CN113930769A - Titanium alloy pickling polishing solution and preparation method and application thereof - Google Patents
Titanium alloy pickling polishing solution and preparation method and application thereof Download PDFInfo
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- CN113930769A CN113930769A CN202111230546.2A CN202111230546A CN113930769A CN 113930769 A CN113930769 A CN 113930769A CN 202111230546 A CN202111230546 A CN 202111230546A CN 113930769 A CN113930769 A CN 113930769A
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- C—CHEMISTRY; METALLURGY
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
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- C—CHEMISTRY; METALLURGY
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/106—Other heavy metals refractory metals
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Abstract
The invention discloses a titanium alloy pickling polishing solution and a preparation method and application thereof, and belongs to the technical field of titanium alloy pretreatment. The preparation method of the titanium alloy pickling polishing solution comprises the following steps: mixing sulfamic acid, ascorbic acid and lactic acid to obtain pickling base liquid, adding an additive, and stirring to obtain the titanium alloy pickling polishing liquid. The prepared titanium alloy pickling polishing solution can effectively improve the acid effect, obtains a clean and bright titanium alloy surface, provides a good foundation for subsequent treatment, can be operated at normal temperature in the whole pickling process, reduces the difficulty of waste liquid treatment in the pickling process, and relieves the harm of fluorine ions in the traditional titanium alloy pickling solution to the environment.
Description
Technical Field
The invention relates to a titanium alloy pickling polishing solution and a preparation method and application thereof, belonging to the technical field of titanium alloy pretreatment.
Background
Because titanium alloy has the advantages of excellent corrosion resistance, extremely high heat resistance, good specific strength and the like, the titanium alloy is widely applied to industries such as aviation industry, chemical industry and the like, but the surface of the titanium alloy is easy to damage in the processing and transportation process, and oxide skin, rust, oil stain, sand blasting residual trace and the like can be generated, so that the surface of the titanium alloy needs to be polished, and the roughness of the surface of a workpiece is reduced by mainly utilizing the mechanical, chemical or electrochemical action in the polishing process, so that the bright and flat surface of the titanium alloy can be obtained.
At present, the surface polishing chemical cleaning of the titanium alloy mainly adopts HF-HNO3The mixed acid pickling method mainly comprises the following pickling principles: dissolution, mechanical exfoliation and reduction. The dissolution is that the oxide layer on the surface of the metal and the components of the pickling solution react chemically to generate metal salt dissolved in water, thereby achieving the purpose of removing the oxide layer skin. The mechanical stripping function is that the acid washing solution enters the pores of the oxide layer to react with the metal simple substance or the matrix simple substance in the oxide layer to generate gas to form expansion pressure to promote the oxide layer to be stripped from the metal surface. The reduction is that a part of hydrogen atoms in the pickling solution has strong reducibility, and the oxide and the high-valence metal salt of the high-valence metal are reduced into low-valence metal oxide and low-valence metal salt which are easily dissolved in the acid solution. In the pickling process, attention is paid to the effect of cleaning the surface of the titanium alloy, the possibility that hydrogen embrittlement (hydrogen dissolved in steel and polymerized into hydrogen molecules to cause stress concentration and exceed the strength limit of the steel and fine cracks, also called white spots, are formed in the steel) occurs to the titanium alloy in the cleaning process, and the waste liquid after cleaning is treated. The titanium alloy has good affinity to hydrogen, hydrogen is easy to generate in the pickling process, when the hydrogen content is accumulated to a limit value, the impact toughness resistance and the tensile strength of the titanium alloy tend to be reduced, so that the titanium alloy is brittle, therefore, in the pickling process, in order to reduce the possibility of hydrogen generation, the HF and the HNO need to be strictly controlled3The concentration ratio of (A) and the temperature of the pickling solution. In addition, the nitric acid used in the pickling solution is generally a 65% aqueous solution, which is highly oxidizing and volatile, and generates a large amount of nitrogen when it reacts with the metal surfaceThe oxygen nitride compounds have high corrosivity to human bodies and the environment, fluorine is accumulated toxicant, once the oxygen nitride compounds enter the environment, the oxygen nitride compounds can cause pollution to a certain degree, plants can absorb the fluorine, animals eat polluted forage, so that joint deformation and osteoporosis are caused, excessive fluorine is ingested by human bodies, the activity of various enzymes in the bodies can be interfered, the metabolic balance of calcium and phosphorus is damaged, and then the fluorosis is caused, so that HF-HNO (hydrogen fluoride-HNO)3The treatment of the waste liquid after pickling is also a non-negligible step, which undoubtedly increases the difficulty of the pickling process.
Therefore, it is necessary to provide a polishing solution which is environmentally friendly and can efficiently clean the surface of the titanium alloy.
