CN106148709A - 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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- CN106148709A CN106148709A CN201610661919.4A CN201610661919A CN106148709A CN 106148709 A CN106148709 A CN 106148709A CN 201610661919 A CN201610661919 A CN 201610661919A CN 106148709 A CN106148709 A CN 106148709A
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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
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- Engineering & Computer Science (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- General Life Sciences & Earth Sciences (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to surface process and sewage treatment area, the nickel recovery and treatment method in a kind of chemical nickel plating waste solution, comprise the following steps: step one: adjust the pH to 6 10 of chemical nickel waste liquid with the NaOH that concentration is 2g/L；Step 2: SSC EN STARTER initiator is equipped with in chemical nickel spent liquor solution groove, solution tank is heated up to 70 95 DEG C；Step 3: added concentration every 5 minutes and be the reducing agent of 1g/L and concentration is the NaOH of 2g/L, stirring at least 0.4 1 hour every time；Step 4: obtain filtrate A after filtration, adjust filtrate ApH to 11 13 with the NaOH that concentration is 2g/L；Step 5: add the SSC EN WT ST additive that concentration is 0.1 1g/L in filtrate A, stir 0.4 1 hours；Step 6: stop stirring, obtains liquor B after filtration, with in dilute sulfuric acid and liquor B is to pH 68.
Description
Technical field
The present invention relates to surface process and sewage treatment area, the nickel recycling side in a kind of chemical nickel plating waste solution
Method.
Background technology
Along with developing rapidly of science and technology, chemical nickel plating application constantly expands.Owing to nickel chemical plating technology is simple,
Practicality is relatively strong, has many advantageous characteristic.But seriously polluted, to environment of the heavy metal ion in chemical nickel plating waste solution
Cause the extensive concern of people.Especially for improving chemical deposit quality and the stability of plating solution, the various chelating agent of interpolation, steady
Determine the Organic substance such as agent and brightener relatively big to environmental hazard, bring difficulty also to the nickel in waste liquid, the isoionic removal of phosphorus.
The chemical nickel plating waste solution processing method of report can be divided into chemical method and Physical generally at present, mainly has 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 such as investment is little, management is simple, easily promotes the use of.Chemical method can be summarized as two approach:
Chemical precipitation oxidizing process, first decomposes and contact break, then is phosphate by hypophosphites and oxidation of phosphite, then utilize CaO
Remove nickel, phosphate, or add DTC (dialkyl dithiocarbamate) class heavy metal capturing agent method Combined Treatment.
Having good effect on this law theory, but in actual application, oxidizing reaction rate is very slow, oxidation is not thorough, and oxidizer
Greatly, costly.After being heated by waste liquid, adding the catalyst such as a certain amount of PdCl2, have also puts into nikel powder iron powder etc.
As derivant, promoting waste liquid to decompose voluntarily, then recycling alkaline matter makes part phosphorus Precipitation.This method uses noble metal
Catalyst made by salt, and cost of material is the highest, it is difficult to use.
In patent CN101434441A, the heat utilizing sodium hydroxide to dissolve neutralization reaction generation promotes waste liquid to occur
Selfdecomposition, generates Ni-P alloy solid granule.In patent CN103736994A, by adding substantial amounts of iron powder and sodium hypophosphite
Carry out nickel coated process.Nikel powder is extracted in smelting through metallurgy industry again.Process is complicated.
Summary of the invention
For solving the problems referred to above, the present invention provides the simple and fast processing method of a kind of chemical nickel plating waste solution, with low cost.
New garbage is produced, it is impossible to accomplish environment friendly and pollution-free problem present in method with the existing Treatment of Electroless Nickel Plating Wastewater of solution
Etc. shortcoming.The processing method of present invention nickel be applicable to various chemical nickel plating waste solutions reclaims.
