CN110923683A - Self-repairing normal-temperature blackening agent for cold-drawn steel pipe and preparation method and application thereof - Google Patents
Self-repairing normal-temperature blackening agent for cold-drawn steel pipe and preparation method and application thereof Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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Abstract
A self-repairing normal temperature blackening agent for cold-drawn steel tubes and a preparation method and application thereof relate to the technical field of metal surface treatment, wherein main film forming materials of the self-repairing normal temperature blackening agent for cold-drawn steel tubes comprise copper sulfate pentahydrate, ammonium tungstate and sodium lignosulfonate doped polyaniline reaction liquid. The blackening agent can simultaneously realize blackening and rust prevention, the blackening film has a self-repairing function, the corrosion resistance of the blackening film formed by the blackening agent is improved by more than ten times compared with the blackening film formed by the traditional normal-temperature blackening agent, and the blackening agent has a very wide market application prospect.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a self-repairing normal temperature blackening agent for a cold-drawn steel pipe, and a preparation method and application thereof.
Background
The blackening treatment of the cold-drawn steel tube is a surface treatment technology and is used for improving the corrosion resistance of the steel tube, and a blackening agent is a chemical agent for realizing the blackening treatment of steel.
Currently, the common blackening methods are: alkaline chemical oxidation and acidic chemical oxidation (ambient blackening). The alkaline chemical oxidation method is to treat the raw materials at a high temperature of 135-150 ℃ for 30-90 min, and the film layer is fine, uniform, bright and black, high in fastness and good in corrosion resistance; but has the problems of long production period, large energy consumption, poor labor condition and serious environmental pollution. The normal temperature blackening of the steel surface is to form a black oxide film without changing the dimensional accuracy of the processed piece. However, most of the blackening agents contain polluting substances such as phosphorus, selenium and nitrite, and the like, or have complicated processes and high cost, and after the iron casting is blackened, the iron casting needs to be immersed in another solvent for rust prevention treatment in order to prevent the surface of the iron casting from rusting, so that the blackening and rust prevention functions cannot be achieved at the same time, and the operation complexity is increased. How to improve the comprehensive performance, especially the antirust performance, of the blackening film and how to solve the problem of severe corrosion at the scratch in the transportation process of the cold-rolled steel pipe become new problems, however, the results of the self-repairing normal-temperature blackening agent are not reported at present.
Disclosure of Invention
One of the objects of the present invention is to provide a room temperature blackening agent which can simultaneously achieve blackening and rust prevention and has a self-repairing function of a blackening film.
In order to solve the technical problems, the invention adopts the following technical scheme: the self-repairing normal temperature blackening agent for cold drawn steel pipe has main filming matter comprising copper sulfate pentahydrate, ammonium tungstate and sodium lignosulfonate doped polyaniline reaction liquid.
Specifically, the self-repairing normal temperature blackening agent for the cold-drawn steel pipe comprises the following components: 10-200 parts of copper sulfate pentahydrate, 20-300 parts of ammonium tungstate, 50-1000 parts of sodium lignosulfonate-doped polyaniline reaction liquid, 5-100 parts of nickel sulfate, 10-150 parts of ammonium thiosulfate, 5-100 parts of trisodium nitrilotriacetate and a proper amount of deionized water.
Preferably, the copper sulfate pentahydrate is 40-100 parts by weight, the ammonium tungstate is 50-150 parts by weight, the sodium lignosulfonate-doped polyaniline reaction liquid is 200-600 parts by weight, the nickel sulfate is 10-50 parts by weight, the ammonium thiosulfate is 40-100 parts by weight, and the trisodium nitrilotriacetate is 20-80 parts by weight.
Preferably, the copper sulfate pentahydrate is 80 parts by weight, the ammonium tungstate is 100 parts by weight, the sodium lignosulfonate-doped polyaniline reaction liquid is 400 parts by weight, the nickel sulfate is 20 parts by weight, the ammonium thiosulfate is 60 parts by weight, and the trisodium nitrilotriacetate is 40 parts by weight.
More preferably, the weight ratio of copper sulfate pentahydrate to ammonium tungstate is 4: 5.
