CN113264607A - Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid - Google Patents
Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid Download PDFInfo
- Publication number
- CN113264607A CN113264607A CN202110525187.7A CN202110525187A CN113264607A CN 113264607 A CN113264607 A CN 113264607A CN 202110525187 A CN202110525187 A CN 202110525187A CN 113264607 A CN113264607 A CN 113264607A
- Authority
- CN
- China
- Prior art keywords
- waste liquid
- nickel
- recovery
- nickel plating
- plating waste
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5281—Installations for water purification using chemical agents
-
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- 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
- C02F2001/007—Processes including a sedimentation step
-
- 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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
Abstract
The invention relates to a method for promoting reduction and recovery of high-concentration nickel in chemical nickel plating waste liquid. The method comprises the following steps: firstly, adjusting the pH value of chemical nickel plating waste liquid to 7-11 by using sodium hydroxide to obtain pretreated waste liquid; heating to 40-100 ℃; preparing 10-20% slurry from the accelerator, adding 10-100 mg/L of the dispersant, uniformly stirring, adding the pretreated waste liquid according to the dosage of 50-500 mg/L, and stirring for reaction for 0.5-2 hours at the temperature of 40-100 ℃; and fourthly, after the reaction is finished, adding 10-100 mg/L of flocculating agent, filtering to obtain a nickel metal product and treated waste liquid, wherein the waste liquid after nickel recovery mainly contains phosphite and organic matters, and after phosphorus resource recovery, feeding the waste liquid into a wastewater treatment system. The method has simple process and mild conditions, overcomes the problems of high catalyst cost, low nickel recovery rate and the like in the existing nickel-containing waste liquid resource recovery process, and solves the problems of difficult chemical nickel-plating waste liquid resource recovery and the like.
Description
Technical Field
The invention belongs to the technical field of nickel-containing heavy metal wastewater recovery, and particularly relates to a method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid.
Background
Electroless nickel plating is a nickel deposition process in which nickel ions are reduced by autocatalytic reduction at the metal surface by means of a suitable reducing agent in solution. The chemical nickel plating solution mainly comprises nickel salt, complexing agent, reducing agent and additive. Nickel salt is the main salt of the plating solution, and generally used are nickel sulfate, nickel chloride, nickel acetate, nickel carbonate and the like; commonly used complexing agents generally comprise citrate, glycollate, lactate and the like, and have the functions of enabling nickel ions to generate stable complexes and simultaneously preventing the generation of hydroxide and phosphite; the reducing agent is generally sodium hypophosphite which has the function of providing active hydrogen atoms through catalytic dehydrogenation to reduce nickel ions into metallic nickel.
The chemical nickel plating solution can age gradually after working for a period of time, and can not be used continuously, thus becoming the chemical nickel plating waste liquid. The waste liquid contains a large amount of organic matters such as complexing agents, buffering agents, stabilizing agents and the like besides nickel ions (2-7 g/L nickel), hypophosphite ions and a large amount of phosphite ions (20-200 g/L), sodium ions and sulfate ions, and the waste liquid is very complex in composition, so that the difficulty in treating the waste liquid is increased.
The prior treatment method of the chemical nickel plating waste liquid mainly comprises a chemical precipitation method, a reduction method, an electrolysis method, an ion exchange method, an electrodialysis method, a solvent extraction method and the like. Wherein the chemical precipitation method can generate a large amount of waste residues, which causes the waste of a large amount of high-value metal nickel; the reduction method adopts an expensive palladium chloride catalyst, has the problems of large medicament dosage, high medicament cost and the like, and the nickel recovery rate is only 60-90%; the electrolysis method has the disadvantages of low current efficiency, high energy consumption and the like due to the fact that waste liquid contains a large amount of organic matters. Due to the complexity of the chemical nickel plating waste liquid, a mature, effective, low-cost, low-energy-consumption, simple and feasible treatment method is not formed at present.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to solve the problem that nickel resources cannot be effectively recovered in the conventional chemical nickel waste liquid treatment process, and provides a method for promoting reduction recovery of nickel in chemical nickel plating waste liquid, which has the advantages of simple operation, low cost, high efficiency, reduction of the concentration of residual nickel ions from 2-7 g/L to 10-50 mg/L, and nickel recovery rate of more than 99%.