For achieving the above object, the present invention adopts the following technical scheme that and is: the nickel in a kind of chemical nickel plating waste solution reclaims
Processing method, comprises the following steps:
Step one: adjust the pH to 6-10 of chemical nickel waste liquid with the NaOH that concentration is 2g/L, in chemical nickel waste liquid now
Nickel content is 4-7g/L, and sodium hypophosphite is 10-40g/L；
Step 2: SSC EN STARTER initiator is added in chemical nickel spent liquor solution, chemical nickel spent liquor solution is added
Temperature, to 70-95 DEG C, now produces substantial amounts of fine nickel-phosphorus alloy granule；
Step 3: adding concentration every 5 minutes and be the reducing agent of 1g/L and concentration is the NaOH of 2g/L, stirring is at least every time
0.4-1 hour, stir 0-3 time；
Step 4: obtaining filtrate A after filtration and reclaim nickel-phosphorus alloy granule, nickel contained in filtrate A is about 5-
30ppm, adjusts the pH to 11-13 of filtrate A with the NaOH that concentration is 2g/L；
Step 5: add the SSC EN WT ST additive that concentration is 0.1-1g/L in filtrate A, 0.4-1 is little in stirring
Time；
Step 6: stop stirring, obtains liquor B after filtration, with in dilute sulfuric acid and liquor B is to pH 6-8.
Wherein, described SSC EN STARTER initiator comprises sodium hypophosphite, sodium sulfite, metallic compound
Combination of compounds.When SSC EN STARTER initiator adds the chemical nickel plating waste solution that temperature is higher than room temperature and meta-alkalescence, wink
Between the acid-base neutralization heat that produces and strong reducing property make at once to produce substantial amounts of fine nickel-phosphorus alloy granule, thus cause chemical plating
The automatic classifying of nickel waste liquid.
Wherein, described metallic compound is aluminum or stannum or zinc or a combination thereof compound.
Wherein, described SSC EN STARTER initiator concentration is 0.03 0.5ml/L
Wherein, described SSC EN WT ST additive comprises the reproducibility chemical combination of sodium hypophosphite and/or sodium sulfite
Thing.
Wherein, in step 6 Filtrate B, nickel content is less than 0.3ppm, directly discharges after regulation pH.
Wherein, in step 6 Filtrate B, ortho phosphorous acid sodium content is the lowest, and liquor B can be as fertilizer
Raw material is used.
The beneficial effects of the present invention is: through present invention process process after, the nickel of aging waste liquid can be down to 0.3ppm with
Under, it is achieved that more than 99.99% recycling to nickel, eliminate the nickel pollution to environment.Remaining aging waste liquid contains
Hypophosphites and phosphite define phosphate by advanced oxidation operation, can facilitate the raw material as fertilizer add in order to
With.Present invention achieves the comprehensive utilization of resource, prevent environmental pollution.
Detailed description of the invention
The present invention is about below in conjunction with specific embodiment, the present invention will be further described, according to following embodiment, permissible
It is more fully understood that the present invention.But, as it will be easily appreciated by one skilled in the art that the content described by embodiment is merely to illustrate this
Invention, and should be also without limitation on the present invention described in detail in claims.
Nickel recovery and treatment method in a kind of chemical nickel plating waste solution, comprises the following steps:
Step one: adjust the pH to 6-10 of chemical nickel waste liquid with the NaOH that concentration is 2g/L, in chemical nickel waste liquid now
Nickel content is 4-7g/L, and sodium hypophosphite is 10-40g/L；
Step 2: SSC EN STARTER initiator is added in chemical nickel spent liquor solution, chemical nickel spent liquor solution is added
Temperature, to 70-95 DEG C, now produces substantial amounts of fine nickel-phosphorus alloy granule；
Step 3: according to the kind of chemical nickel plating waste solution, added reducing agent that concentration is 1g/L every 5 minutes and concentration is
The NaOH of 2g/L, stirs at least 0.4-1 hour every time, stirs 0-3 time；
Step 4: obtaining filtrate A after filtration and reclaim nickel-phosphorus alloy granule, nickel contained in filtrate A is about 5-
30ppm, adjusts the pH to 11-13 of filtrate A with the NaOH that concentration is 2g/L；
Step 5: add the SSC EN WT ST additive that concentration is 0.1-1g/L in filtrate A, 0.4-1 is little in stirring
Time；
Step 6: stop stirring, obtains liquor B after filtration, with in dilute sulfuric acid and liquor B is to pH 6-8.