The sodium lignosulfonate-doped polyaniline reaction solution can be synthesized by an emulsion polymerization method, and the components used in the synthesis process comprise sodium lignosulfonate and aniline, wherein the weight ratio of the sodium lignosulfonate to the aniline is 1: 1.
Specifically, the sodium lignosulfonate-doped polyaniline reaction solution is synthesized by the following method:
firstly, weighing 13-24 parts by weight of sodium lignosulphonate, pouring the sodium lignosulphonate into 70-130 parts by weight of (0.8-1.2) mol/L sulfuric acid solution, fully stirring and uniformly mixing, then taking 13-24 parts by weight of aniline, slowly adding the aniline into the mixed solution under the stirring effect, fully stirring and uniformly mixing to prepare solution D;
weighing 32-59 parts by weight of ammonium persulfate, dissolving in 70-130 parts by weight of (0.8-1.2) mol/L citric acid solution to obtain ammonium persulfate-citric acid solution, dropwise adding the ammonium persulfate-citric acid solution into the solution D, and fully and uniformly stirring the reaction system at the temperature of 0-5 ℃;
and thirdly, allowing the reaction to be further completed at room temperature to obtain a target reaction solution.
Preferably, in the step one, the sodium lignosulfonate is used in an amount of 18.6 parts by weight, the sulfuric acid solution has a concentration of 1mol/L and is used in an amount of 100 parts by weight, and the aniline is used in an amount of 18.6 parts by weight; in the second step, the using amount of the ammonium persulfate is 45.6 parts by weight, the concentration of the citric acid solution is 1mol/L, and the using amount of the citric acid solution is 100 parts by weight.
As another aspect of the present invention, a method for preparing the above self-repairing type room temperature blackening agent for cold-drawn steel pipes, comprising the steps of:
firstly, adding copper sulfate pentahydrate, ammonium thiosulfate, ammonium tungstate and nickel sulfate into a proper amount of deionized water to prepare solution A;
adding trisodium nitrilotriacetic acid into a proper amount of deionized water, uniformly stirring, and then slowly dropwise adding sodium lignosulfonate-doped polyaniline reaction liquid to prepare liquid B;
and thirdly, mixing the solution B with the solution A, stirring uniformly, and standing to prepare the self-repairing normal-temperature blackening agent for the cold-drawn steel pipe.
As another aspect of the present invention, the self-repairing type room temperature blackening agent for cold drawn steel pipe described above is used in the surface rust preventive treatment of cold drawn seamless steel pipe.
The self-repairing normal temperature blackening agent for the cold-drawn steel pipe has the environmental protection characteristic of no selenium and no phosphorus, and because the blackening film is rich in sodium lignosulfonate doped polyaniline material, the dispersion stability, the conductivity and the corrosion resistance of the polyaniline are all superior to those of the conventional polyaniline, the sodium lignosulfonate doped polyaniline cuts off the direct connection between metal and oxygen through the reversible oxidation-reduction reaction with the oxygen, a compact metal oxide layer is formed at the interface of the metal and the film, so that the electrode potential of the metal can be effectively positioned in a passivation area, when the blackened film has scratches, the sodium lignosulfonate doped polyaniline can passivate the exposed metal at the scratches again through oxidation-reduction reaction, has extremely strong self-repairing function, compared with the traditional blackening agent, the anti-corrosion performance of the black coating is obviously improved, and the black coating has the characteristics of low production cost, simple process, high blackening speed, uniform and fine blackening film and strong adhesive force.
Detailed Description
The invention is different from the prior art in that the blackening film is mainly formed by taking copper sulfate pentahydrate, ammonium tungstate and sodium lignosulfonate doped polyaniline reaction liquid as main film forming materials, the formed blackening film is rich in sodium lignosulfonate doped polyaniline materials, the dispersion stability, the conductivity and the corrosion resistance of the black-emitting agent are all superior to those of polyaniline in the traditional black-emitting agent, particularly, sodium lignosulfonate doped polyaniline can cut off the direct connection between metal and oxygen through the reversible oxidation-reduction reaction with oxygen, a compact metal oxide layer is formed at the interface of the metal and the film, so that the electrode potential of the metal can be effectively positioned in a passivation area, when the blackening film has scratches, the sodium lignosulfonate doped polyaniline can passivate the exposed metal at the scratches again through oxidation-reduction reaction, has a strong self-repairing function, and the anti-corrosion performance of the blackening agent is obviously improved compared with that of the traditional blackening agent.
