CN106148709B - Nickel recovery and treatment method in chemical nickel plating waste solution - Google Patents

Nickel recovery and treatment method in chemical nickel plating waste solution Download PDF

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Publication number
CN106148709B
CN106148709B CN201610661919.4A CN201610661919A CN106148709B CN 106148709 B CN106148709 B CN 106148709B CN 201610661919 A CN201610661919 A CN 201610661919A CN 106148709 B CN106148709 B CN 106148709B
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nickel
concentration
filtrate
chemical nickel
ssc
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CN106148709A (en
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江建平
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Star Special Chemicals (singapore) Co Ltd
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Star Special Chemicals (singapore) Co Ltd
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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
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/265General methods for obtaining phosphates
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • C22B23/0453Treatment or purification of solutions, e.g. obtained by leaching
    • C22B23/0461Treatment or purification of solutions, e.g. obtained by leaching by chemical methods

Abstract

The present invention relates to surface treatment and sewage treatment area, the nickel recovery and treatment method in espespecially a kind of chemical nickel plating waste solution, comprises the following steps:Step 1:The pH to 6 10 for the NaOH adjustment chemical nickel waste liquids for being 2g/L with concentration;Step 2:SSC EN STARTER initiators are added and are equipped with chemical nickel spent liquor solution groove, 70 95 DEG C are heated up to solution tank;Step 3:The reducing agent that concentration is 1g/L and the NaOH that concentration is 2g/L were added every 5 minutes, every time stirring at least 0.4 1 hours;Step 4:Filtrate A is obtained after filtering, the NaOH for being 2g/L with concentration adjusts filtrate ApH to 11 13;Step 5:The SSC EN WT ST additives that concentration is 0.1-1g/L are added into filtrate A, are stirred 0.4 1 hours;Step 6:Stop stirring, liquor B is obtained after filtering, with dilute sulfuric acid and liquor B is to pH 68.

