CN114108031B - Environment-friendly cyanide-free alkaline copper plating refiner and preparation method thereof - Google Patents
Environment-friendly cyanide-free alkaline copper plating refiner and preparation method thereof Download PDFInfo
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- CN114108031B CN114108031B CN202111499919.6A CN202111499919A CN114108031B CN 114108031 B CN114108031 B CN 114108031B CN 202111499919 A CN202111499919 A CN 202111499919A CN 114108031 B CN114108031 B CN 114108031B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses an environment-friendly cyanide-free alkaline copper plating refiner and a preparation method thereof, and particularly relates to the technical field of metal surface treatment. An environment-friendly cyanide-free alkaline copper plating refiner comprises the following components in concentration: 0.1-1g/L of p-methoxy benzyl chloride and 1-10g/L of 7-chloroquinaldine, and the solvent is water. A preparation method of an environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps: weighing appropriate amount of p-methoxy benzyl chloride and 7-chloroquinaldine, adding a small amount of distilled water, continuously stirring until the p-methoxy benzyl chloride and the 7-chloroquinaldine are completely dissolved, and fixing the volume with the distilled water and uniformly mixing after clarifying. The technical scheme of the invention solves the problem of poor dispersibility and brightness of the copper plating layer of the cyanide-free copper plating, and can improve the stability of the cyanide-free copper plating.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to an environment-friendly cyanide-free alkaline copper plating refiner and a preparation method thereof.
Background
The electroplating is a process of plating a thin layer containing other metals or alloys on the surface of some metals by utilizing the principle of electrolysis, and is a process of adhering a layer of metal film on the surface of a metal or other material workpiece by utilizing the action of electrolysis, thereby playing the role of preventing the metal from being oxidized and also playing the roles of improving the wear resistance, the conductivity, the light reflection property, the corrosion resistance and the like. The electroplating process is basically as follows: the plating metal is at the anode, the substance to be plated is at the cathode, and the cathode and the anode are connected through electrolyte solution. When a direct current power supply is applied, the metal at the anode is oxidized (electrons are lost), and positive ions in the solution are reduced (electrons are obtained) at the cathode to form atoms and are accumulated on the surface layer of the cathode.
Various electroplating baths with cyanide as complexing agent have been used successfully for copper plating for many years. In these baths, copper is present as a complex of monovalent copper and cyanide. Although such baths have been used successfully, the industry has long sought alternatives to the highly toxic cyanide ions.
To date, there is no cyanide-free copper plating process that can completely replace cyanide copper plating. The difference of the performances of the plating solution is mainly reflected in the stability of the plating solution. The main difference of the coating performance is the dispersibility and the brightness of the coating, and the brightness of the cyanide-free copper plating is poorer than that of the cyanide copper plating.
The demand for finding a cyanide-free copper plating additive for obtaining a good plating layer is increasingly strong, and a solid step is taken for realizing the aim of replacing cyanide electroplating with cyanide electroplating in the early days.
Disclosure of Invention
The invention aims to provide an environment-friendly cyanide-free alkaline copper plating refiner and a preparation method thereof, and solves the problem that the dispersibility and the brightness of a copper plating layer of cyanide-free copper plating are poor.
In order to achieve the above purpose, one technical solution of the present invention is as follows: an environment-friendly cyanide-free alkaline copper plating refiner and a preparation method thereof, which comprises the following components in percentage by concentration: 0.1-1g/L of p-methoxy benzyl chloride and 1-10g/L of 7-chloroquinaldine, and the solvent is water.
Further, the solvent is distilled water.
The other technical scheme of the invention is as follows: a preparation method of an environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps: weighing appropriate amount of p-methoxy benzyl chloride and 7-chloroquinaldine, adding a small amount of distilled water, continuously stirring until the p-methoxy benzyl chloride and the 7-chloroquinaldine are completely dissolved, and fixing the volume with the distilled water and uniformly mixing after clarifying.
Compared with the prior art, the beneficial effect of this scheme:
the refiner can greatly reduce the roughness of the plated workpiece and reach the level close to or even surpass that of a cyanide copper plating layer. The scheme solves the problem of coarse crystallization of the cyanide-free copper plating layer, reduces the production cost of cyanide-free copper plating, thereby promoting the development of cyanide-free electroplating and being widely applied to the field of cyanide-free copper plating processes.
