CN105908223A - Alkaline electrolyte and method for preparing bright nickel by means of electrolysis in alkaline electrolyte - Google Patents
Alkaline electrolyte and method for preparing bright nickel by means of electrolysis in alkaline electrolyte Download PDFInfo
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- CN105908223A CN105908223A CN201610412645.5A CN201610412645A CN105908223A CN 105908223 A CN105908223 A CN 105908223A CN 201610412645 A CN201610412645 A CN 201610412645A CN 105908223 A CN105908223 A CN 105908223A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/36—Pretreatment of metallic surfaces to be electroplated of iron or steel
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
- C25D5/40—Nickel; Chromium
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- Chemical Kinetics & Catalysis (AREA)
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses an alkaline electrolyte and a method for preparing bright nickel by means of electrolysis in the alkaline electrolyte. The alkaline electrolyte comprises nickel chloride, ammonium chloride, ammonia water, benzene sulfinic acid sodium salt and water, wherein the concentration of nickel chloride is 50g/L to 400g/L; the concentration of ammonium chloride is 80g/L to 450g/L; the concentration of ammonia water is 30g/L to 350g/L; the concentration of benzene sulfinic acid sodium salt is 0.03g/L to 1g/L. The method for preparing bright nickel by means of electrolysis in the alkaline electrolyte comprises the following steps: (1) preparing the alkaline electrolyte; (2) removing surface oxide layers of a cathode material, degreasing the cathode material, and soaking an anode material in nitric acid to remove the surface oxide layers and impurities; (3) performing electro-deposition on the pretreated cathode material and anode material in an electrolytic cell containing the alkaline electrolyte to obtain a bright and smooth nickel layer. The alkaline electrolyte disclosed by the invention is capable of effectively solving the difficult problem that a deposited nickel layer is black and fragile and can be used for successfully preparing bright nickel; the method has the advantages that the current efficiency is high, the prepared nickel is bright and good in toughness and the like.
Description
(1) technical field
The present invention relates to a kind of alkaline electrolyte and in this alkaline electrolyte the method for electrolytic preparation bright nickel, belong to
In technical field of non-ferrous metallurgy.
(2) background technology
In the electrolytic industry of current nickel produces, mainly carry out electrolytic preparation light with the watts nickel liquid of boric acid system
Nickel, this technique is through the transformation of many decades and innovation, the most perfect, the most ripe, but is as society
Development, science and technology progress, traditional electrolytic nickel technique the most day by day appear its exist shortcoming.Tradition
Electrolytic nickel technique exist shortcoming as follows:
1. use acid system electrolytic nickel technique, with boric acid as buffer agent, need strictly to be controlled by pH 4.5～5.4
In the range of, the too low meeting of pH causes cathode efficiency to reduce, and the too high meeting of pH causes the formation of nickel hydroxide, nickel
Physical property and bad appearance.
2. use sulfate～chlorate mixed system electrolytic nickel electric current density low, it is difficult to strengthening digestion, production capacity mistake
Low.
3. obtain the thick nickel of raw material of electrolytic nickel, nickel sulfide, converter mattes, need through numerous and diverse production technology, week
Phase is long, and waste material is many, and energy consumption is big.And using diaphragm electrolysis, tank voltage is high, adds energy consumption, cleaning system
Long flow path, operation easier is big.
Therefore, a kind of relative efficiency of research is green, technological process relative ease, it is possible to be suitable for automatic and mechanical
Producing, increase production capacity, the pH scope expanding buffer additive prepares the electrolytic method of bright nickel for nickel work
Industry produces self-evident huge meaning, and also complies with the green production policy that country advocates instantly.With
Ammonia leaching solution has the highest researching value directly as electrolyte electrolytic nickel, but relative to the most ripe nickel
Industrial electrolysis nickel system, the research of this respect is the most blank, and there is many deficiencies in related application.
Disclosure sets forth the research of electrolytic preparation bright nickel under alkaline system, there is huge prospect, environment
And economic benefit.