Wherein, described SSC EN STARTER initiator comprises the group of sodium hypophosphite, sodium sulfite, metallic compound
Polymerisable compounds.When SSC EN STARTER initiator adds the chemical nickel plating waste solution that temperature is higher than room temperature and meta-alkalescence, moment
The acid-base neutralization heat produced and strong reducing property make at once to produce substantial amounts of fine nickel-phosphorus alloy granule, thus cause chemical nickel plating
The automatic classifying of waste liquid.
Wherein, described metallic compound is aluminum or stannum or zinc or a combination thereof compound.
Wherein, described SSC EN STARTER initiator concentration is 0.03 0.5ml/L.
Wherein, in step 3, reducing agent and sodium hydroxide are to add in reactive tank according to the kind of chemical nickel plating waste solution.
Wherein, described SSC EN WT ST additive comprises the reproducibility chemical combination of sodium hypophosphite and/or sodium sulfite
Thing.
Wherein, in step 6 Filtrate B, nickel content is less than 0.3ppm, directly discharges after regulation pH.
Wherein, in step 6 Filtrate B, ortho phosphorous acid sodium content is the lowest, and liquor B can be as fertilizer
Raw material is used.
Embodiment one: the process of phosphorus chemistry nickel-plating waste liquid in acidity
Step one: inject chemical nickel waste liquid in solution tank, adjust the pH of chemical nickel waste liquid with the NaOH that concentration is 2g/L
To 8-9, heating chemical nickel waste liquid is to 80-85 DEG C；
Step 2: the SSC EN STARTER initiator that concentration is 0.05ml/L is added in chemical nickel waste liquid；
Step 3: after stirring 20 minutes；
Step 4: stop stirring, filters waste liquid and obtains filtrate A；
Step 5: adjust the pH to 11-13 of filtrate A with the NaOH that concentration is 2g/L, adds the SSC EN that concentration is 1g/L
WT ST additive also stirs after at least 0.5 hour；
Step 6: obtain liquor B after filtration, with in 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 process of acid high phosphorus chemical plating nickel waste liquid
Step one: inject chemical nickel waste liquid in solution tank, adjust the pH of chemical nickel waste liquid with the NaOH that concentration is 2g/L
To 8-9, it is heated to 80-85 DEG C；
Step 2: the SSC EN STARTER initiator that concentration is 0.2ml/L is added chemical nickel waste liquid；
Step 3: be 1g/L reducing agent and concentration is 2g/L NaOH every adding concentration for 5 minutes points 2 times, stir 20 every time
Minute；
Step 4: stop stirring and filter acquisition filtrate A；
Step 5: adjust the pH to 11-13 of filtrate A with the NaOH that concentration is 2g/L, adds the SSC EN that concentration is 1g/L
WT ST additive also stirs at least 0.5 hour；
Step 6: after filter obtain liquor B, with in dilute sulfuric acid and liquor B to pH (6-8), now, in the filtrate of extraction nickel from
Sub-content has descended to below 0.3ppm.
