CN111206270A - Trivalent chromium electroplating solution and preparation method thereof - Google Patents
Trivalent chromium electroplating solution and preparation method thereof Download PDFInfo
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- 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
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
- C25D3/06—Electroplating: Baths therefor from solutions of chromium from solutions of trivalent chromium
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- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/04—Electroplating: Baths therefor from solutions of chromium
- C25D3/10—Electroplating: Baths therefor from solutions of chromium characterised by the organic bath constituents used
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Abstract
The invention provides a trivalent chromium electroplating solution and a preparation method thereof, wherein each liter of the trivalent chromium electroplating solution comprises the following components: 20-50 g/L of main salt, 130-200 g/L of conductive salt, 40-60 g/L of buffering agent, 25-50 g/L of complexing agent, 0.05-0.2 g/L of stabilizing agent, 0.05-0.2 g/L of impurity removing agent and 0.01-0.03 g/L of wetting agent; the impurity removing agent is prepared from 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 3-cinnamoyl tropolone according to a mass ratio of 0.5-1: 1, preparing a composition; the stabilizer is prepared from sodium bisulfate and glucosamine according to a mass ratio of 0.8-1.2: 1. The trivalent chromium electroplating solution has good stability, and the thickness of a plating layer prepared on a brass workpiece can reach 67 mu m.
Description
Technical Field
The invention relates to the technical field of electroplating, in particular to a trivalent chromium electroplating solution and a preparation method thereof.
Background
Currently, chromium plating occupies a significant market share in the electroplating industry. The chromium coating not only has the performance characteristics of high hardness, strong wear resistance and the like, but also has certain decorative performance, can be used as a coating with both functionality and decoration, and is widely applied to the industries of machine manufacturing, household kitchen industry, hardware industry and the like.
The chromium plating process can be classified into hexavalent chromium plating and trivalent chromium plating. The trivalent chromium electroplating solution has lower toxicity which is only one percent of hexavalent chromium electroplating solution, and the safety problem of the chromium plating process is improved. Wherein, trivalent chromium electroplating solution system can be divided into chloride system and sulfate system. Under the condition of high current density, a large amount of chlorine gas is generated and separated out, the separated chlorine gas can cause great pollution to the environment, and chloride ions in a chloride system are easy to corrode electroplating equipment, so that the service life of the electroplating equipment is influenced. The sulfate system does not produce toxic gas polluting the environment and is more environment-friendly. However, the conventional sulfate system has problems such as instability of the plating solution and thin plating.
Disclosure of Invention
The invention provides a trivalent chromium electroplating solution which is good in stability, and the thickness of a prepared plating layer meets the requirement of hard chromium plating.
The invention also provides a preparation method of the trivalent chromium electroplating solution.
In order to solve the problems, the invention discloses a trivalent chromium electroplating solution, wherein each liter of the trivalent chromium electroplating solution comprises the following components:
the impurity removing agent is prepared from 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 3-cinnamoyl tropolone according to a mass ratio of 0.5-1: 1, preparing a composition; the stabilizer is prepared from sodium bisulfate and glucosamine according to a mass ratio of 0.8-1.2: 1.
The invention adopts the sodium bisulfate and the glucosamine with the mass ratio as the stabilizing agents of the trivalent chromium electroplating solution; the sodium bisulfate and the glucosamine have reducibility and water solubility, and can effectively inhibit the generation of hexavalent chromium ions in the electroplating solution and improve the stability of the electroplating solution under the synergistic effect of the sodium bisulfate and the glucosamine, and the impurity removing agent 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 3-cinnamoyltropolone can play a good role in complexing impurity metal ions in the electroplating solution under the mass ratio, thereby effectively avoiding the damage of the impurity metal ions to the electroplating solution, reducing the sensitivity of the electroplating solution to the impurity metal ions and improving the stability of electroplating.
In addition, the sodium bisulfate, the 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and the 3-cinnamoyl tropolone are acidic, and the pH value of the trivalent chromium electroplating solution can be adjusted in the electroplating process, so that the pH value in the electroplating solution is kept in a set acidic range, and the electroplating stability is further improved.
Preferably, the impurity removing agent is prepared from 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 3-cinnamoyl tropolone according to a mass ratio of 0.78: 1.
Preferably, the stabilizer is prepared from sodium bisulfate and glucosamine in a mass ratio of 1:1.
Preferably, the main salt is one or more of chromium sulfate hexahydrate and basic chromium sulfate. Wherein the main salt is capable of continuously and effectively replenishing chromium ions consumed by the plating solution.
