CN108707936A - The method that choline chloride-glycerine system electrochemistry prepares metal spelter coating - Google Patents
The method that choline chloride-glycerine system electrochemistry prepares metal spelter coating Download PDFInfo
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- CN108707936A CN108707936A CN201810685829.8A CN201810685829A CN108707936A CN 108707936 A CN108707936 A CN 108707936A CN 201810685829 A CN201810685829 A CN 201810685829A CN 108707936 A CN108707936 A CN 108707936A
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- Prior art keywords
- glycerine
- choline chloride
- spelter coating
- zinc
- prepares metal
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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
- C25D3/66—Electroplating: Baths therefor from melts
- C25D3/665—Electroplating: Baths therefor from melts from ionic liquids
Abstract
The present invention relates to the methods that a kind of choline chloride-glycerine system electrochemistry prepares metal spelter coating, configure choline chloride-original electrolyte of glycerine-zinc chloride, using zinc metal sheet as soluble anode, red copper block is as cathode, electrode is immersed after above-mentioned ionic liquid and is connect with power supply by copper wire, high current density constant current electro-deposition is carried out under constant temperature, and after electro-deposition, sample is cleaned by ultrasonic, is dried.This method raw material is simple, easy to operate, safe and non-toxic, electric conductivity is excellent, improves electrodepositing speed, reduces manufacturing cost.
Description
Technical field
The present invention relates to electroplating technology fields, and in particular to a kind of choline chloride-glycerine system electrochemistry prepares metal
The method of spelter coating.
Background technology
China is the maximum country of zinc reserves, and China's zinc yield ranked first in the world since 1992.Metallic zinc conduct
A kind of basic material in modern industrial society, is widely used in various fields.Electrogalvanizing is widely used in steel material
Protective coating is suitble to be widely popularized in large-scale industrial production since the electro-deposition techniques cost of zinc is relatively low.
Especially prevent atmospheric corrosion.Traditional galvanized method has zinc-plated, chloride galvanizing of cyanide etc..Wherein cyanide is zinc-plated because containing
The cyanide of severe toxicity, it is seriously polluted.Contain a large amount of potassium chloride severe corrosion to equipment in chloride galvanizing electroplate liquid.How
It obtains the metallic zinc of high quality and elimination electrodeposit liquid has become Green Electrochemical and environment-protecting industrial to the harm of environment and urgently solves
Certainly the problem of.
Ionic liquid be it is a kind of salt being melted by the room temperature that ion is constituted completely, usually by geometry it is asymmetric it is organic sun from
Sub and inorganic or organic anion composition.Ionic liquid is high with chemical thermal stability, non-combustible, steam forces down, conductivity is high,
The characteristics such as small toxicity, electrochemical window mouth width.Ionic liquid can be obtained the ability electro-deposition in high-temperature molten salt and obtains at room temperature
Metal and its alloy, but again without strong corrosive as high-temperature molten salt.Eutectic ionic liquid is typically by centainly changing
Learn the eutectic mixing that the quaternary ammonium salt for measuring ratio and hydrogen-bond donor (such as amide, carboxylic acid and polyalcohol compound) are composed
Object.Eutectic ionic liquid have electrochemical window mouth width, dissolubility and good conductivity, steam forces down and good physical chemistry
The advantages that stability is a kind of novel green solvent.In terms of electrodeposit metals, since eutectic ionic liquid can select
Property dissolving metal oxide, while there is good electric conductivity and relatively negative reduction potential, i.e. electrodepositable obtains at room temperature
To most of metals that can be obtained in aqueous solution, obtained metal quality is good, and current efficiency is high.Simultaneously as eutectic is molten
The preparation process of agent is simple, low in raw material price, has broad application prospects in non-ferrous metallurgy technology field.State's inner beam
Seminar of army is somebody's turn to do by successfully preparing spelter coating by adding zinc chloride in choline chloride-urea eutectic system
It is relatively low that method prepares current density used by spelter coating, and electrodepositing speed is relatively slow, and (Wang Wei, big, the Liang Jun of first blueness, waits chlorination courages
[ of the Mg alloy surface electro-deposition current density to zinc coat performance in alkali-urea ionic liquid;J]Material protection, 2013,
46(8):1-4.).Number of patent application 201510821792.3, title are " a kind of based on choline chloride-xylitol eutectic solvent
Electrogalvanizing method " application discloses a kind of method preparing zinc coating, this method with xylitol, choline chloride, distilled water according to
Molar ratio 1：2：3 obtain ionic liquid, and zinc chloride is then added and is electroplated to obtain zinc coating.Change method addition distilled water amount compared with
It is more, hydrogen is easy tod produce using high current density.
Invention content
The purpose of the present invention is being directed to current eutectic electro-deposition to prepare some problems existing for spelter coating, a kind of profit is proposed
The method that electro-deposition prepares spelter coating is carried out with choline chloride-glycerine-zinc chloride system, this method raw material is simple, operation is simple
Just, safe and non-toxic, electric conductivity is excellent, improves electrodepositing speed, reduces manufacturing cost.
