A processing method for improving the degreasing performance of titanium strip coil
By employing pre-degreasing, powder degreasing, and electrolytic degreasing processes that do not require unwinding, combined with the use of alkaline solutions and electrolytes, the problem of incomplete removal of grease from the surface of titanium strip rolls has been solved, achieving efficient and stable degreasing results and avoiding the defects of unwinding.
Patent Information
- Application Number
- CN202410940143.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-15
- Publication Date
- 2025-12-05
- Estimated Expiration
- 2044-07-15
AI Technical Summary
Existing methods for degreasing titanium strip rolls require unwinding, which makes the operation complex and time-consuming, and may damage or contaminate the surface of the titanium strip roll, and it is difficult to completely remove the grease and impurities from the surface.
The process employs a non-unwinding method, including pre-degreasing, powder degreasing, electrolytic degreasing, and annealing. It combines the use of alkaline solution, degreasing agent, and electrolyte to thoroughly remove oil stains through high-pressure spraying and electrolytic reaction. The synergistic effect of air-absorbing powder and electrolyte is utilized to improve the degreasing effect.
It achieves efficient degreasing of uncoiled titanium strip, with a wet area ratio of 99.5-99.9% after degreasing. This avoids the local deformation problem of uncoiling, ensures the integrity and stability of the titanium strip, and improves the degreasing efficiency and effect.
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Figure CN118880348B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of grease removal technology on the surface of alloy strip coils, specifically to a processing method for improving the degreasing performance of titanium strip coils. Background Technology
[0002] During the cold rolling process of titanium strip, lubricating oil needs to be sprayed onto the surface for lubrication and cooling. Therefore, after rolling, a layer of rolling oil film remains on the surface of the titanium coil. To clean the titanium coil thoroughly, the surface oil film must be removed quickly. To avoid lubricating oil contaminating the surface quality of the titanium strip, the surface must be cleaned and degreased before annealing. In the production process of titanium strip coil, surface grease removal is a critical step. This step is mainly to ensure that the rolling oil and other grease substances on the surface of the titanium strip coil are completely removed before entering the vacuum furnace for heat treatment. If these greases remain on the surface of the titanium strip coil, even in small amounts, they may cause oxidation contamination and discoloration of the titanium strip surface, thereby affecting the quality and performance of the product.
[0003] Furthermore, most existing degreasing methods for titanium strip coils require unwinding before operation. While unwinding degreasing can more directly degrease each part of the titanium strip coil, this process is usually more complex and time-consuming. After unwinding, each layer or section needs to be processed separately before rewinding, which not only increases the complexity and time cost of the operation, but may also cause damage or contamination to the surface of the titanium strip coil due to multiple processing. In order to solve the above problems, this invention proposes a processing method that has good degreasing performance without unwinding. Summary of the Invention
[0004] To address the aforementioned problems, this invention provides a processing method for improving the degreasing performance of titanium strip rolls.
[0005] The technical solution of this invention is: a processing method for improving the degreasing performance of titanium strip coils, comprising the following steps:
[0006] S1, Pre-degreasing
[0007] The titanium strip roll is sequentially passed through a first alkaline solution tank, an immersion tank, a second alkaline solution tank, a rinsing tank, a third alkaline solution tank, and a cleaning tank, and ultrasonically treated for 5-10 minutes each to obtain a pre-degreased titanium strip roll. The alkalinity point of the first alkaline solution tank is 3-5%, and then the alkalinity point of each subsequent tank is increased by 2.5-5%. The rinsing tank contains a solution of nitric acid with a concentration of 15-20 g / L and hydrofluoric acid with a concentration of 30-50 g / L, mixed at a mass ratio of 2-2.5:1. The alkaline solution temperature is 15-30℃.
[0008] The soaking tank contains water at a temperature of 40-50℃; the top of the cleaning tank is equipped with a spray nozzle for spraying degreasing agent A at a temperature of 50-60℃, and a brush roller is rotatably mounted above the cleaning tank; the brush roller brushes the upper surface of the titanium strip roll to clean the impurities adhering to the surface of the titanium strip roll.
[0009] S2, Degreasing treatment
[0010] S2-1, Powder Degreasing:
[0011] The air-absorbing powder, binder, and degreasing agent A flowing from the bottom of the titanium strip roll are mixed at a mass ratio of 0.3-0.5:0.05-0.1:1 to obtain degreasing agent B, which is then divided into 2-3 equal portions. The pre-degreased titanium strip roll is then placed vertically, and one portion of degreasing agent B is sprayed through the gaps between the top layers of the titanium strip roll using a high-pressure rotary nozzle. The flow rate of the high-pressure nozzle is 1.5-2 m³ / h. 3 The nozzle pressure is 0.8-1.8 MPa, and the spray angle is 45-65°. The degreasing agent is sprayed onto the surface of the strip at the aforementioned pressure. This helps the degreasing liquid penetrate the interlayer of the strip, reducing the residue of internal impurities. This method ensures more thorough contact between the degreasing agent and the oil stains than traditional soaking or surface coating, thus improving the degreasing effect. The high-pressure airflow not only helps the degreasing agent to be evenly distributed on the surface of the titanium strip, but may also enhance its permeability, allowing the degreasing agent to penetrate deeper into the oil stains, especially those adhering to the inside of the titanium strip or in complex structures. This helps to remove oil stains more thoroughly and improves the degreasing quality. The binder provides a carrier and mechanical support for the air-absorbing powder, giving it good flowability, thereby forming a stable degreasing agent B, which provides the necessary promotion for improving the electrolytic degreasing effect of degreasing agent B on the surface of the titanium strip.