Preferably, the conductive salt is one or more of sodium sulfate, ammonium sulfate and aluminum potassium sulfate. The aluminum potassium sulfate can ensure the conductivity of the electroplating solution in the electroplating solution, and the brightness of the coating can be improved by the generated aluminum ions.
Preferably, the buffer is one or more of boric acid, glycine, sodium citrate, and aluminum sulfate.
Further preferably, the buffering agent is prepared from aluminum sulfate and boric acid in a mass ratio of 0.05-0.2: 1.
Preferably, the complexing agent is one or more of formic acid, acetic acid, oxalic acid, malic acid, tartaric acid, citric acid and glycolic acid. The complexing agent is preferably one or more of formic acid, oxalic acid, citric acid and glycolic acid.
Preferably, the wetting agent is an alkyl sulfate or alkyl sulfonate. The wetting agent is preferably sodium dodecyl sulfate or sodium dodecyl benzene sulfonate.
The invention also discloses a preparation method of the trivalent chromium electroplating solution, which comprises the following steps:
s1, soaking the tank body in a sulfuric acid solution with the volume ratio of 1%, and then injecting water into the tank body and heating to 60 ℃;
s2, adding main salt and a complexing agent into the tank body, stirring and preserving heat for 1-2 hours, then sequentially adding a buffering agent, a conductive agent and a stabilizing agent into the tank body, and uniformly stirring;
s3, adding the wetting agent and the brightening agent into the tank, and adding water while stirring to obtain a uniform mixed solution;
s4, adjusting the pH value of the mixed solution obtained in the step S3 to 2.5-4.0, and obtaining the trivalent chromium electroplating solution.
Compared with the prior art, the embodiment of the invention has the following advantages:
the invention adopts the following components in a mass ratio of 0.8-1.2: 1, sodium bisulfate and glucosamine which are used as stabilizers have synergistic effect, so that the generation of hexavalent chromium ions in the electroplating solution can be effectively inhibited, and the stability of the electroplating solution is improved; the invention also adopts the following components in a mass ratio of 0.5-1: the 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and the 3-cinnamoyl tropolone of 1 are used as impurity removing agents, and the synergistic effect of the impurity removing agents and the 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate can play a good complexing role in impurity metal ions of an electroplating solution, so that the damage of the impurity metal ions to the electroplating solution is effectively avoided, the sensitivity of the electroplating solution to the impurity metal ions is reduced, the electroplating stability is improved, and the thickness of a coating of the prepared coating on a brass workpiece can reach 67 mu m.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the above objects, features and advantages more apparent and understandable.
Example 1
The trivalent chromium electroplating solution of the present embodiment comprises: the main salt is 30g/L chromium sulfate hexahydrate and 10g/L basic chromium sulfate; the conductive salt is 120g/L sodium sulfate and 30g/L ammonium sulfate; the buffering agent is 5g/L of aluminum sulfate and 45g/L of boric acid; the complexing agent is 30g/L formic acid and 10g/L glycolic acid; the stabilizer is 0.05g/L sodium bisulfate and 0.05g/L glucosamine; the impurity removing agent is 0.044 g/L3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 0.056 g/L3-cinnamoyl tropolone; the wetting agent is 0.02g/L sodium dodecyl benzene sulfonate.
The preparation method of the trivalent chromium electroplating solution in the embodiment comprises the following steps:
s1, soaking the tank body in a sulfuric acid solution with the volume ratio of 1%, and then injecting water into the tank body and heating to 60 ℃;
s2, adding main salt and a complexing agent into the tank body, stirring and preserving heat for 1-2 hours, then sequentially adding a buffering agent, a conductive agent and a stabilizing agent into the tank body, and uniformly stirring;
s3, adding the wetting agent and the brightening agent into the tank, and adding water while stirring to obtain a uniform mixed solution;
s4, adjusting the pH value of the mixed solution in the step S3 to 2.5, and obtaining the trivalent chromium electroplating solution.
Example 2
The trivalent chromium electroplating solution of the present embodiment comprises: the main salt is 30g/L chromium sulfate hexahydrate and 20g/L basic chromium sulfate; the conductive salt is 100g/L sodium sulfate, 50g/L ammonium sulfate and 50g/L potassium aluminum sulfate; the buffering agent is 10g/L of aluminum sulfate and 50g/L of boric acid; the complexing agent is 25g/L formic acid and 20g/L citric acid; the stabilizer is 0.03g/L sodium bisulfate and 0.03g/L glucosamine; the impurity removing agent is 0.025 g/L3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 0.025 g/L3-cinnamoyl tropolone; the wetting agent is 0.03g/L sodium dodecyl benzene sulfonate.