To achieve the above object, technical solution provided by the invention is：
A kind of method that choline chloride-glycerine system electrochemistry prepares metal spelter coating, it is characterised in that：Including as follows
Step：
1) configuration of electrolyte：By a certain percentage then choline chloride, glycerine and zinc chloride are heated after mixing
To 63 DEG C~67 DEG C, constant temperature is that choline chloride-glycerine-zinc chloride is original until the sticky liquid of the transparence of stirring generation
Electrolyte；A certain amount of anhydrous second is added in choline chloride-glycerine-zinc chloride ionic liquid then according to fixed volume ratio
Alcohol reduces the viscosity of ionic liquid；
2) connection electrode：In above-mentioned ionic liquid, zinc metal sheet as soluble anode, red copper block as cathode, anode and
Distance is 3cm between cathode；
3) electro-deposition：Electrode is immersed after above-mentioned ionic liquid and is connect with power supply by copper wire, high current is carried out under constant temperature
Density constant current electro-deposition；
4) sample is taken out：After electro-deposition, sample is cleaned by ultrasonic, is dried；
In step 1), the ratio molar ratio of choline chloride, glycerine and zinc chloride is 2 in electrolyte:6:1.
In step 1), the volume ratio of absolute ethyl alcohol and choline chloride-original electrolyte of glycerine-zinc chloride is 1：20.
In step 2), using double anode.
In step 3), constant current density 50-60mA/cm2。
In step 3), electrodeposition temperature is 63 DEG C~67 DEG C.
In step 3), electrodeposition time is 40-60 minutes.
Compared with prior art, the beneficial effects of the invention are as follows：
The raw material that the present invention uses is simple, requires no recrystallization processing, only adds a small amount of ethyl alcohol, add without other
Add agent, operation is simple, environmentally protective, safe and non-toxic, and adoptable current density is high, and electrodepositing speed is fast, can be
Thick spelter coating is quickly prepared on Copper substrate.
Description of the drawings
Fig. 1 is the SEM linear sweep graphs of the spelter coating obtained in example 1.
Fig. 2 is the EDS collection of illustrative plates of the spelter coating obtained in example 2.
Fig. 3 is the SEM fracture figures of the spelter coating obtained in example 3.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
Embodiment 1
1) molar ratio of choline chloride, glycerine and zinc chloride is 2 in original electrolyte:6:1, by a certain percentage by chlorination
Choline and glycerine are then heated to 63 DEG C after mixing, and constant temperature is until the sticky liquid of the transparence of stirring generation.Then
It is 1 according to the volume ratio of absolute ethyl alcohol and choline chloride-glycerine-zinc chloride ionic liquid：20 are added one in former ionic liquid
Quantitative absolute ethyl alcohol.
2) using zinc metal sheet as soluble anode, red copper block is put into as cathode in the above-mentioned mixing liquid for being heated to 63 DEG C
Double anode constant current electro-deposition in 40 minutes is carried out, distance is 3cm, current density 50mA/cm wherein between anode and cathode2。
3) after electro-deposition, sample taking-up absolute ethyl alcohol, deionized water is cleaned by ultrasonic, finally blown with hair-dryer low temperature.
The SEM linear sweep graphs of gained coating are referring to Fig. 1, it can be found that the coating on red copper matrix is coated layer.
Embodiment 2
1) molar ratio of choline chloride, glycerine and zinc chloride is 2 in original electrolyte:6:1, by a certain percentage by chlorination
Choline and glycerine are then heated to 65 DEG C after mixing, and constant temperature is until the sticky liquid of the transparence of stirring generation.Then
It is 1 according to the volume ratio of absolute ethyl alcohol and choline chloride-glycerine-zinc chloride ionic liquid：20 are added one in former ionic liquid
Quantitative absolute ethyl alcohol.
2) using zinc metal sheet as soluble anode, red copper block is put into as cathode in the above-mentioned mixing liquid for being heated to 65 DEG C
Double anode constant current electro-deposition in 50 minutes is carried out, distance is 3cm, current density 55mA/cm wherein between anode and cathode2。
3) after electro-deposition, sample taking-up absolute ethyl alcohol, deionized water is cleaned by ultrasonic, finally blown with hair-dryer low temperature.
The Surface energy spectrum analysis figure of gained coating is referring to Fig. 2, it can be found that the coating on red copper matrix is spelter coating.
Embodiment 3
1) molar ratio of choline chloride, glycerine and zinc chloride is 2 in original electrolyte:6:1, by a certain percentage by chlorination
Choline and glycerine are then heated to 67 DEG C after mixing, and constant temperature is until the sticky liquid of the transparence of stirring generation.Then
It is 1 according to the volume ratio of absolute ethyl alcohol and choline chloride-glycerine-zinc chloride ionic liquid：20 are added one in former ionic liquid
Quantitative absolute ethyl alcohol.
2) using zinc metal sheet as soluble anode, red copper block is put into as cathode in the above-mentioned mixing liquid for being heated to 67 DEG C
Double anode constant current electro-deposition in 60 minutes is carried out, distance is 3cm, current density 60mA/cm wherein between anode and cathode2。
3) after electro-deposition, sample taking-up absolute ethyl alcohol, deionized water is cleaned by ultrasonic, finally blown with hair-dryer low temperature.