Description

Nickel recovery and treatment method in chemical nickel plating waste solution
Technical field
The present invention relates to surface treatment and sewage treatment area, the nickel recycling side in espespecially a kind of chemical nickel plating waste solution Method.
Background technology
With the rapid development of science and technology, chemical nickel plating application field constantly expands.Because nickel chemical plating technology is simple, Practicality is stronger, has many advantageous characteristics.But the heavy metal ion in chemical nickel plating waste solution is to the seriously polluted of environment, Cause the extensive concern of people.It is the various complexing agents of addition, steady especially for the stability for improving chemical deposit quality and plating solution Determine that the organic matters such as agent and brightener are larger to environmental hazard, the also removal to the nickel in waste liquid, phosphorus plasma brings difficulty.
The chemical nickel plating waste solution processing method reported at present can generally be divided into chemical method and Physical, mainly have catalysis also Former method, chemical precipitation method, ion-exchange, electrolysis, electroosmose process, bioanalysis, absorption method and several method comprehensive utilization Deng.
Chemical method has the advantages that investment is small, management is simple, easily promotes the use of.Chemical method can be summarized as two approach: Chemical precipitation oxidizing process, is decomposed and contact break first, then by hypophosphites and oxidation of phosphite is phosphate, then utilizes CaO Remove nickel, phosphate, or addition DTC (dialkyl dithiocarbamate) class heavy metal capturing agent method Combined Treatment. There is good effect on the law theory, but oxidizing reaction rate is very slow in practical application, and oxidation is not thorough, and oxidizer Greatly, it is costly.After waste liquid is heated, the catalyst such as a certain amount of PdCl2 are added, some is also put into nickel powder iron powder etc. As derivant, promote waste liquid voluntarily to decompose, then recycle alkaline matter to make part phosphorus Precipitation.The method uses noble metal Salt makees catalyst, and cost of material is very high, it is difficult to uses.
In patent CN101434441A, waste liquid is promoted to occur certainly using heat caused by sodium hydroxide dissolving neutralization reaction Decompose, generate Ni-P alloy solid particles.In patent CN103736994A, entered by adding substantial amounts of iron powder and sodium hypophosphite The processing of row nickel coated.Again nickel powder is extracted by the smelting of metallurgy industry.Process is complicated.
The content of the invention
To solve the above problems, present invention offer a kind of simple and fast processing method, the cost of chemical nickel plating waste solution is cheap. To solve to produce new discarded object present in the method for existing Treatment of Electroless Nickel Plating Wastewater, it is impossible to accomplish the problem of environment friendly and pollution-free The shortcomings of.Nickel recovery of the processing method of the present invention suitable for various chemical nickel plating waste solutions.
To achieve the above object, the present invention, which adopts the following technical scheme that, is:A kind of nickel recovery in chemical nickel plating waste solution Processing method, comprise the following steps:
Step 1:The pH to 6-10 for the NaOH adjustment chemical nickel waste liquids for being 2g/L with concentration, in chemical nickel waste liquid now Nickel content is 4-7g/L, sodium hypophosphite 10-40g/L;
Step 2:SSC EN STARTER initiators are added in chemical nickel spent liquor solution, chemical nickel spent liquor solution is added Temperature now produces substantial amounts of fine nickel-phosphorus alloy particle to 70-95 DEG C;
Step 3:The reducing agent that concentration is 1g/L and the NaOH that concentration is 2g/L were added every 5 minutes, is stirred every time at least 0.4-1 hours, stir 0-3 times;
Step 4:Filtrate A is obtained after filtering and reclaims nickel-phosphorus alloy particle, contained nickel is about 5- in filtrate A 30ppm, the NaOH for being 2g/L with concentration adjust filtrate A pH to 11-13;
Step 5:The SSC EN WT ST additives that concentration is 0.1-1g/L are added into filtrate A, stirring 0.4-1 is small When;
Step 6:Stop stirring, liquor B is obtained after filtering, with dilute sulfuric acid and liquor B is to pH 6-8.
Wherein, described SSC EN STARTER initiators include sodium hypophosphite, sodium sulfite, the group of metallic compound Polymerisable compounds.When SSC EN STARTER initiators add temperature higher than the chemical nickel plating waste solution of normal temperature and meta-alkalescence, moment Caused acid-base neutralization heat and strong reducing property to produce substantial amounts of fine nickel-phosphorus alloy particle at once, so as to trigger chemical nickel plating The automatic classifying of waste liquid.
Wherein, described metallic compound is aluminium or tin or zinc or its combination of compounds.
Wherein, described SSC EN STARTER initiator concentrations are 0.03-0.5ml/L
Wherein, described SSC EN WT ST additives include the reproducibility chemical combination of sodium hypophosphite and/or sodium sulfite Thing.
Wherein, it is less than 0.3ppm by nickel content in step 6 Filtrate B, is directly discharged after adjusting pH.
Wherein, very low by ortho phosphorous acid sodium content in step 6 Filtrate B, liquor B can be as fertilizer Raw material is used.
The beneficial effects of the present invention are:After present invention process is handled, the nickel of aging waste liquid can be down to 0.3ppm with Under, realize and recycled to more than the 99.99% of nickel, eliminate pollution of the nickel to environment.Contain in remaining aging waste liquid Hypophosphites and phosphite phosphate is formd by advanced oxidation process, conveniently can be subject to profit as the raw material of fertilizer With.The present invention realizes the comprehensive utilization of resource, prevents environmental pollution.
