing rinsing wastewater, ni, of electroplating production line 2+ At a concentration of 118mg/L, filtered, ni 2+ The wastewater enters a 116 sodium type weak acid cation exchange resin column for ion exchange, and the 116 sodium type weak acid cation exchange resin column adsorbs Ni in a saturated way 2+ After ionization, washing, first with 0.5% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 1.5 times of the column volume, and the elution rate is 0.5 times of the column volume/h; thereafter adopt 20% H 2 SO 4 Eluting with eluent at flow rate 2 times of column volume/h, and collecting Ni-containing solution 2+ Concentrating the ion effluent, and returning to electroplatingThe process line is used.
Comparative example Ni 2+ Ion effluent, ni 2+ Concentration 29g/L, na + ＜1mg/L，pH＜1。
Comparative example 5
The comparative example includes the following steps: collecting nickel-containing rinsing wastewater, ni, of electroplating production line 2+ At a concentration of 118mg/L, filtered, ni 2+ The wastewater enters a 116 sodium type weak acid cation exchange resin column for ion exchange, and the 116 sodium type weak acid cation exchange resin column adsorbs Ni in a saturated way 2+ After ionization, washing, first with 0.5% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 1.5 times of the column volume, and the elution rate is 0.5 times of the column volume/h; thereafter adopt 5% of 2 SO 4 Eluting with eluent at flow rate 2 times of column volume/h, and collecting Ni-containing solution 2+ The ion effluent is concentrated and then returns to the electroplating process line for use.
Comparative example Ni 2+ Ion effluent, ni 2+ The concentration of Na is 14g/L + ＜1mg/L，pH 6。
Example 3
The embodiment specifically comprises the following steps: collecting zinc-containing rinsing wastewater, zn, of the electroplating production line 2+ Concentration 121mg/L, after filtration, zn 2+ The ion wastewater enters a D152 sodium type weak acid cation exchange resin column for ion exchange, and the D152 sodium type weak acid cation exchange resin column adsorbs Zn in a saturated way 2+ After ionization, washing, first with 1% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 2 times of the column volume, and the elution rate is 0.75 times of the column volume/h; thereafter adopt 10% H 2 SO 4 Eluting with eluent at flow rate 3 times of column volume/h, and collecting Zn 2+ The ion effluent is concentrated and then returns to the electroplating process line for use.
Example Zn 2+ Ion effluent, zn 2+ Concentration 31g/L, na + ＜1mg/L，pH 6.5。
In conclusion, the weak acid cation exchange resin adopted by the invention has the strong and weak order of adsorption on cations of H + ＞＞Cu 2+ ＞Zn 2+ ＞Ni 2+ ＞＞Na + When the resin is exchanged with the plating waste water, heavy metal ions (e.g., cu) 2+ ) Is easy to react with Na + The exchange and the adsorption are favorable for obtaining higher heavy metal ion exchange efficiency, so that the concentration of the heavy metal ions in the elution effluent is high. On the other hand, due to the presence of ion exchange defects, a certain amount of Na will be present in the column + Is not exchanged but remains in the column, and Na is contained + Will be eluted together with heavy metal ions, resulting in the return of the bath solution Na + High content, and influence the quality of heavy metal ion returning. Before the heavy metal ions are eluted, the invention adopts low-concentration H + Eluting the column with a concentration (dilute sulphuric acid 0.5-1%) and controlling the slow elution rate (0.5-0.75 column volume/H) and elution time (elution volume 1.5-2 column volumes) to form H + Exchange for Na only + Without exchanging the dynamic equilibrium of heavy metal ions and letting Na + Fully exchange to realize heavy metal ions and Na in the exchange column + Separation of (1); after this, high concentrations of sulfuric acid (8-12% H) are used 2 SO 4 ) As eluent, from high concentration of H + Exchanging heavy metal ions to obtain high-purity heavy metal ion effluent, and evaporating and concentrating the heavy metal ion effluent for returning to the tank.
Due to the ion exchange resin used in the process, for H + Has strong adsorption capacity, avoids heavy metal ions and H + The exchange is incomplete in the exchange process, and a large amount of acid-washing stripping agent flows out, so that the concentration of free acid in the liquid returned to the tank is too high, and the concentration of heavy metal ions is low.
The foregoing embodiments may be modified in many different ways by one skilled in the art without departing from the spirit and scope of the invention, which is defined by the appended claims and not by the preceding embodiments, and all embodiments within their scope are intended to be limited by the scope of the invention.