The technical scheme of the invention is that the method for promoting reduction and recovery of nickel in the chemical nickel plating waste liquid is characterized by comprising the following steps:
firstly, adjusting the pH value of chemical nickel plating waste liquid to 7-11 by using sodium hydroxide to obtain pretreated waste liquid;
heating to 40-100 ℃;
preparing 10-20% slurry from the accelerator, adding 10-100 mg/L of dispersant, uniformly stirring, adding 50-500 mg/L of pretreated waste liquid, controlling the temperature at 40-100 ℃, and stirring for reacting for 0.5-2 hours;
and immediately adding a flocculating agent after the reaction is finished, wherein the addition amount of the flocculating agent is 10-100 mg/L, filtering while the reaction is hot to obtain a nickel metal product and a treated waste liquid, and recovering the nickel to obtain the waste liquid containing phosphite radicals and organic matters and then feeding the waste liquid into a wastewater treatment system after recovering phosphorus resources.
Preferably, the method comprises the following steps: selecting one or the following components in combination as the accelerator: beryllium alloys, aluminum alloys, iron alloys, titanium alloys, cobalt alloys, nickel alloys.
Preferably, the method comprises the following steps: the crystal form of the accelerator is one or any two of a hypoeutectic crystal form, a eutectic crystal form and a hypereutectic crystal form; the grain size range of the accelerator is 1-20 mm.
Preferably, the method comprises the following steps: and step three, the dispersing agent is polyacrylic acid with low molecular weight, and the molecular weight is not more than 5000.
Preferably, the method comprises the following steps: and step four, the flocculant is a high-temperature-resistant PAM-series anionic flocculant and has a molecular weight of more than 1000 ten thousand.
Compared with the prior art, the invention has the beneficial effects that:
the method has the advantages that nickel ions in the chemical nickel plating waste liquid are efficiently recycled, the concentration of the residual nickel ions is reduced to 10-50 mg/L, and the nickel recovery rate is more than 99%; 2. the metal alloy is used as an accelerant to obtain a nickel metal product with the nickel purity of more than 90 percent, and the method is simple to operate, high in product purity and low in cost.
Drawings
FIG. 1 is a process flow chart of the method for promoting reduction and recovery of nickel in the chemical nickel plating waste liquid.
Detailed Description
The invention will be further described in detail with reference to the following examples:
the waste liquid in the embodiment is taken from the waste liquid of a chemical nickel plating plant tank, the concentration of nickel ions is 3.0-5.0 g/L, and the pH value is 3.6-4.5.
Example 1
As shown in figure 1, the method for promoting reduction and recovery of nickel in the chemical nickel plating waste liquid comprises the following specific steps: taking 1L of waste liquid, adjusting the pH value to 8 by using 40% sodium hydroxide, heating a water bath kettle to 60 ℃, opening a stirrer, rotating at the speed of 250r/min, taking 0.3g of ferroalloy and the particle size of 5mm, preparing 15% slurry by using water, adding 20mg/L of polyacrylic acid, slowly adding the mixture into the heated waste liquid after uniformly stirring, stirring at a constant temperature for 1h, reducing the stirring speed to 50r/min after the reaction is finished, adding 10mL (0.1%) of anionic polyacrylamide, standing for 5 min, and filtering to obtain the nickel metal product.
Example 2
Taking 1L of waste liquid, adjusting the pH value to 10 by using 40% sodium hydroxide, heating a water bath kettle to 90 ℃, opening a stirrer, rotating at the speed of 200r/min, taking 0.1g of aluminum alloy and 5mm in particle size, preparing 15% slurry by using water, adding 20mg/L of polyacrylic acid, slowly adding the mixture into the heated waste liquid after uniformly stirring, stirring at a constant temperature for 1h, reducing the stirring speed to 50r/min after the reaction is finished, adding 10mL (0.1%) of anionic polyacrylamide, standing for 5 minutes, and filtering to obtain the nickel metal product.