Embodiment
The present invention is on reference to specific embodiment, the present invention will be further described, can be with according to following embodiments More fully understand the present invention.However, as it will be easily appreciated by one skilled in the art that the content described by embodiment is merely to illustrate this Invention, without should be also without limitation on the present invention described in detail in claims.
A kind of nickel recovery and treatment method in chemical nickel plating waste solution, comprises the following steps:
Step 1:The pH to 6-10 for the NaOH adjustment chemical nickel waste liquids for being 2g/L with concentration, in chemical nickel waste liquid now Nickel content is 4-7g/L, sodium hypophosphite 10-40g/L;
Step 2:SSC EN STARTER initiators are added in chemical nickel spent liquor solution, chemical nickel spent liquor solution is added Temperature now produces substantial amounts of fine nickel-phosphorus alloy particle to 70-95 DEG C;
Step 3:According to the species of chemical nickel plating waste solution, it is every the reducing agent and concentration that 5 minutes addition concentration is 1g/L 2g/L NaOH, every time stirring at least 0.4-1 hours, stir 0-3 times;
Step 4:Filtrate A is obtained after filtering and reclaims nickel-phosphorus alloy particle, contained nickel is about 5- in filtrate A 30ppm, the NaOH for being 2g/L with concentration adjust filtrate A pH to 11-13;
Step 5:The SSC EN WT ST additives that concentration is 0.1-1g/L are added into filtrate A, stirring 0.4-1 is small When;
Step 6:Stop stirring, liquor B is obtained after filtering, with dilute sulfuric acid and liquor B is to pH 6-8.
Wherein, described SSC EN STARTER initiators include sodium hypophosphite, sodium sulfite, the group of metallic compound Polymerisable compounds.When SSC EN STARTER initiators add temperature higher than the chemical nickel plating waste solution of normal temperature and meta-alkalescence, moment Caused acid-base neutralization heat and strong reducing property to produce substantial amounts of fine nickel-phosphorus alloy particle at once, so as to trigger chemical nickel plating The automatic classifying of waste liquid.
Wherein, described metallic compound is aluminium or tin or zinc or its combination of compounds.
Wherein, described SSC EN STARTER initiator concentrations are 0.03-0.5ml/L.
Wherein, in step 3, reducing agent and sodium hydroxide are to be added according to the species of chemical nickel plating waste solution in reactive tank.
Wherein, described SSC EN WT ST additives include the reproducibility chemical combination of sodium hypophosphite and/or sodium sulfite Thing.
Wherein, it is less than 0.3ppm by nickel content in step 6 Filtrate B, is directly discharged after adjusting pH.
Wherein, very low by ortho phosphorous acid sodium content in step 6 Filtrate B, liquor B can be as fertilizer Raw material is used.
Embodiment one:The processing of phosphorus chemistry nickel-plating waste liquid in acidity
Step 1:Chemical nickel waste liquid is injected in solution tank, the NaOH for being 2g/L with concentration adjusts the pH of chemical nickel waste liquid To 8-9, heating chemical nickel waste liquid is to 80-85 DEG C;
Step 2:The SSC EN STARTER initiators that concentration is 0.05ml/L are added in chemical nickel waste liquid;
Step 3:After stirring 20 minutes;
Step 4:Stop stirring, waste liquid is filtered and obtains filtrate A;
Step 5:The pH to 11-13 for the NaOH adjustment filtrates A for being 2g/L with concentration, adds the SSC EN that concentration is 1g/L WT ST additives and stir at least 0.5 hour after;
Step 6:Liquor B is obtained after filtering, with dilute sulfuric acid and liquor B is to pH (6-8), now, nickel in the filtrate of extraction Ion concentration has descended to below 0.3ppm.
Embodiment two:The processing of acid high phosphorus chemical plating nickel waste liquid
Step 1:Chemical nickel waste liquid is injected in solution tank, the NaOH for being 2g/L with concentration adjusts the pH of chemical nickel waste liquid To 8-9,80-85 DEG C is heated to;
Step 2:The SSC EN STARTER initiators that concentration is 0.2ml/L are added into chemical nickel waste liquid;
Step 3:Every 5 minutes points of 2 addition concentration be 1g/L reducing agents and concentration is 2g/L NaOH, stirs 20 every time Minute;
Step 4:Stop stirring and filtering obtaining filtrate A;
Step 5:The pH to 11-13 for the NaOH adjustment filtrates A for being 2g/L with concentration, adds the SSC EN that concentration is 1g/L WT ST additives simultaneously stir at least 0.5 hour;
Step 6:Liquor B is obtained after filter, with dilute sulfuric acid and liquor B is to pH (6-8), now, in the filtrate of extraction nickel from Sub- content has descended to below 0.3ppm.
Embodiment three:The processing of the low-phosphorous chemical nickel plating waste solution of alkalescence
Step 1:Chemical nickel waste liquid is injected in solution tank, the NaOH for being 2g/L with concentration adjusts the pH of chemical nickel waste liquid To 9-10,85-90 DEG C is heated to;
Step 2:It is that 0.5ml/LSSC EN STARTER initiators add chemical nickel waste liquid by concentration;
Step 3:The NaOH for being 2g/L every reducing agent and concentration that 5 minutes points of 3 addition concentration are 1g/L, stirring 20 Minute;
Step 4:Stop stirring, be filtrated to get filtrate A;
Step 5:The pH to 11-13 for the NaOH adjustment filtrates A for being 2g/L with concentration, adds the SSC EN that concentration is 1g/L WT ST additives simultaneously stir at least 0.5 hour;
Step 6:Filtering obtains liquor B, with dilute sulfuric acid and liquor B is to pH (6-8), now, in the filtrate of extraction nickel from Sub- content has descended to below 0.3ppm.
Embodiment of above is only that the preferred embodiment of the present invention is described, and not the scope of the present invention is entered Row limits, on the premise of design spirit of the present invention is not departed from, technical side of this area ordinary skill technical staff to the present invention The various modifications and improvement that case is made, it all should fall into the protection domain of claims of the present invention determination.