The trivalent chromium plating solution of this example was prepared in substantially the same manner as in example 1, except that the pH of the mixed solution described in S3 was 2.5.
Example 3
The trivalent chromium electroplating solution of the present embodiment comprises: the main salt is 15g/L chromium sulfate hexahydrate and 20g/L basic chromium sulfate; the conductive salt is 180g/L sodium sulfate; the buffer is 15g/L aminoacetic acid and 35g/L boric acid; the complexing agent is 30g/L formic acid and 20g/L citric acid; the stabilizer is 0.071g/L sodium bisulfate and 0.089g/L glucosamine; the impurity removing agent is 0.08 g/L3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 0.08 g/L3-cinnamoyl tropolone; the wetting agent is 0.02g/L sodium dodecyl benzene sulfonate.
The trivalent chromium plating solution of this example was prepared in substantially the same manner as in example 1, except that the pH of the mixed solution described in S3 was 3.0.
Example 4
The trivalent chromium electroplating solution of the present embodiment comprises: the main salt is 20g/L chromium sulfate hexahydrate; the conductive salt is 180g/L sodium sulfate; the buffering agent is 130g/L aluminum potassium sulfate; the complexing agent is 15g/L oxalic acid and 10g/L glycolic acid; the stabilizer is 0.11g/L sodium bisulfate and 0.09g/L glucosamine; the impurity removing agent is 0.067 g/L3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 0.133 g/L3-cinnamoyl trolene; the wetting agent is 0.01g/L dialkyl sodium sulfate.
The trivalent chromium plating solution of this example was prepared in substantially the same manner as in example 1, except that the pH of the mixed solution of S3 was 4.0.
Comparative example 1
The trivalent chromium plating solution, the preparation method and the plating conditions of the present comparative example were substantially the same as those of example 1 except that no stabilizer was added to the trivalent chromium plating solution.
Comparative example 2
The trivalent chromium electroplating solution, the preparation method and the electroplating conditions of the comparative example are basically the same as those of the example 1, and the difference is that the mass ratio of the stabilizer sodium bisulfate to the glucosamine added into the trivalent chromium electroplating solution is 0.2:1, namely the stabilizer is the sodium bisulfate with the mass ratio of 0.017g/L and the glucosamine with the mass ratio of 0.083 g/L.
Comparative example 3
The trivalent chromium electroplating solution, the preparation method and the electroplating conditions of the comparative example are basically the same as those of the example 1, and the difference is that the mass ratio of sodium bisulfate and glucosamine, which are stabilizing agents, added into the trivalent chromium electroplating solution is 2:1, namely the stabilizing agents are 0.067g/L of sodium bisulfate and 0.033g/L of glucosamine.
Comparative example 4
The trivalent chromium plating solution, the preparation method and the plating conditions of the comparative example are substantially the same as those of example 1, except that no impurity removal agent is added to the trivalent chromium plating solution.
Comparative example 5
The trivalent chromium electroplating solution, the preparation method and the electroplating conditions of the comparative example are basically the same as those in example 1, and the difference is that the impurity removing agent added into the trivalent chromium electroplating solution is only 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate, and 3-cinnamoyl tropolone is not included.
And (3) performance testing:
the trivalent chromium plating solutions of examples 1 to 4 and comparative examples 1 to 5 were subjected to the plating solution stability, anode performance and plating thickness tests, respectively, in the following specific procedures:
1. stability test of plating solution
Taking 1000mL of trivalent chromium electroplating solution to carry out rack plating test, wherein the cathode current density is 15A/dm2The on-off period of the control current is as follows: electrifying for 5min, powering off for 15s, replacing the test piece every 1h, supplementing and maintaining according to the working ampere hours according to the process requirements, observing the stability of the trivalent chromium electroplating solution in the rack plating process, and observing the plating layer of the test piece by 1500 times under a microscope.
2. Anodic testing
Investigating Cr in electroplating solution by Hull cell test6+The specific method is as follows: in the absence of Cr6+Continuously performing 5 Hull cell tests (5A, 10min) in the trivalent chromium electroplating solution, and detecting whether Cr exists in the trivalent chromium electroplating solution by adopting a diphenylcarbohydrazide spectrophotometry6+And (4) generating.
3. Coating thickness test
Electroplating conditions are as follows: titanium-based iridium dioxide is taken as an anode, 65 # manganese steel is taken as a cathode, the electroplating temperature is 30 ℃, and the cathode current density is 15A/dm2The electroplating time was 60 minutes, and the area ratio of the cathode to the anode was 1: 1.5. After the electroplating is completed, the thickness of the coating is tested by an XRF instrument.