In order to make the improvement of the present invention over the prior art more clear to those skilled in the art, the following will further describe the self-repairing room temperature blackening agent of the present invention with reference to the following examples.
Example 1:
| component name | Parts by weight |
| Blue vitriod | 10 |
| Ammonium tungstate | 300 |
| Sodium lignosulfonate-doped polyaniline reaction liquid | 700 |
| Nickel sulfate | 50 |
| Ammonium thiosulfate | 80 |
| Nitrilotriacetic acid trisodium salt | 40 |
The sodium lignosulfonate-doped polyaniline reaction solution can be synthesized by the following method:
firstly, weighing 13-24 parts by weight (for example, 18.6 parts by weight) of sodium lignosulfonate, pouring the sodium lignosulfonate into 70-130 parts by weight (for example, 100 parts by weight) of (0.8-1.2) mol/L sulfuric acid solution (the concentration of the sulfuric acid solution is preferably 1mol/L), fully stirring and uniformly mixing, then taking 13-24 parts by weight (for example, 18.6 parts by weight) of aniline, slowly adding the aniline into the mixed solution under the action of stirring, fully stirring and uniformly mixing to prepare solution D.
Weighing 32-59 parts by weight (for example, 45.6 parts by weight) of ammonium persulfate, dissolving in 70-130 parts by weight (for example, 100 parts by weight) of (0.8-1.2) mol/L citric acid solution (the concentration of the citric acid solution is preferably 1mol/L) to obtain ammonium persulfate-citric acid solution, dropwise adding the ammonium persulfate-citric acid solution into the solution D, and fully and uniformly stirring the reaction system at the temperature of 0-5 ℃;
and thirdly, allowing the reaction to be further completed at room temperature to obtain a target reaction solution.
It should be noted that the sodium lignosulfonate-doped polyaniline reaction solution is a key raw material for improving the antirust performance of the metal blackening film, and because the environment of the synthetic sodium lignosulfonate-doped polyaniline reaction solution is acidic, an acid does not need to be additionally added into the formula of the blackening agent. The sodium lignosulfonate used in the synthesis reaction is a natural high molecular polymer and an anionic surfactant, can reduce the surface tension of a solution, has strong dispersing capacity, and can stably disperse polyaniline in an aqueous medium. It should be emphasized that, when the weight ratio of the sodium lignosulfonate to the aniline is 1:1, the dispersion stability of the synthesized sodium lignosulfonate doped polyaniline reaction and the corrosion resistance of the blackening film obtained after the sodium lignosulfonate doped polyaniline is used in the blackening agent are obviously better than other proportioning ratios (the performance improvement range can reach 20% -25%). In examples 1 to 8, the sodium lignosulfonate-doped polyaniline reaction solution synthesized by the above method was used, and the weight ratio of sodium lignosulfonate to aniline used in the synthesis process was 1: 1.
