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 PDFInfo
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- 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
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- chemical nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working 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
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/265—General methods for obtaining phosphates
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment 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
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)
- 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. 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.
- 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.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610661919.4A CN106148709B (en) | 2016-08-12 | 2016-08-12 | Nickel recovery and treatment method in chemical nickel plating waste solution |
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|---|---|---|---|
| CN201610661919.4A CN106148709B (en) | 2016-08-12 | 2016-08-12 | Nickel recovery and treatment method in chemical nickel plating waste solution |
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| CN106148709B true CN106148709B (en) | 2018-01-05 |
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| CN113264607A (en) * | 2021-05-14 | 2021-08-17 | 深圳市小荷环保技术有限公司 | Method for promoting reduction recovery of high-concentration nickel in chemical nickel plating waste liquid |
| CN114032558B (en) * | 2021-12-14 | 2022-11-15 | 北京科技大学 | Method for preparing NiP micron particles from chemical nickel plating waste liquid through electrolysis |
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