(3) summary of the invention
It is an object of the invention to the deficiency for existing boric acid system, and nickel ammonia complexing alkaline system electrolytic preparation
Nickel blackout embrittlement problem, propose a kind of alkaline electrolyte and in this alkaline system the side of electrolytic preparation bright nickel
Method, described alkaline electrolyte, by adding appropriate benzene sulfinic acid sodium salt at nickel ammonia complexing alkaline system, can solve effectively
Certainly a difficult problem for deposited nickel layer blackout embrittlement, successfully prepares bright nickel, and it is high that this method has current efficiency, preparation
Nickel light, the advantage such as toughness is good.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of alkaline electrolyte, it includes Nickel dichloride., ammonium chloride, ammonia, benzene sulfinic acid sodium salt and water, wherein chlorine
Change nickel concentration scope be 50～400g/L, ammonium chloride concentration scope be 80～450g/L, ammonia concn (with
NH3·H2O counts) scope is 30～350g/L, benzene sulfinic acid sodium salt concentration range is 0.03～1g/L.
Further, described Nickel dichloride. preferred concentration is 80～200g/L.
Further, described ammonium chloride preferred concentration is 100～350g/L.
Further, described ammonia preferred concentration is 50～250g/L.
Further, described benzene sulfinic acid sodium salt preferred concentration is 0.05～0.4g/L.
Further, described alkaline electrolyte is by the preparation of Nickel dichloride., ammonium chloride, ammonia, benzene sulfinic acid sodium salt and water
Become.
Further, the preparation steps of described alkaline electrolyte is: Nickel dichloride., ammonium chloride are added in a small amount of water
Heating for dissolving, adds ammonia and water mixing after solution cools down, stirs under 25～65 DEG C of constant temperatures,
Adding benzene sulfinic acid sodium salt, final preparation obtains alkaline electrolyte.
Invention further provides a kind of method of electrolytic preparation bright nickel in alkaline electrolyte, described method
Comprise the following steps:
(1) preparation alkaline electrolyte；
(2) cathode material is removed surface oxide layer, oil removal treatment, anode material is placed in 1～5mol/L
Nitric acid in soak 10～60min removal surface oxide layers and impurity；
(3) cathode material after step (2) pre-treatment and anode material are placed in equipped with alkaline electrolyte
In electrolysis bath, control electrodeposition temperature 25～65 DEG C and electrolyte mixing speed 250～650r/min, use permanent electricity
The mode of stream, controlling electric current density electric current density is-100～-500A/m2, electro-deposition 0.5～100h, take out the moon
Pole washes, cold wind i.e. obtains the nickel dam that light is smooth after drying up.
Further, in step (2), cathode material can be that existing electrolysis tech field can be used as negative electrode
Electrode material, preferably cathode material is rustless steel, nickel or copper.In negative electrode pre-treatment, it is generally available sand paper and beats
Grinding off except oxide on surface, then carry out oil removing cleaning by cleaning solvent, cleaning solvent can be acetone, second
Alcohol, water etc..
Further, in step (2), anode material can be that existing electro-deposition techniques field can be used as sun
The electrode material of pole, preferred anodes material is thick nickel, nickel sulfide or converter mattes.In anode pre-treatment, nitric acid is dense
Degree is preferably 2～4mol/L, and soak time is preferably 20～40min.
Further, in step (2), electrolysis temperature ranges preferably from 40～60 DEG C.
Further, in step (2), electrolyte mixing speed is preferably 300～500r/min.
Further, in step (2), electric current density is preferably-200～-400A/m2。
Further, in step (2), electrolysis time is preferably 1～40h.
Further, in step (2), the bright nickel layer obtained by electrolysis, for high-purity nickel
Further, described preparation is made up of step (1)～(3).
The invention has the beneficial effects as follows: the present invention solves asking of the blackout embrittlement of electrolytic nickel in nickel ammonia alkaline system
Topic, the bright nickel prepared under alkaline system, there is preferable toughness, it is possible to meet industrial requirement.This
Bright required electrolyte can obtain with ammonia extract technology, technological process is simple, and anode does not produce poisonous chlorine,
Environmental protection, has huge prospect, environment and economic benefit.