Detailed Description
The invention is explained in more detail below by means of specific embodiments:
example 1
An environment-friendly cyanide-free alkaline copper plating refiner comprises the following components: 10g of p-methoxybenzyl chloride with the concentration of 0.1g/L and 100g of 7-chloroquinaldine with the concentration of 1g/L, and the balance of the solution is distilled water. Wherein the p-methoxybenzyl chloride is also named 4-methoxybenzyl chloride and p-methoxybenzyl chloride, is colorless and odorless transparent liquid, and has a melting point of-1 ℃. The 7-chloroquinaldine is also named as 2-methyl-7-chloroquinoline, 7-chloro-2-methylquinoline and 7-chloroquinaldine, has a melting point of 75-77 ℃, is a white powder crystal and is soluble in water.
The preparation method of the environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps: dissolving p-methoxybenzyl chloride and 7-chloroquinaldine in a small amount of distilled water, stirring for dissolving until the solution is clear, then adding water to a constant volume of 1L, and continuously stirring to uniformly mix the solution.
The performance detection of the environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps:
10ml of the above prepared refiner was added to 1L of cyanide-free copper plating base solution. The cyanide-free copper plating base solution comprises the following components in parts by weight: 50-60 g/L of basic copper carbonate, 20-40 g/L of potassium sodium tartrate, 250-300 g/L of citric acid and 10-15 g/L of sodium carbonate. Hanging the iron piece to be plated in the prepared plating solution, wherein the plating time is 30min, and the current density is 1A/dm 2 At a temperature of 55 ℃. Meanwhile, in the cyanide-free copper plating solution and the cyanide copper plating solution without added refiner, the same type of iron piece is electroplated under the same electroplating condition. The roughness of iron pieces made in the three baths was compared.
The detection results are compared to show that: roughness of copper plating layer of iron piece: the additive is added to the cyanide-free copper plating, the cyanide copper plating is less than the cyanide copper plating.
Example 2
An environment-friendly cyanide-free alkaline copper plating refiner comprises the following components: 10g of p-methoxybenzyl chloride with the concentration of 0.5g/L and 100g of 7-chloroquinaldine with the concentration of 5g/L, and the balance of the solution is distilled water. Wherein the p-methoxybenzyl chloride is also named 4-methoxybenzyl chloride and p-methoxybenzyl chloride, is colorless and odorless transparent liquid, and has a melting point of-1 ℃. The 7-chloroquinaldine is also named as 2-methyl-7-chloroquinoline, 7-chloro-2-methylquinoline and 7-chloroquinaldine, has a melting point of 75-77 ℃, is a white powder crystal and is soluble in water.
The preparation method of the environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps: dissolving p-methoxybenzyl chloride and 7-chloroquinaldine in a small amount of distilled water, stirring for dissolving until the solution is clear, then adding water to a constant volume of 1L, and continuously stirring to uniformly mix the solution.
The performance detection of the environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps:
50ml of the refiner prepared above is added into 1L of cyanide-free copper plating base solution. The cyanide-free copper plating base solution comprises the following components in percentage by weight: 50-60 g/L of basic copper carbonate, 20-40 g/L of potassium sodium tartrate, 250-300 g/L of citric acid and 10-15 g/L of sodium carbonate. Hanging the iron piece to be plated in the prepared plating solution, wherein the plating time is 30min, and the current density is 1A/dm 2 At a temperature of 55 ℃. Meanwhile, in the cyanide-free copper plating solution and the cyanide copper plating solution without added refiner, the same type of iron piece is electroplated under the same electroplating condition. The roughness of iron pieces made in the three baths was compared.
The detection results are compared to show that: roughness of copper plating layer of iron part: the additive is added to the cyanide-free copper plating, the cyanide copper plating is less than the cyanide copper plating.