The SEM fractures of gained coating are referring to Fig. 3, it can be found that red copper matrix and coating are tightly combined.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, any ripe
Professional and technical personnel is known, without departing from the scope of the present invention, according to the technical essence of the invention, to above real
Apply any simple modification, equivalent replacement and improvement etc. made by example, still fall within technical solution of the present invention protection domain it
It is interior.
Claims (7)
1. the method that a kind of choline chloride-glycerine system electrochemistry prepares metal spelter coating, it is characterised in that：Including walking as follows
Suddenly：
1) configuration of electrolyte：Choline chloride, glycerine and zinc chloride are then heated to 63 after mixing by a certain percentage
DEG C~67 DEG C, constant temperature is choline chloride-original electrolysis of glycerine-zinc chloride until the sticky liquid of the transparence of stirring generation
Liquid；A certain amount of absolute ethyl alcohol is added in choline chloride-glycerine-zinc chloride ionic liquid then according to fixed volume ratio,
Reduce the viscosity of ionic liquid；
2) connection electrode：In above-mentioned ionic liquid, zinc metal sheet is as soluble anode, and red copper block is as cathode, anode and cathode
Between distance be 3cm；
3) electro-deposition：Electrode is immersed after above-mentioned ionic liquid and is connect with power supply by copper wire, high current density is carried out under constant temperature
Constant current electro-deposition；
4) sample is taken out：After electro-deposition, sample is cleaned by ultrasonic, is dried.
2. the method that choline chloride according to claim 1-glycerine system electrochemistry prepares metal spelter coating, feature
It is：In step 1), the ratio molar ratio of choline chloride, glycerine and zinc chloride is 2 in electrolyte:6:1.
3. the method that choline chloride according to claim 1-glycerine system electrochemistry prepares metal spelter coating, feature
It is：In step 1), the volume ratio of absolute ethyl alcohol and choline chloride-original electrolyte of glycerine-zinc chloride is 1：20.
4. the method that choline chloride according to claim 1-glycerine system electrochemistry prepares metal spelter coating, feature
It is：In step 2), using double anode.
5. the method that choline chloride according to claim 1-glycerine system electrochemistry prepares metal spelter coating, feature
It is：In step 3), constant current density 50-60mA/cm2。
6. the method that choline chloride according to claim 1-glycerine system electrochemistry prepares metal spelter coating, feature
It is：In step 3), electrodeposition temperature is 63 DEG C~67 DEG C.
7. the method that choline chloride according to claim 1-glycerine system electrochemistry prepares metal spelter coating, feature
It is：In step 3), electrodeposition time is 40-60 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109825289A (en) * | 2019-03-26 | 2019-05-31 | 河北科技大学 | A kind of eutectic solvent is in the preparation method for preparing application and metal-doped carbon quantum dot in metal-doped carbon quantum dot |
| CN114378300A (en) * | 2022-01-21 | 2022-04-22 | 重庆科技学院 | Method for preparing nano copper powder by using copper oxide as raw material |
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| CN105063665A (en) * | 2015-08-05 | 2015-11-18 | 北京工业大学 | Method for electrically depositing nanometer platinum powder from ionic liquid |
| CN105256343A (en) * | 2015-11-23 | 2016-01-20 | 安徽工业大学 | Electrogalvanizing method based on choline chloride-xylitol deep eutectic solvent |
| CN106591890A (en) * | 2016-11-23 | 2017-04-26 | 昆明理工大学 | Method for preparing micro-nano-porous silver based on eutectic flux in-situ alloy deposition/alloy removing method |
| CN107761142A (en) * | 2017-11-10 | 2018-03-06 | 昆明理工大学 | A kind of method of eutectic solvent Electrodeposition Bath of Iron evanohm coating |
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2018
- 2018-06-28 CN CN201810685829.8A patent/CN108707936A/en active Pending
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| CN105063665A (en) * | 2015-08-05 | 2015-11-18 | 北京工业大学 | Method for electrically depositing nanometer platinum powder from ionic liquid |
| CN105256343A (en) * | 2015-11-23 | 2016-01-20 | 安徽工业大学 | Electrogalvanizing method based on choline chloride-xylitol deep eutectic solvent |
| CN106591890A (en) * | 2016-11-23 | 2017-04-26 | 昆明理工大学 | Method for preparing micro-nano-porous silver based on eutectic flux in-situ alloy deposition/alloy removing method |
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| CN109825289A (en) * | 2019-03-26 | 2019-05-31 | 河北科技大学 | A kind of eutectic solvent is in the preparation method for preparing application and metal-doped carbon quantum dot in metal-doped carbon quantum dot |
| CN114378300A (en) * | 2022-01-21 | 2022-04-22 | 重庆科技学院 | Method for preparing nano copper powder by using copper oxide as raw material |
| CN114378300B (en) * | 2022-01-21 | 2023-10-20 | 重庆科技学院 | Method for preparing nanometer copper powder by taking copper oxide as raw material |
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