(4) accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of embodiment 3 electrolytic nickel.
(5) detailed description of the invention
Below by specific embodiment, the present invention is further detailed, but protection scope of the present invention is also
It is not limited only to this.
Embodiment 1
Configuration chloride containing nickel 50g/L, ammonium chloride 80g/L, ammonia 30g/L, the electricity of benzene sulfinic acid sodium salt 0.03g/L
Solve liquid 250mL.With thick nickel electrode anode, in the nitric acid of 1mol/L, leaching is put 60min and is removed surface oxide layer
And impurity, taking-up deionized water rinsing, cold wind dries up.With rustless steel as cathode material, respectively through 1#,
After 3#, 5# sand papering, dehydrated alcohol oil removing, deionized water wash cold wind dry up, by negative electrode, anode simultaneously
Putting in electrolysis bath, controlling electrodeposition temperature is 25 DEG C, and electric current density is-500A/m2, stirring electrolyte speed
Degree is 650r/min, after electro-deposition 0.5h, takes out negative electrode, rinses the entrained electrolyte on surface, cold wind with water
After drying up, nickel is peeled off from rustless steel, obtain surface-brightening and be rich in the high purity nickel of toughness.
The current efficiency of the electrolytic nickel based on example 1 is 98.35%.
Embodiment 2
Configuration chloride containing nickel 400g/L, ammonium chloride 450g/L, ammonia 350g/L, the electricity of benzene sulfinic acid sodium salt 1g/L
Solve liquid 250mL.With thick nickel electrode anode, in the nitric acid of 5mol/L, leaching is put 10min and is removed surface oxide layer
And impurity, taking-up deionized water rinsing, cold wind dries up.With rustless steel as cathode material, respectively through 1#,
After 3#, 5# sand papering, dehydrated alcohol oil removing, deionized water wash cold wind dry up, by negative electrode, anode simultaneously
Putting in electrolysis bath, controlling electrodeposition temperature is 65 DEG C, and electric current density is-100A/m2, stirring electrolyte speed
Degree is 250r/min, after electro-deposition 100h, takes out negative electrode, rinses the entrained electrolyte on surface, cold wind with water
After drying up, nickel is peeled off from rustless steel, obtain surface-brightening and be rich in the high purity nickel of toughness.
The current efficiency of the electrolytic nickel based on example 2 is 97.73%.
Embodiment 3
Configuration chloride containing nickel 80g/L, ammonium chloride 100g/L, ammonia 50g/L, benzene sulfinic acid sodium salt 0.05g/L's
Electrolyte 250mL.With thick nickel electrode anode, in the nitric acid of 2mol/L, leaching is put 40min and is removed surface oxidation
Layer and impurity, taking-up deionized water rinsing, cold wind dries up.With rustless steel as cathode material, respectively through
After 1#, 3#, 5# sand papering, dehydrated alcohol oil removing, deionized water wash cold wind dry up, by negative electrode, anode
Putting in electrolysis bath, controlling electrodeposition temperature is 40 DEG C, and electric current density is-400A/m simultaneously2, stirring electrolysis
Liquid speed is 500r/min, after electro-deposition 1h, takes out negative electrode, rinses the entrained electrolyte on surface with water, cold
After wind is dry, nickel is peeled off from rustless steel, obtains surface-brightening and be rich in the high purity nickel of toughness.
The current efficiency of the electrolytic nickel based on example 3 is 96.98%.
Embodiment 4
Configuration chloride containing nickel 200g/L, ammonium chloride 350g/L, ammonia 250g/L, benzene sulfinic acid sodium salt 0.4g/L's
Electrolyte 250mL.With thick nickel electrode anode, in the nitric acid of 4mol/L, leaching is put 20min and is removed surface oxidation
Layer and impurity, taking-up deionized water rinsing, cold wind dries up.With rustless steel as cathode material, respectively through
After 1#, 3#, 5# sand papering, dehydrated alcohol oil removing, deionized water wash cold wind dry up, by negative electrode, anode
Putting in electrolysis bath, controlling electrodeposition temperature is 60 DEG C, and electric current density is-200A/m simultaneously2, stirring electrolysis
Liquid speed is 500r/min, after electro-deposition 40h, takes out negative electrode, rinses the entrained electrolyte on surface with water,
After cold wind dries up, nickel is peeled off from rustless steel, obtain surface-brightening and be rich in the high purity nickel of toughness.