Example 2:
compared with the example 1, the example 2 only changes the mixture ratio of the components, and the mixture ratio of the components in the example 2 is as follows:
example 3:
compared with the examples 1 and 2, the example 3 only changes the mass percentage of each component, and the mixture ratio of each component in the example 3 is as follows:
| component name | Parts by weight |
| Blue vitriod | 100 |
| Ammonium tungstate | 200 |
| Sodium lignosulfonate-doped polyaniline reaction liquid | 50 |
| Nickel sulfate | 5 |
| Ammonium thiosulfate | 10 |
| Nitrilotriacetic acid trisodium salt | 5 |
Example 4:
compared with the examples 1 to 3, the example 4 only changes the mass percentage of each component, and the mixture ratio of each component in the example 4 is as follows:
| component name | Parts by weight |
| Blue vitriod | 150 |
| Ammonium tungstate | 250 |
| Sodium lignosulfonate-doped polyaniline reaction liquid | 500 |
| Nickel sulfate | 50 |
| Ammonium thiosulfate | 150 |
| Nitrilotriacetic acid trisodium salt | 50 |
Example 5:
compared with the above examples, the example 5 only changes the mass percentage of each component, and the ratio of each component in the example 5 is as follows:
| component name | Parts by weight |
| Blue vitriod | 40 |
| Ammonium tungstate | 50 |
| Sodium lignosulfonate-doped polyaniline reaction liquid | 200 |
| Nickel sulfate | 10 |
| Ammonium thiosulfate | 40 |
| Nitrilotriacetic acid trisodium salt | 20 |
Example 6:
compared with the above examples, the example 6 only changes the mass percentage of each component, and the ratio of each component in the example 6 is as follows:
| component name | Parts by weight |
| Blue vitriod | 100 |
| Ammonium tungstate | 150 |
| Sodium lignosulfonate-doped polyaniline reaction liquid | 600 |
| Nickel sulfate | 50 |
| Ammonium thiosulfate | 100 |
| Nitrilotriacetic acid trisodium salt | 80 |
Example 7:
compared with the above examples, the example 7 only changes the mass percentage of each component, and the ratio of each component in the example 7 is as follows:
| component name | Parts by weight |
| Blue vitriod | 70 |
| Ammonium tungstate | 100 |
| Sodium lignosulfonate-doped polyaniline reaction liquid | 400 |
| Nickel sulfate | 30 |
| Ammonium thiosulfate | 70 |
| Nitrilotriacetic acid trisodium salt | 50 |
Example 8:
compared with the above examples, the example 8 only changes the mass percentage of each component, and the ratio of each component in the example 8 is as follows:
| component name | Parts by weight |
| Blue vitriod | 80 |
| Ammonium tungstate | 100 |
| Sodium lignosulfonate-doped polyaniline reaction liquid | 400 |
| Nickel sulfate | 20 |
| Ammonium thiosulfate | 60 |
| Nitrilotriacetic acid trisodium salt | 40 |
The preparation method of the self-repairing normal temperature blackening agent in the above embodiments 1-8 comprises the following steps: firstly, adding blue vitriol, ammonium thiosulfate, ammonium tungstate and nickel sulfate into a proper amount of deionized water to prepare solution A. And secondly, adding trisodium nitrilotriacetic acid into a proper amount of deionized water, uniformly stirring, and then slowly dropwise adding sodium lignosulfonate-doped polyaniline reaction liquid to prepare liquid B. And thirdly, mixing the solution B with the solution A, stirring uniformly, and standing to prepare the self-repairing normal-temperature blackening agent for the cold-drawn steel pipe. The self-repairing type normal temperature blackening agent prepared is a dark green uniform solution, and the optimal storage temperature of the self-repairing type normal temperature blackening agent is 20-35 ℃.
In the components for preparing the self-repairing normal temperature blackening agent, copper sulfate pentahydrate, ammonium tungstate and sodium lignosulfonate doped polyaniline reaction liquid are used as main film forming materials, nickel sulfate is used as a secondary film forming material, ammonium thiosulfate is used as a film forming auxiliary agent, and trisodium nitrilotriacetate is used as a chelating agent, wherein the sodium lignosulfonate doped polyaniline reaction liquid also plays a role of a dispersion stabilizer. It should be noted that, in the process of preparing the self-repairing normal temperature blackening agent, the applicant finds that the ratio of the copper sulfate pentahydrate to the ammonium tungstate has a relatively obvious influence on the film forming effect of the blackening agent and the film adhesion, and when the ratio of the copper sulfate pentahydrate to the ammonium tungstate is 4:5, the film forming effect of the blackening film is very good, and the adhesion and the corrosion resistance of the film are also obviously improved.