Example 3
Taking 1L of waste liquid, adjusting the pH value to 10 by using 40% sodium hydroxide, heating a water bath kettle to 80 ℃, opening a stirrer, rotating at the speed of 250r/min, taking 0.4g of nickel alloy and 5mm in particle size, preparing 15% slurry by using water, adding 20mg/L of polyacrylic acid, slowly adding the mixture into the heated waste liquid after uniformly stirring, stirring at constant temperature for 1h, reducing the stirring speed to 50r/min after the reaction is finished, adding 10mL (0.1%) of anionic polyacrylamide, standing for 5 min, and filtering to obtain the nickel metal product.
The waste liquid and nickel metal products treated in the three examples were analyzed, and the specific analysis results are shown in table 1.
Table 1: the nickel content in the waste liquid and nickel metal product treated by the embodiment of the invention is shown in the table
| Example 1 | Example 2 | Example 3 | |
| Stock solution nickel ion concentration (mg/L) | 4000 | 3900 | 4200 |
| Concentration of nickel ion (mg/L) in the treated liquid | 30 | 19.2 | 40 |
| Nickel metal product purity (%) | 92.5 | 93.2 | 90.2 |
| Nickel recovery (%) | 99.25 | 99.51 | 99.05 |
The above-mentioned embodiments are only preferred embodiments of the present invention, and all equivalent changes and modifications made within the scope of the claims of the present invention should be covered by the claims of the present invention.
Claims (5)
1. A method for promoting reduction and recovery of nickel in chemical nickel plating waste liquid is characterized by comprising the following steps:
firstly, adjusting the pH value of chemical nickel plating waste liquid to 7-11 by using sodium hydroxide to obtain pretreated waste liquid;
heating to 40-100 ℃;
preparing 10-20% slurry from the accelerator, adding 10-100 mg/L of dispersant, uniformly stirring, adding 50-500 mg/L of pretreated waste liquid, controlling the temperature at 40-100 ℃, and stirring for reacting for 0.5-2 hours; and immediately adding a flocculating agent after the reaction is finished, wherein the addition amount of the flocculating agent is 10-100 mg/L, filtering while the reaction is hot to obtain a nickel metal product and a treated waste liquid, and recovering the nickel to obtain the waste liquid containing phosphite radicals and organic matters and then feeding the waste liquid into a wastewater treatment system after recovering phosphorus resources.
2. The method for promoting reduction recovery of nickel in the chemical nickel plating waste liquid according to claim 1, characterized by selecting one or the combination of the following components from the promoters: beryllium alloys, aluminum alloys, iron alloys, titanium alloys, cobalt alloys, nickel alloys.
3. The method for promoting reduction and recovery of nickel in the chemical nickel plating waste liquid according to claim 1, characterized in that the crystal form of the promoter is one or any two of a hypo-eutectic form, a cocrystal form and a hyper-eutectic form; the grain size range of the accelerator is 1-20 mm.
4. The method for promoting the reduction recovery of nickel in the chemical nickel plating waste liquid according to claim 1, characterized in that the dispersant is polyacrylic acid with low molecular weight, and the molecular weight is not more than 5000.
5. The method for promoting reduction and recovery of nickel in an electroless nickel plating waste liquid according to claim 1, wherein the flocculant in step four is a high-temperature resistant PAM-series anionic flocculant and has a molecular weight of 1000 ten thousand or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110525187.7A CN113264607A (en) | 2021-05-14 | 2021-05-14 | Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110525187.7A CN113264607A (en) | 2021-05-14 | 2021-05-14 | Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113264607A true CN113264607A (en) | 2021-08-17 |
Family
ID=77230766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110525187.7A Pending CN113264607A (en) | 2021-05-14 | 2021-05-14 | Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113264607A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115057516A (en) * | 2022-04-28 | 2022-09-16 | 深圳市点石源水处理技术有限公司 | Chemical plating waste liquid treating agent and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0657438A (en) * | 1992-08-06 | 1994-03-01 | Agency Of Ind Science & Technol | Treatment of aged plating liquid and production of iron power coated with different metal |
| TW200811060A (en) * | 2006-08-21 | 2008-03-01 | Mitac Prec Technology Corp | Method of recycle and treatment of used chemical nickel plating electrolyte |