The current efficiency of the electrolytic nickel based on example 4 is 97.55%.
Embodiment 5
Configuration chloride containing nickel 130g/L, ammonium chloride 212g/L, ammonia 126g/L, benzene sulfinic acid sodium salt 0.2g/L's
Electrolyte 250mL.With thick nickel electrode anode, in the nitric acid of 3mol/L, leaching is put 30min and is removed surface oxidation
Layer and impurity, taking-up deionized water rinsing, cold wind dries up.With rustless steel as cathode material, respectively through
After 1#, 3#, 5# sand papering, dehydrated alcohol oil removing, deionized water wash cold wind dry up, by negative electrode, anode
Putting in electrolysis bath, controlling electrodeposition temperature is 50 DEG C, and electric current density is-300A/m simultaneously2, stirring electrolysis
Liquid speed is 400r/min, after electro-deposition 15h, takes out negative electrode, rinses the entrained electrolyte on surface with water,
After cold wind dries up, nickel is peeled off from rustless steel, obtain surface-brightening and be rich in the high purity nickel of toughness.
The current efficiency of the electrolytic nickel based on example 5 is 98.69%.
Embodiment 6
Configuration chloride containing nickel 130g/L, ammonium chloride 212g/L, ammonia 126g/L, benzene sulfinic acid sodium salt 0.2g/L's
Electrolyte 250mL.With nickel sulfide electrode anode, in the nitric acid of 3mol/L, leaching is put 30min and is removed Surface Oxygen
Changing layer and impurity, taking-up deionized water rinsing, cold wind dries up.With copper as cathode material, respectively through 1#,
After 3#, 5# sand papering, dehydrated alcohol oil removing, deionized water wash cold wind dry up, by negative electrode, anode simultaneously
Putting in electrolysis bath, controlling electrodeposition temperature is 50 DEG C, and electric current density is-300A/m2, stirring electrolyte speed
Degree is 400r/min, after electro-deposition 15h, takes out negative electrode, rinses the entrained electrolyte on surface, cold wind with water
After drying up, nickel is peeled off from rustless steel, obtain surface-brightening and be rich in the high purity nickel of toughness.
The current efficiency of the electrolytic nickel based on example 6 is 96.88%.
Embodiment 7
Configuration chloride containing nickel 130g/L, ammonium chloride 212g/L, ammonia 126g/L, benzene sulfinic acid sodium salt 0.2g/L's
Electrolyte 250mL.With converter mattes electrode anode, in the nitric acid of 3mol/L, leaching is put 30min and is removed Surface Oxygen
Changing layer and impurity, taking-up deionized water rinsing, cold wind dries up.With nickel as cathode material, respectively through 1#,
After 3#, 5# sand papering, dehydrated alcohol oil removing, deionized water wash cold wind dry up, by negative electrode, anode simultaneously
Putting in electrolysis bath, controlling electrodeposition temperature is 50 DEG C, and electric current density is-300A/m2, stirring electrolyte speed
Degree is 400r/min, after electro-deposition 15h, takes out negative electrode, rinses the entrained electrolyte on surface, cold wind with water
After drying up, nickel is peeled off from rustless steel, obtain surface-brightening and be rich in the high purity nickel of toughness.
The current efficiency of the electrolytic nickel based on example 7 is 97.52%.
Claims (10)
1. an alkaline electrolyte, it is characterised in that: described alkaline electrolyte include Nickel dichloride., ammonium chloride,
Ammonia, benzene sulfinic acid sodium salt and water, wherein Nickel dichloride. concentration range be 50～400g/L, ammonium chloride concentration scope be
80～450g/L, ammonia concn scope be 30～350g/L, benzene sulfinic acid sodium salt concentration range be 0.03～1g/L.