Disclosure of Invention
In order to solve the technical problems, the invention provides a titanium alloy pickling polishing solution and a preparation method and application thereof.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of titanium alloy pickling polishing solution, which comprises the following steps:
mixing sulfamic acid, ascorbic acid and lactic acid to obtain pickling base liquid, adding an additive, and stirring to obtain the titanium alloy pickling polishing liquid.
Further, the mass ratio of the sulfamic acid to the ascorbic acid to the lactic acid is 1: (0.5-1): (1-2).
Furthermore, the concentration of sulfamic acid is 160g/L of 120-ketone, the concentration of ascorbic acid is 60-160g/L, and the concentration of lactic acid is 320g/L of 120-ketone.
Further, the additive comprises one or more of sodium chloride, potassium pyrophosphate, hydrazine hydrate and OP-10 surfactant.
Furthermore, the addition amount of the sodium chloride in the acid washing base liquid is 0-15g/L, the addition amount of the potassium pyrophosphate in the acid washing base liquid is 0-15g/L, the addition amount of the hydrazine hydrate in the acid washing base liquid is 0-5g/L, the addition amount of the OP-10 surfactant in the acid washing base liquid is 0-3g/L, and the addition amounts of the substances are not 0 at the same time.
Further, the preparation method is carried out at normal temperature.
The invention also provides the titanium alloy pickling polishing solution prepared by the preparation method.
The invention also provides application of the titanium alloy pickling polishing solution in removing a titanium alloy surface pollution layer, and the specific process comprises the following steps: and (3) placing the titanium alloy material into titanium alloy pickling polishing solution, and soaking at normal temperature.
Further, the soaking treatment time is 10-20 min.
The invention discloses the following technical effects:
the organic acid of sulfamic acid, ascorbic acid and lactic acid used in the invention is solid in a normal state, is safer in the transportation process, has weaker acidity than inorganic acid, is not easy to corrode, and the waste liquid of pickling is easy to treat; sodium chloride, potassium pyrophosphate, hydrazine hydrate and OP-10 are added to achieve the effect of improving the pickling effect and prevent the secondary corrosion of the titanium alloy surface caused by excessive pickling.
The pickling solution is formed by compounding organic acid and neutral salt, the main component of sulfamic acid has the advantages of nonvolatility, no odor, low toxicity and the like, most metal salts of sulfamic acid have good solubility, are not easy to precipitate in the pickling solution, can effectively improve the acid effect, obtain a clean and bright titanium alloy surface, provide a good foundation for subsequent treatment, can be operated at normal temperature in the whole pickling process, and reduce the heating cost and the occupied area of heating facilities in production. Meanwhile, the main components of the acid solution can not corrode the surface of the titanium alloy, the acid washing process is relatively smooth and stable, the difficulty of waste liquid treatment in the acid washing process is reduced, and the harm of fluorine ions in the traditional titanium alloy acid washing solution to the environment is relieved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
Fig. 1 is a surface view of a titanium alloy test piece plate in example 8 before and after immersion, wherein (a) is before immersion and (b) is after immersion.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification.
The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 120g/L ascorbic acid and 120g/L lactic acid at the room temperature of 25 ℃ according to the mass ratio of 1:1:1 to prepare an acid-washing polishing solution, and standing at the normal temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish normal-temperature pickling of the titanium alloy. And residual oxide scale on the surface of the titanium alloy after acid cleaning.
Example 2
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 60g/L ascorbic acid and 120/L lactic acid according to the mass ratio of 1:0.5:1 at room temperature and 25 ℃ to prepare an acid-washing polishing solution, and standing at normal temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish normal-temperature pickling of the titanium alloy. And residual oxide scale on the surface of the titanium alloy after acid cleaning.
Example 3
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 120g/L ascorbic acid and 240g/L lactic acid at the room temperature of 25 ℃ according to the mass ratio of 1:1:2 to prepare an acid-washing polishing solution, and standing at the room temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish normal-temperature pickling of the titanium alloy. And residual oxide scale on the surface of the titanium alloy after acid cleaning.
Example 4
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 120g/L ascorbic acid and 240g/L lactic acid at room temperature of 25 ℃ according to the mass ratio of 1:1:2, adding 10g/L sodium chloride to prepare an acid-washing polishing solution, and standing at normal temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish pickling the titanium alloy at normal temperature. And residual oxide scale on the surface of the titanium alloy after acid cleaning. The surface of the titanium alloy after acid washing has no residual oxide skin, and the added sodium chloride has a micro-polishing effect, so that the brightness is improved.
Example 5
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 120g/L ascorbic acid and 240g/L lactic acid at room temperature of 25 ℃ according to the mass ratio of 1:1:2, adding 10g/L sodium chloride and 10g/L potassium pyrophosphate to prepare an acid-washing polishing solution, and standing at normal temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish pickling the titanium alloy at normal temperature. The surface of the titanium alloy after acid washing has no residual oxide skin, and the added sodium chloride and potassium pyrophosphate synergistically play a micro-polishing role, so that the brightness is improved.