Example 3
An environment-friendly cyanide-free alkaline copper plating refiner comprises the following components: 10g of 1g/L p-methoxy benzyl chloride and 100g of 10 g/L7-chloroquinaldine, and the balance of the solution is distilled water. Wherein the p-methoxybenzyl chloride is also named 4-methoxybenzyl chloride and p-methoxybenzyl chloride, is colorless and odorless transparent liquid, and has a melting point of-1 ℃. The 7-chloroquinaldine is also named as 2-methyl-7-chloroquinoline, 7-chloro-2-methylquinoline and 7-chloroquinaldine, has a melting point of 75-77 ℃, is a white powder crystal and is soluble in water.
The preparation method of the environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps: dissolving p-methoxybenzyl chloride and 7-chloroquinaldine in a small amount of distilled water, stirring for dissolving until the solution is clear, then adding water to a constant volume of 1L, and continuously stirring to uniformly mix the solution.
The performance detection of the environment-friendly cyanide-free alkaline copper plating refiner comprises the following steps:
100ml of the refiner prepared above is added into 1L of cyanide-free copper plating base solution. The cyanide-free copper plating base solution comprises the following components in parts by weight: 50-60 g/L of basic copper carbonate, 20-40 g/L of potassium sodium tartrate, 250-300 g/L of citric acid and 10-15 g/L of sodium carbonate. The iron piece to be plated is hung in the prepared plating solution, the plating time is 30min, the current density is 1A/dm2, and the temperature is 55 ℃. Meanwhile, in cyanide-free copper plating solution and cyanide copper plating solution without added refiner, iron parts with the same model are electroplated under the same electroplating condition. The roughness of iron pieces made in the three baths was compared.
The detection results are compared to show that: roughness of copper plating layer of iron piece: additive for cyanide-free copper plating = cyanide copper plating < cyanide-free copper plating.
From the detection results of the embodiments 1 to 3, the cyanide-free copper plating grain refiner of the present invention has a significant effect on improving the fineness of the copper plating layer, and solves a problem in cyanide-free copper plating.
The foregoing are merely examples of the present invention and common general knowledge of known specific structures and/or features of the schemes has not been described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (3)
1. A cyanide-free alkaline copper plating refiner is characterized in that: comprises the following components in concentration ratio: 0.1-1g/L of p-methoxy benzyl chloride and 1-10g/L of 7-chloroquinaldine, and the solvent is water.
2. The cyanide-free alkaline copper plating refiner according to claim 1, characterized in that: the solvent is distilled water.
3. A preparation method of a cyanide-free alkaline copper plating refiner is characterized by comprising the following steps: the method comprises the following steps: weighing the following components in concentration ratio: 0.1-1g/L of p-methoxy benzyl chloride and 1-10g/L of 7-chloroquinaldine, adding a small amount of distilled water, continuously stirring until the p-methoxy benzyl chloride and the 7-chloroquinaldine are completely dissolved, and fixing the volume by using the distilled water and uniformly mixing after clarifying.
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| US4225407A (en) * | 1979-04-04 | 1980-09-30 | The Dow Chemical Company | Cathodic electrodeposition of polymers onto a conductive surface |
| SU1024530A1 (en) * | 1982-01-18 | 1983-06-23 | Калининградский государственный университет | Aqueous electrolyte for bright copper plating |
| JP3871018B2 (en) * | 2000-06-23 | 2007-01-24 | 上村工業株式会社 | Tin-copper alloy electroplating bath and plating method using the same |
| RU2210638C2 (en) * | 2001-08-17 | 2003-08-20 | Калининградский государственный университет | Electrolyte for bright nickel-plating |
| TW201343638A (en) * | 2012-01-20 | 2013-11-01 | 參天製藥股份有限公司 | Industrial manufacturing method of 1,2-dihydro-quinoline derivative or a salt thereof and manufacturing intermediate thereof |
| CN102995077B (en) * | 2012-12-28 | 2014-12-31 | 武汉吉和昌化工科技有限公司 | Cyanide-free alkaline bright copper plating solution and preparation method and electroplating process thereof |
| CN104356000B (en) * | 2014-11-18 | 2016-09-28 | 响水恒利达科技化工有限公司 | A kind of preparation method of 3-nitro-4-methoxybenzoic acid |
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