After the common carbon steel subjected to degreasing and water washing treatment is placed in a self-repairing normal-temperature blackening agent for treatment, the performance of the blackening film is detected according to the following standard. The test items for the black coating layer include: 1. the appearance of the film was as follows, QB/T2505-2000 "technical conditions for blackening sewing machine parts". 2. The abrasion resistance of the film layer is tested by friction test with reference to QB/T3820-1999 abrasion resistance test method of metal coating and chemical treatment layer of light industry products, and the number of times of friction when the substrate is exposed is recorded. 3. The membrane layer was observed for its denseness by dropping 3% copper sulfate on the membrane layer and recording the surface change (in seconds) according to QB/T3824-1999 test method for ferrous metal chemical protective layer of light industry. 4. And (3) testing the corrosion resistance of the film, and recording the duration time without the corrosion spots by soaking the film in a 3% sodium chloride solution according to QB/T2505-2000 technical conditions for blackening sewing machine parts. The test results are shown in the following table.
From the test results in the table above, it can be seen that the duration of the non-color change of the surface of the film layer formed by using 3% copper sulfate drops in all the examples reaches more than 70s, which indicates that the formed blackening film has high compactness (the detection qualification standard is more than 30s), the number of times of friction in all the examples is more than 150, which indicates that the formed blackening film has good binding force with the substrate, especially, the results obtained by soaking all the examples in 3% sodium chloride solution reach more than 70h, which shows excellent corrosion resistance (the test results of the blackening film formed by using a normal temperature blackening agent are mostly within several hours), and the index is improved by more than 10 times compared with the test results of the blackening film formed by using a normal temperature blackening agent, which is also closely related to the self-repairing performance of the blackening film formed by using the present invention.
The above embodiments are preferred implementations of the present invention, and the present invention can be implemented in other ways without departing from the spirit of the present invention. Some descriptions of the present invention have been simplified to facilitate understanding of the improvement of the present invention over the prior art by those of ordinary skill in the art, and some other elements have been omitted from this document for clarity, and those omitted elements should be recognized by those of ordinary skill in the art to constitute the content of the present invention.
Claims (10)
1. The self-repairing normal temperature blackening agent for cold drawn steel pipe features that its main filming material includes copper sulfate pentahydrate, ammonium tungstate and reaction liquid of sodium lignosulfonate doped with polyaniline.
2. The self-repairing type room temperature blackening agent for cold-drawn steel pipes according to claim 1, characterized by comprising the following components: 10-200 parts of copper sulfate pentahydrate, 20-300 parts of ammonium tungstate, 50-1000 parts of sodium lignosulfonate-doped polyaniline reaction liquid, 5-100 parts of nickel sulfate, 10-150 parts of ammonium thiosulfate, 5-100 parts of trisodium nitrilotriacetate and a proper amount of deionized water.
3. The self-repairing type room temperature blackening agent for cold-drawn steel pipes according to claim 2, characterized in that: 40-100 parts of copper sulfate pentahydrate, 50-150 parts of ammonium tungstate, 200-600 parts of sodium lignosulfonate-doped polyaniline reaction liquid, 10-50 parts of nickel sulfate, 40-100 parts of ammonium thiosulfate and 20-80 parts of trisodium nitrilotriacetate.
4. The self-repairing type room temperature blackening agent for cold-drawn steel pipes according to claim 3, characterized in that: the copper sulfate pentahydrate is 80 parts by weight, the ammonium tungstate is 100 parts by weight, the sodium lignosulfonate-doped polyaniline reaction liquid is 400 parts by weight, the nickel sulfate is 20 parts by weight, the ammonium thiosulfate is 60 parts by weight, and the trisodium nitrilotriacetate is 40 parts by weight.
5. The self-repairing type room temperature blackening agent for cold-drawn steel pipes according to any one of claims 1 to 4, characterized in that: the weight ratio of the copper sulfate pentahydrate to the ammonium tungstate is 4: 5.
6. The self-repairing type room temperature blackening agent for cold-drawn steel pipes according to any one of claims 1 to 4, characterized in that: the sodium lignosulfonate-doped polyaniline reaction liquid is synthesized by an emulsion polymerization method, and the components used in the synthesis process comprise sodium lignosulfonate and aniline, wherein the weight ratio of the sodium lignosulfonate to the aniline is 1: 1.