Example 6
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 120g/L ascorbic acid and 240g/L lactic acid according to the mass ratio of 1:1:2 at room temperature and 25 ℃, adding 10g/L sodium chloride, 10g/L potassium pyrophosphate and 3g/L hydrazine hydrate to prepare an acid-washing polishing solution, and standing at normal temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish pickling the titanium alloy at normal temperature. After acid washing, a clean titanium alloy matrix is obtained, and the titanium alloy matrix has no oxide skin and no corrosion mark. The surface of the titanium alloy after acid washing has no residual oxide skin, and the added sodium chloride, potassium pyrophosphate and hydrazine hydrate cooperatively play a role in micro-polishing, so that the brightness is improved.
Example 7
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 120g/L ascorbic acid and 240g/L lactic acid according to the mass ratio of 1:1:2 at room temperature and 25 ℃, adding 10g/L sodium chloride, 10g/L potassium pyrophosphate, 3g/L hydrazine hydrate and 1g/L OP-10 to prepare an acid-washing polishing solution, and standing at normal temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish pickling the titanium alloy at normal temperature. The surface of the titanium alloy after acid washing has no residual oxide skin, and the added sodium chloride, potassium pyrophosphate, hydrazine hydrate and OP-10 cooperatively play a role in micro-polishing, so that the brightness is improved.
Example 8
The normal-temperature pickling method for the titanium alloy comprises the following process steps:
1. pretreatment of titanium alloy material
Cutting the titanium alloy into sample plates with the diameter of 20mm multiplied by 30 mm; cleaning with clear water, drying the sample with a blower, and placing the sample in a dry place for later use.
2. Acid pickling treatment of titanium alloy
Mixing 120g/L sulfamic acid, 120g/L ascorbic acid and 240g/L lactic acid according to the mass ratio of 1:1:2 at room temperature and 25 ℃, adding 15g/L sodium chloride, 15g/L potassium pyrophosphate, 5g/L hydrazine hydrate and 3g/L OP-10 to prepare an acid-washing polishing solution, and standing at normal temperature for later use; and (3) placing the sample plate 1 in an acid pickling polishing solution, and pickling for 15min at normal temperature to finish pickling the titanium alloy at normal temperature. Referring to the front and rear comparative drawings of the titanium alloy test piece plate of this example, FIG. 1 shows that (a) the titanium alloy test piece plate is before soaking and (b) the titanium alloy test piece plate is after soaking, and the clean and bright titanium alloy matrix is obtained after acid washing, and the titanium alloy test piece plate has no scale and no corrosion mark.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. The preparation method of the titanium alloy pickling polishing solution is characterized by comprising the following steps of:
mixing sulfamic acid, ascorbic acid and lactic acid to obtain pickling base liquid, adding an additive, and stirring to obtain the titanium alloy pickling polishing liquid.
2. The production method according to claim 1, wherein the mass ratio of the sulfamic acid, the ascorbic acid and the lactic acid is 1: (0.5-1): (1-2).
3. The method as claimed in claim 1, wherein the concentration of sulfamic acid is 160 g/L-120-.
4. The method according to claim 1, wherein the additive added to the acid-washing base solution comprises one or more of sodium chloride, potassium pyrophosphate, hydrazine hydrate and OP-10 surfactant.
5. The process according to claim 4, wherein the sodium chloride is added in an amount of 0 to 15g/L, the potassium pyrophosphate is added in an amount of 0 to 15g/L, the hydrazine hydrate is added in an amount of 0 to 5g/L, the OP-10 surfactant is added in an amount of 0 to 3g/L, and the amounts of the above substances are not 0 at the same time.
6. The method of claim 1, wherein the method is performed at room temperature of 25 ℃.
7. A titanium alloy pickling polishing solution prepared by the preparation method of any one of claims 1 to 6.
8. The application of the titanium alloy pickling polishing solution in the removal of the pollution layer on the surface of the titanium alloy in claim 7 is characterized by comprising the following specific steps: and (3) placing the titanium alloy material into titanium alloy pickling polishing solution, and soaking at normal temperature.
9. Use according to claim 8, wherein the soaking treatment time is 10-20 min.
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2021
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| US4470920A (en) * | 1981-05-11 | 1984-09-11 | Custom Research And Development | Metal oxide remover for stainless steels |
| US4367092A (en) * | 1981-07-16 | 1983-01-04 | Roto-Finish Company, Inc. | Corrosion-inhibiting acid burnishing compound |
| CN1288920A (en) * | 1999-09-21 | 2001-03-28 | 不二见株式会社 | Polishing composition |
| CN103074635A (en) * | 2013-01-05 | 2013-05-01 | 辽宁省电力有限公司电力科学研究院 | Metal surface cleaning anti-scaling agent containing compound acid |
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