Claims (5)

1. A process for removing sodium from the electroplating heavy metal ions in the tank includes collecting the waste water containing electroplating heavy metal ions, coarse filtering, fine filtering, and passing the solution of heavy metal ions through a filterA sodium weak acid cation exchange resin column for exchanging and adsorbing heavy metal ions; after saturation, dilute H with 0.5-1% concentration is used 2 SO 4 Eluting the cation exchange column with eluent in countercurrent at an elution rate of 0.5-0.75 times column volume/h and an elution volume of 1.5-2 times column volume; then using 8-12% of 2 SO 4 Eluting with eluent at 2-3 times of column volume/h, collecting heavy metal ion effluent, concentrating, and returning to electroplating line.
2. A process as claimed in claim 1, wherein said heavy metal ions comprise: cu 2+ 、Ni 2+ 、Zn 2+ 。
3. The process for removing sodium in an electroplating heavy metal ion return tank as claimed in claim 1 or 2, which is characterized by comprising the following steps: collecting copper-containing rinsing wastewater and Cu in electroplating production line 2+ Concentration 102mg/L, after filtration, cu 2+ The wastewater ions enter a 110 sodium type weak acid cation exchange resin column for ion exchange, and the sodium type weak acid cation exchange resin column adsorbs Cu in a saturated way 2+ After ionization, washing, first with 0.75% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 1.75 times of the column volume, and the elution rate is 0.65 times of the column volume/h; thereafter adopt 10% H 2 SO 4 Eluting with eluent at flow rate and volume 2.5 times of column volume/h, and collecting Cu-containing solution 2 + The ion effluent is concentrated and then returns to the electroplating process line for use.
4. The electroplating heavy metal ion sodium removal process by returning to the tank as claimed in claim 1 or 2, which is characterized by comprising the following steps: collecting nickel-containing rinsing wastewater and Ni in electroplating production line 2+ Concentration 118mg/L, after filtration, ni 2+ The wastewater enters a 116 sodium type weak acid cation exchange resin column for ion exchange, and the 116 sodium type weak acid cation exchange resin column adsorbs Ni in a saturated way 2+ After ionization, washing, first with 0.5% dilute H 2 SO 4 The elution is carried out in a counter-current way for the eluent,the elution volume is 1.5 times of the column volume, and the elution rate is 0.5 times of the column volume/h; thereafter adopting 10% of 2 SO 4 Eluting with eluent at flow rate 2 times of column volume/h, and collecting Ni-containing solution 2+ The ion effluent is concentrated and then returns to the electroplating process line for use.
5. The process as claimed in claim 1 or 2, wherein the zinc-containing rinsing wastewater from the electroplating production line, zn, is collected 2+ At a concentration of 121mg/L, filtered, zn 2+ The ion wastewater enters a D152 sodium type weak acid cation exchange resin column for ion exchange, and the D152 sodium type weak acid cation exchange resin column adsorbs Zn in a saturated manner 2+ After ionization, washing, first with 1% dilute H 2 SO 4 Carrying out countercurrent elution for the eluent, wherein the elution volume is 2 times of the column volume, and the elution rate is 0.75 times of the column volume/h; thereafter adopt 10% H 2 SO 4 Eluting with eluent at flow rate 3 times of column volume/h, and collecting Zn 2+ And concentrating the ion effluent liquid and returning the concentrated ion effluent liquid to an electroplating process line for use.
CN202111101839.0A 2021-09-18 2021-09-18 Process for removing sodium by returning electroplating heavy metal ions to tank Active CN113754122B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101746906A (en) * 2008-12-03 2010-06-23 五邑大学 Method for processing electroplating wastewater with heavy metal ions
CN201660466U (en) * 2010-03-19 2010-12-01 深圳市山水乐环保科技有限公司 Online recycling and treatment system for electroplating waste water containing heavy metal ions
CN102766059A (en) * 2011-05-05 2012-11-07 重庆紫光化工股份有限公司 Method for preparing high-purity iminodiacetic acid
CN103713063A (en) * 2013-12-31 2014-04-09 中华人民共和国湖北出入境检验检疫局 Method for simultaneously and rapidly detecting contents of multiple heavy metal elements in salt

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101746906A (en) * 2008-12-03 2010-06-23 五邑大学 Method for processing electroplating wastewater with heavy metal ions
CN201660466U (en) * 2010-03-19 2010-12-01 深圳市山水乐环保科技有限公司 Online recycling and treatment system for electroplating waste water containing heavy metal ions
CN102766059A (en) * 2011-05-05 2012-11-07 重庆紫光化工股份有限公司 Method for preparing high-purity iminodiacetic acid
CN103713063A (en) * 2013-12-31 2014-04-09 中华人民共和国湖北出入境检验检疫局 Method for simultaneously and rapidly detecting contents of multiple heavy metal elements in salt

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