Claims (3)

  1. A kind of 1. nickel recovery and treatment method in chemical nickel plating waste solution, it is characterised in that:Comprise the following steps:
    Step 1:The NaOH for being 2g/L with concentration adjusts the pH to 6-10 of chemical nickel waste liquid, and nickel contains in chemical nickel waste liquid now Measure as 4-7g/L, sodium hypophosphite 10-40g/L;
    Step 2:SSC EN STARTER initiators are added in chemical nickel spent liquor solution, chemical nickel spent liquor solution is heated up to 70-95 DEG C, substantial amounts of fine nickel-phosphorus alloy particle is now produced, described SSC EN STARTER initiators include ortho phosphorous acid Sodium, sodium sulfite, the combination of compounds of metallic compound;
    Step 3:The reducing agent that concentration is 1g/L and the NaOH that concentration is 2g/L were added every 5 minutes, it is small to stir 0.4-1 every time When, stir 0-3 times;
    Step 4:Filtrate A is obtained after filtering and reclaims nickel-phosphorus alloy particle, contained nickel is 5-30ppm in filtrate A, uses concentration Filtrate A pH to 11-13 is adjusted for 2g/L NaOH;
    Step 5:The SSC EN WT ST additives that concentration is 0.1-1g/L are added into filtrate A, stir 0.4-1 hours, institute The SSC EN WT ST additives stated include sodium hypophosphite and/or the reproducibility compound of sodium sulfite;
    Step 6:Stop stirring, liquor B is obtained after filtering, with dilute sulfuric acid and liquor B is to pH 6-8, nickel in Filtrate B Content is less than 0.3ppm, is directly discharged after adjusting pH, ortho phosphorous acid sodium content is very low in Filtrate B, and liquor B can be made It is used for the raw material of fertilizer.
  2. 2. the nickel recovery and treatment method in a kind of chemical nickel plating waste solution according to claim 1, it is characterised in that:Described Metallic compound is aluminium, tin, any two simple substance mixtures of zinc.
  3. A kind of 3. processing method of chemical nickel plating waste solution according to claim 1, it is characterised in that:Described SSC EN STARTER initiator concentrations are 0.03-0.5ml/L.
CN201610661919.4A 2016-08-12 2016-08-12 Nickel recovery and treatment method in chemical nickel plating waste solution Active CN106148709B (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59185770A (en) * 1983-04-05 1984-10-22 Oosakafu Method for recovering nickel from waste chemical nickel plating bath
CN1094457A (en) * 1993-04-30 1994-11-02 国营庆安宇航设备公司 A kind of renovation process of acid chemical plating nickel solution
CN1237543A (en) * 1999-06-04 1999-12-08 河北省冶金设计研究院 Method for treating waste water produced by electroplating process
CN101434441A (en) * 2008-12-03 2009-05-20 山东建筑大学 Processing method of chemical nickel phosphor plating
CN101805831A (en) * 2010-03-24 2010-08-18 埃梯星(厦门)电子科技有限公司 Method for directly extracting nickel in alkaline chemical nickel-plating waste liquid
CN101892389A (en) * 2010-07-14 2010-11-24 王昊杨 Method for preparing nano metallic nickel in spent electroless nickel plating solution
CN102071410A (en) * 2011-01-21 2011-05-25 深圳市瑞世兴科技有限公司 Method for recovering nickel resource from waste liquid of chemical nickel plating
CN103991916A (en) * 2014-06-12 2014-08-20 杭州一清环保工程有限公司 Comprehensive electroplating wastewater treating agent
CN105060561A (en) * 2015-08-12 2015-11-18 太仓中化环保化工有限公司 Method for removing heavy metal ions in wastewater

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59185770A (en) * 1983-04-05 1984-10-22 Oosakafu Method for recovering nickel from waste chemical nickel plating bath
CN1094457A (en) * 1993-04-30 1994-11-02 国营庆安宇航设备公司 A kind of renovation process of acid chemical plating nickel solution
CN1237543A (en) * 1999-06-04 1999-12-08 河北省冶金设计研究院 Method for treating waste water produced by electroplating process
CN101434441A (en) * 2008-12-03 2009-05-20 山东建筑大学 Processing method of chemical nickel phosphor plating
CN101805831A (en) * 2010-03-24 2010-08-18 埃梯星(厦门)电子科技有限公司 Method for directly extracting nickel in alkaline chemical nickel-plating waste liquid
CN101892389A (en) * 2010-07-14 2010-11-24 王昊杨 Method for preparing nano metallic nickel in spent electroless nickel plating solution
CN102071410A (en) * 2011-01-21 2011-05-25 深圳市瑞世兴科技有限公司 Method for recovering nickel resource from waste liquid of chemical nickel plating
CN103991916A (en) * 2014-06-12 2014-08-20 杭州一清环保工程有限公司 Comprehensive electroplating wastewater treating agent
CN105060561A (en) * 2015-08-12 2015-11-18 太仓中化环保化工有限公司 Method for removing heavy metal ions in wastewater

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Title
"应用于可穿戴电子器件柔性线路板的化镍金技术";江建平;《中国表面工程协会电镀分会成立三十周年之电子与微电子表面处理研讨会论文集》;20140917;正文60页 *

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