Embodiment three: the process of alkaline low-phosphorous chemical nickel plating waste solution
Step one: inject chemical nickel waste liquid in solution tank, adjust the pH of chemical nickel waste liquid with the NaOH that concentration is 2g/L
To 9-10, it is heated to 85-90 DEG C；
Step 2: by concentration be 0.5ml/LSSC EN STARTER initiator add chemical nickel waste liquid；
Step 3: every adding reducing agent that concentration are 1g/L for 5 minutes points 3 times and concentration is the NaOH of 2g/L, stir 20
Minute；
Step 4: stop stirring, be filtrated to get filtrate A；
Step 5: adjust the pH to 11-13 of filtrate A with the NaOH that concentration is 2g/L, adds the SSC EN that concentration is 1g/L
WT ST additive also stirs at least 0.5 hour；
Step 6: filter obtain liquor B, with in dilute sulfuric acid and liquor B 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 to be described the preferred embodiment of the present invention, not enters the scope of the present invention
Row limits, on the premise of designing spirit without departing from the present invention, and this area ordinary skill technical staff technical side to the present invention
Various deformation that case is made and improvement, all should fall in the protection domain that claims of the present invention determines.
Claims (7)
1. the nickel recovery and treatment method in a chemical nickel plating waste solution, it is characterised in that: comprise the following steps:
Step one: adjust the pH to 6-10 of chemical nickel waste liquid with the NaOH that concentration is 2g/L, in chemical nickel waste liquid now, nickel contains
Amount is 4-7g/L, and sodium hypophosphite is 10-40g/L；
Step 2: SSC EN STARTER initiator is added in chemical nickel spent liquor solution, chemical nickel spent liquor solution is heated up to
70-95 DEG C, now produce substantial amounts of fine nickel-phosphorus alloy granule；
Step 3: added concentration every 5 minutes and be the reducing agent of 1g/L and concentration is the NaOH of 2g/L, stir at least 0.4-every time
1 hour, stir 0-3 time；
Step 4: obtaining filtrate A after filtration and reclaim nickel-phosphorus alloy granule, nickel contained in filtrate A is about 5-30ppm, uses
Concentration is the pH to 11-13 of the NaOH adjustment filtrate A of 2g/L；
Step 5: add the SSC EN WT ST additive that concentration is 0.1-1g/L in filtrate A, stir 0.4-1 hour；
Step 6: stop stirring, obtains liquor B after filtration, with in dilute sulfuric acid and liquor B is to pH 6-8.
Nickel recovery and treatment method in a kind of chemical nickel plating waste solution the most according to claim 1, it is characterised in that: described
SSC EN STARTER initiator comprises the combination of compounds of sodium hypophosphite, sodium sulfite, metallic compound.
Nickel recovery and treatment method in a kind of chemical nickel plating waste solution the most according to claim 1, it is characterised in that: described
Metallic compound is aluminum or stannum or zinc or a combination thereof compound.
The processing method of a kind of chemical nickel plating waste solution the most according to claim 1, it is characterised in that: described SSC EN
STARTER initiator concentration is 0.03 0.5ml/L.
Nickel recovery and treatment method in a kind of chemical nickel plating waste solution the most according to claim 1, it is characterised in that: described
SSC EN WT ST additive comprises the reproducibility compound of sodium hypophosphite and/or sodium sulfite.
Nickel recovery and treatment method in a kind of chemical nickel plating waste solution the most according to claim 1, it is characterised in that: Jing Guobu
In rapid six Filtrate B, nickel content is less than 0.3ppm, directly discharges after regulation pH.
Nickel recovery and treatment method in a kind of chemical nickel plating waste solution the most according to claim 1, it is characterised in that: Jing Guobu
In rapid six Filtrate B, ortho phosphorous acid sodium content is the lowest, and liquor B can be used as the raw material of fertilizer.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 CN106148709B (en) | 2018-01-05 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114032558A (en) * | 2021-12-14 | 2022-02-11 | 北京科技大学 | Method for preparing NiP micron particles from chemical nickel plating waste liquid through electrolysis |
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|---|---|---|---|---|
| JPS59185770A (en) * | 1983-04-05 | 1984-10-22 | Oosakafu | Method for recovering nickel from waste chemical nickel plating bath |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114032558A (en) * | 2021-12-14 | 2022-02-11 | 北京科技大学 | Method for preparing NiP micron particles from chemical nickel plating waste liquid through electrolysis |
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| CN106148709B (en) | 2018-01-05 |
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