7. The self-repairing normal temperature blackening agent for the cold-drawn steel pipe according to any one of claims 1 to 4, wherein the sodium lignosulfonate-doped polyaniline reaction solution is synthesized by the following method:
firstly, weighing 13-24 parts by weight of sodium lignosulphonate, pouring the sodium lignosulphonate into 70-130 parts by weight of (0.8-1.2) mol/L sulfuric acid solution, fully stirring and uniformly mixing, then taking 13-24 parts by weight of aniline, slowly adding the aniline into the mixed solution under the stirring effect, fully stirring and uniformly mixing to prepare solution D.
Weighing 32-59 parts by weight of ammonium persulfate, dissolving in 70-130 parts by weight of (0.8-1.2) mol/L citric acid solution to obtain ammonium persulfate-citric acid solution, dropwise adding the ammonium persulfate-citric acid solution into the solution D, and fully and uniformly stirring the reaction system at the temperature of 0-5 ℃;
and thirdly, allowing the reaction to be further completed at room temperature to obtain a target reaction solution.
8. The self-repairing type room temperature blackening agent for cold-drawn steel pipes according to claim 7, wherein: in the first step, the dosage of the sodium lignosulfonate is 18.6 parts by weight, the concentration of the sulfuric acid solution is 1mol/L, the dosage of the sulfuric acid solution is 100 parts by weight, and the dosage of the aniline is 18.6 parts by weight; in the second step, the using amount of the ammonium persulfate is 45.6 parts by weight, the concentration of the citric acid solution is 1mol/L, and the using amount of the citric acid solution is 100 parts by weight.
9. The method for preparing the self-repairing type room temperature blackening agent for cold-drawn steel pipes according to any one of claims 1 to 8, characterized by comprising the steps of:
firstly, adding copper sulfate pentahydrate, ammonium thiosulfate, ammonium tungstate and nickel sulfate into a proper amount of deionized water to prepare solution A;
adding trisodium nitrilotriacetic acid into a proper amount of deionized water, uniformly stirring, and then slowly dropwise adding sodium lignosulfonate-doped polyaniline reaction liquid to prepare liquid B;
and thirdly, mixing the solution B with the solution A, stirring uniformly, and standing to prepare the self-repairing normal-temperature blackening agent for the cold-drawn steel pipe.
10. Use of the self-repairing type room temperature blackening agent for cold-drawn steel pipes according to any one of claims 1 to 8 for rust prevention treatment of the surface of cold-drawn seamless steel pipes.
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| CN115613019A (en) * | 2022-09-29 | 2023-01-17 | 南京科润工业介质股份有限公司 | Waste heat blackening liquid for workpiece suitable for full-automatic weighing and packaging machine subpackaging |
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| CN103046038A (en) * | 2012-12-06 | 2013-04-17 | 安徽未来表面技术有限公司 | Room temperature blackening agent suitable for iron casting and method for preparing room temperature blackening agent suitable for iron casting |
| CN105315829A (en) * | 2015-12-02 | 2016-02-10 | 马鞍山市三江机械有限公司 | Room-temperature rust removal blackening agent and preparation method thereof |
| CN108976870A (en) * | 2018-06-27 | 2018-12-11 | 福建师范大学 | A kind of aqueous dispersion polyaniline compound anticorrosive additive and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103046038A (en) * | 2012-12-06 | 2013-04-17 | 安徽未来表面技术有限公司 | Room temperature blackening agent suitable for iron casting and method for preparing room temperature blackening agent suitable for iron casting |
| CN105315829A (en) * | 2015-12-02 | 2016-02-10 | 马鞍山市三江机械有限公司 | Room-temperature rust removal blackening agent and preparation method thereof |
| CN108976870A (en) * | 2018-06-27 | 2018-12-11 | 福建师范大学 | A kind of aqueous dispersion polyaniline compound anticorrosive additive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115613019A (en) * | 2022-09-29 | 2023-01-17 | 南京科润工业介质股份有限公司 | Waste heat blackening liquid for workpiece suitable for full-automatic weighing and packaging machine subpackaging |
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