| CN104105818A (en) * | 2012-02-08 | 2014-10-15 | 石原化学株式会社 | Pretreatment solution for electroless nickel plating or electroless nickel alloy plating, and plating method |
| CN106148709A (en) * | 2016-08-12 | 2016-11-23 | 星特殊化学品（新加坡）有限公司 | Nickel recovery and treatment method in chemical nickel plating waste solution |
| CN108356281A (en) * | 2018-03-16 | 2018-08-03 | 南京林业大学 | A kind of preparation method of Nickel Powder |
| CN110395817A (en) * | 2019-07-25 | 2019-11-01 | 苏州湛清环保科技有限公司 | The recycling processing method of chemical nickel plating waste solution |
-
2021
- 2021-05-14 CN CN202110525187.7A patent/CN113264607A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0657438A (en) * | 1992-08-06 | 1994-03-01 | Agency Of Ind Science & Technol | Treatment of aged plating liquid and production of iron power coated with different metal |
| TW200811060A (en) * | 2006-08-21 | 2008-03-01 | Mitac Prec Technology Corp | Method of recycle and treatment of used chemical nickel plating electrolyte |
| CN104105818A (en) * | 2012-02-08 | 2014-10-15 | 石原化学株式会社 | Pretreatment solution for electroless nickel plating or electroless nickel alloy plating, and plating method |
| CN106148709A (en) * | 2016-08-12 | 2016-11-23 | 星特殊化学品（新加坡）有限公司 | Nickel recovery and treatment method in chemical nickel plating waste solution |
| CN108356281A (en) * | 2018-03-16 | 2018-08-03 | 南京林业大学 | A kind of preparation method of Nickel Powder |
| CN110395817A (en) * | 2019-07-25 | 2019-11-01 | 苏州湛清环保科技有限公司 | The recycling processing method of chemical nickel plating waste solution |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115057516A (en) * | 2022-04-28 | 2022-09-16 | 深圳市点石源水处理技术有限公司 | Chemical plating waste liquid treating agent and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110819821B (en) | Method for intensively purifying zinc sulfate solution | |
| CN105149610B (en) | A kind of chemical nickeling ageing liquid treatment process | |
| CN110395817A (en) | The recycling processing method of chemical nickel plating waste solution | |
| CN109437446A (en) | A kind of zinc nickel alloy electroplating waste water treatment process | |
| CN113264607A (en) | Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid | |
| CN103736994A (en) | Electroless nickel plating solution treatment method | |
| CN104475039A (en) | Biological adsorbent capable of removing fluorine and heavy metals in wastewater, preparation method and application method thereof | |
| CN111892217A (en) | Method for converting and recycling nickel-containing compound in chemical nickel plating waste liquid | |
| CN103805774A (en) | Method for synergistically reducing pyrolusite by using organic matters with low carbon numbers | |
| CN107235570B (en) | Method and system for standard reaching and recycling of cold rolling acidic wastewater | |
| CN107828965A (en) | A kind of method of cobalt and manganese in separating and recovering cobalt manganese waste material | |
| CN108423865B (en) | Treatment method of chemical nickel plating waste liquid | |
| CN110563218A (en) | method for recovering phosphorus resource from chemical nickel waste liquid | |
| CN102912324B (en) | High-stability palladium catalyst concentrated solution and preparation method thereof | |
| CN108178370B (en) | Method for breaking nickel-containing complex by persulfate and catalytic ceramsite participating in advanced oxidation | |
| CN1932083A (en) | Silver electrolyzing process | |
| CN106085508A (en) | A kind of catalytic coal gasifaction method | |
| CN111517421A (en) | Method for improving iron-carbon micro-electrolysis reaction efficiency by using iron-containing waste acid liquor wastewater | |
| CN115722251A (en) | Preparation method and application of hetero-atom-doped algae-based biochar loaded nano zero-valent metal catalyst | |
| CN106148709B (en) | Nickel recovery and treatment method in chemical nickel plating waste solution | |
| CN107755712B (en) | Method for preparing metal antimony powder | |
| CN114604885B (en) | Preparation method for preparing calcium chloride by using waste hydrochloric acid | |
| CN106365136B (en) | The method of nickel plating Ageing solution preparation recycling metal nickel powder, phosphoric acid and gypsum | |
| CN113772869B (en) | Quality-based treatment method for gold smelting wastewater | |
| CN103641209B (en) | A kind of copper-containing wastewater combined electrolysis groove treatment process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210817 |
|
| RJ01 | Rejection of invention patent application after publication |