The results of the performance tests of the trivalent chromium plating solutions of examples 1 to 4 and comparative examples 1 to 2 are shown in table 1:
TABLE 1
Note: plating stability is determined by the stability of the plating solution and the Cr content of the plating solution6+The conditions are jointly reacted, wherein the electroplating solution is clear, the coating thickness is uniform, the coating is smooth, and no Cr exists in the electroplating solution6+Then, the electroplating stability is good; otherwise, the plating stability is poor.
As can be seen from Table 1, the trivalent chromium plating solutions of examples 1-4 are relatively stable, the thickness of the plated layer on the test piece is uniform, and no Cr is found in the trivalent chromium plating solutions of examples 1-36+However, the trivalent chromium plating solutions of comparative examples 1 to 5 were significantly cloudy after a certain period of time of plating and the test pieces were not uniformly plated, and as a whole, the plating stability of the trivalent chromium plating solutions of examples 1 to 4 was superior to that of the trivalent chromium plating solutions of comparative examples 1 to 5, and the plating thicknesses obtained in examples 1 to 4 were also significantly greater than those obtained in comparative examples 1 to 5. Among them, the trivalent chromium plating solution of example 1 is the best in plating stability, and the thickness of the obtained plating layer reaches 67 μm.
It is noted that, for simplicity of explanation, the method embodiments are described as a series of acts or combination of acts, but those skilled in the art will appreciate that the present invention is not limited by the order of acts, as some steps may occur in other orders or concurrently in accordance with the embodiments of the invention. Further, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred and that no particular act is required to implement the invention.
The embodiments in the present specification are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
While preferred embodiments of the present invention have been described, additional variations and modifications of these embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the true scope of the embodiments of the invention.
Finally, it should be further noted that, in the present document, the term "comprises/comprising" is intended to cover a non-exclusive inclusion, such that a process, a method including a series of elements, not only those elements, but also other elements not explicitly listed, or inherent to such a process, method, is included. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in the processes or methods for which the element is included.
The technical solutions provided by the present invention are described in detail above, and the principle and the implementation of the present invention are explained in this document by applying specific examples, and the descriptions of the above examples are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. A trivalent chromium electroplating solution, characterized in that the composition of each liter of said trivalent chromium electroplating solution is:
the impurity removing agent is prepared from 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 3-cinnamoyl tropolone according to a mass ratio of 0.5-1: 1, preparing a composition; the stabilizer is prepared from sodium bisulfate and glucosamine according to a mass ratio of 0.8-1.2: 1.
2. The trivalent chromium electroplating solution according to claim 1, wherein the impurity removal agent is prepared from 3-amino-2-hydroxy-5-nitrobenzenesulfonic acid hydrate and 3-cinnamoyl tropolone according to a mass ratio of 0.78: 1.
3. The trivalent chromium electroplating solution according to claim 1, wherein the stabilizer is a mixture of sodium bisulfate and glucosamine in a mass ratio of 1:1.
4. The trivalent chromium electroplating solution according to claim 1, wherein the primary salt is one or more of chromium sulfate hexahydrate and basic chromium sulfate.
5. The trivalent chromium electroplating solution according to claim 1, wherein the conductive salt is one or more of sodium sulfate, ammonium sulfate, and potassium aluminum sulfate.
6. The trivalent chromium electroplating solution according to claim 1, wherein the buffer is one or more of boric acid, glycine, sodium citrate, aluminum sulfate.
7. The trivalent chromium electroplating solution according to claim 6, wherein the buffer is prepared from aluminum sulfate and boric acid at a mass ratio of 0.05-0.2: 1.
8. The trivalent chromium electroplating solution according to claim 1, wherein the complexing agent is one or more of formic acid, acetic acid, oxalic acid, malic acid, tartaric acid, citric acid, glycolic acid.
9. The trivalent chromium electroplating solution according to claim 1, wherein the wetting agent is an alkyl sulfate or an alkyl sulfonate.
10. A method for preparing a trivalent chromium electroplating solution according to any one of claims 1 to 9, characterized by comprising the steps of:
s1, soaking the tank body in a sulfuric acid solution with the volume ratio of 1%, and then injecting water into the tank body and heating to 60 ℃;
s2, adding main salt and a complexing agent into the tank body, stirring and preserving heat for 1-2 hours, then sequentially adding a buffering agent, a conductive agent and a stabilizing agent into the tank body, and uniformly stirring;
s3, adding the wetting agent and the brightening agent into a tank, and adding water while stirring to obtain a uniform mixed solution;
s4, adjusting the pH value of the mixed solution obtained in the step S3 to 2.5-4.0, and obtaining the trivalent chromium electroplating solution.
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