2. alkaline electrolyte as claimed in claim 1, it is characterised in that: described alkaline electrolyte is by chlorination
Nickel, ammonium chloride, ammonia, benzene sulfinic acid sodium salt and water are formulated.
3. alkaline electrolyte as claimed in claim 1 or 2, it is characterised in that: described Nickel dichloride. concentration is
80～200g/L.
4. alkaline electrolyte as claimed in claim 1 or 2, it is characterised in that: described ammonium chloride concentration is
100～350g/L.
5. alkaline electrolyte as claimed in claim 1 or 2, it is characterised in that: described ammonia concn is
50～250g/L.
6. alkaline electrolyte as claimed in claim 1 or 2, it is characterised in that: described benzene sulfinic acid sodium salt is dense
Degree is 0.05～0.4g/L.
7. a method for electrolytic preparation bright nickel in alkaline electrolyte, said method comprising the steps of:
(1) alkaline electrolyte as claimed in claim 1 is prepared；
(2) cathode material is removed surface oxide layer, oil removal treatment, anode material is placed in 1～5mol/L
Nitric acid in soak 10～60min removal surface oxide layers and impurity；
(3) cathode material after step (2) pre-treatment and anode material are placed in equipped with alkaline electrolyte
Electrolysis bath in, control electrodeposition temperature 25～65 DEG C and electrolyte mixing speed 250～650r/min, use
The mode of constant current, controlling electric current density electric current density is-100～-500A/m2, electro-deposition 0.5～100h, take
Go out that negative electrode washes, cold wind i.e. obtains the smooth nickel dam of light after drying up.
8. the method for electrolytic preparation bright nickel in alkaline electrolyte as claimed in claim 7, its feature exists
In: in step (2), cathode material is rustless steel, nickel or copper；Anode material is thick nickel, nickel sulfide or height
Ice nickel.
9. the method for electrolytic preparation bright nickel in alkaline electrolyte as claimed in claim 7 or 8, it is special
Levying and be: in step (2), electrolysis temperature scope is 40～60 DEG C；Electrolyte mixing speed is 300～500r/min；
Electric current density is-200～-400A/m2；Electrolysis time is 1～40h.
10. the method for electrolytic preparation bright nickel in alkaline electrolyte as claimed in claim 7 or 8, its
It is characterised by: described preparation is made up of step (1)～(3).
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| CN201610412645.5A CN105908223A (en) | 2016-06-14 | 2016-06-14 | Alkaline electrolyte and method for preparing bright nickel by means of electrolysis in alkaline electrolyte |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108374183A (en) * | 2018-03-14 | 2018-08-07 | 浙江工业大学 | A kind of Ni-based composite array material and its preparation process and application |
| CN108411323A (en) * | 2018-03-16 | 2018-08-17 | 浙江工业大学 | A kind of preparation method and applications of nickel-nickel selenium core-shell structure copolymer array material |
| CN108456901A (en) * | 2018-03-16 | 2018-08-28 | 浙江工业大学 | A kind of preparation method and applications of nickel selenium array material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108374183A (en) * | 2018-03-14 | 2018-08-07 | 浙江工业大学 | A kind of Ni-based composite array material and its preparation process and application |
| CN108411323A (en) * | 2018-03-16 | 2018-08-17 | 浙江工业大学 | A kind of preparation method and applications of nickel-nickel selenium core-shell structure copolymer array material |
| CN108456901A (en) * | 2018-03-16 | 2018-08-28 | 浙江工业大学 | A kind of preparation method and applications of nickel selenium array material |
| CN108411323B (en) * | 2018-03-16 | 2019-04-23 | 浙江工业大学 | A kind of preparation method and applications of nickel-nickel selenium core-shell structure copolymer array material |
| CN108456901B (en) * | 2018-03-16 | 2019-06-25 | 浙江工业大学 | A kind of preparation method and applications of nickel selenium array material |
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