[0012] S2-2, Electrolytic Degreasing
[0013] The titanium strip roll is placed in an electrolytic cell, with the titanium strip roll serving as the cathode and the electrode plate as the anode. Electricity is then applied. The electrolyte in the electrolytic cell is a potassium hydroxide solution with a molar concentration of 0.15-0.2 mol / L. For every 5-10°C increase in electrolyte temperature, 1 / 8-1 / 4 of the remaining degreasing agent B and 0.5-0.7% of the mass of degreasing agent B, a low-foaming surfactant, are added. The mixture is kept at this temperature for 5-7 minutes. After the degreasing agent B has been completely added, the titanium strip roll is removed and rinsed with water spray at a pressure of 0.15-0.25 MPa and a temperature of 40-50°C. The current in the electrolytic cell is 2400-2600 A, and the current density is 5-10 A / dm³. 2 ;
[0014] S3, Annealing treatment
[0015] The electrolytically degreased titanium strip is fed into a vacuum furnace at 750-800℃ and heated at a speed of 25-45m. 3 Helium gas is introduced at a flow rate of / h for annealing, and then straightening is performed after annealing.
[0016] S4. Leveling treatment
[0017] The titanium strip coil that has undergone the tension straightening treatment is then subjected to surface leveling treatment to obtain a leveled titanium strip coil.
[0018] Description: This method for degreasing titanium strip coils can treat the surface of titanium strip coils with open lengths of up to thousands of meters and coiled into a ring shape. The wet area ratio after degreasing can reach 99.5-99.9%, which is only slightly different from the degreasing effect after unwinding using traditional degreasing processes. Air-purifying powder degreasing is used as a preliminary treatment step to remove most of the grease and dirt from the surface of the titanium strip coil. Subsequent electrolytic degreasing can further clean the surface, removing more difficult-to-remove oil and residues. This combined degreasing method improves the thoroughness and efficiency of degreasing. The cleaner surface of the titanium strip coil after air-purifying powder degreasing reduces the content of impurities and contaminants in the electrolytic degreasing solution, thus helping to maintain the stability and activity of the electrolytic degreasing solution and extend its service life.
[0019] Potassium hydroxide solution, as a strong electrolyte, can form ions in water, thereby enhancing the conductivity of the solution. This helps the electrolysis reaction proceed more efficiently, improving the speed and effect of degreasing. It also ensures that the pH value of the degreasing solution is maintained within the alkaline range. An alkaline environment promotes the saponification and emulsification of greases, thus more effectively removing oil stains from the surface of the titanium strip. Furthermore, adding degreasing agent B according to its mass percentage can also play a positive role in supplementing the degreasing capacity, thereby improving the degreasing effect and efficiency.
[0020] The suction powder can adsorb grease from the surface of the titanium strip because grease molecules are typically oleophilic, while the suction powder is hydrophilic. Under high-pressure airflow, the suction powder is sprayed onto the surface of the titanium strip. Upon contact with the grease molecules, it firmly adsorbs them through physical or chemical adsorption, thus removing the grease. In addition to adsorbing grease, the suction powder, through its physical shape (such as spherical or irregular shapes), can create tiny unevenness on the surface of the titanium strip. This increases the mechanical force during the cleaning process, helping to more thoroughly remove surface grease and other particles.
[0021] Further, in step S1, during the rinsing process, shot blasting is performed using spherical cast steel sand with a particle size of 1-3 mm. The shot blasting speed is 40-200 m / min, the spray angle is 30-50°, the amount of shot blasting sand is 600-800 kg / min, and the shot blasting time is 30-120 s.
[0022] Note: Shot blasting removes residues, oil, and other impurities from the surface of titanium strip coils through high-speed impact of spherical cast steel sand. This enhances the rinsing effect, making the rinsing process more thorough. Furthermore, shot blasting improves the surface morphology of the titanium strip coils and increases surface roughness, which helps improve the adhesion and penetration of subsequent degreasing agents. Under the above-mentioned treatment parameters, excessive damage to the titanium strip coils can be avoided during shot blasting.
[0023] Further, in step S1, the alkali solution in the first alkali solution tank, the second alkali solution tank, and the third alkali solution tank is a sodium hydroxide solution, and microwave-assisted heating is performed while each alkali solution tank is immersed; wherein, the microwave power is 18-20kW, the heating temperature is 25-40℃, and the microwave time is 5-25min.
[0024] Note: Microwave-assisted treatment can also improve the cleanliness of the titanium strip roll surface by alkaline solution. Since the titanium strip roll is not unwound, the microwave action can accelerate the decomposition and removal of grease and impurities in the gaps on the surface of the titanium strip roll, thereby improving the treatment effect of alkaline solution on the surface of the titanium strip roll.
[0025] Furthermore, in step S1, the brush roller is one of nylon brush roller, non-woven brush roller, and ceramic brush roller;
[0026] Note: Nylon and non-woven fabric brush rollers have small capillary branches and are generally soft, which can effectively clean dirt and oil stains on the end face of titanium strip rolls. In addition, they can clean gently without damaging the surface of titanium strip rolls. Ceramic brush rollers can significantly improve the surface smoothness of the end face of titanium strip rolls and remove undesirable surface conditions through the micro-friction and passivation effect of the bristles.
[0027] Further, in step S1, the degreasing agent A comprises, by mass parts: 2-5 parts acetone, 0.5-3 parts sodium carbonate, 8-12 parts benzotriazole, 3-4 parts emulsified microcapsules, 4-6 parts penetrant JFC, and 35-65 parts deionized water.
[0028] The emulsified microcapsules, by weight percentage, comprise 25-40% resin microspheres, 2-8% sodium silicate solution with a concentration of 25-35 g / L, 10-20% silica dispersant, 1-5% dextrin, 1.5-2% silica sol, 0.8-1.2% curing agent, and the balance being water.
[0029] Explanation: By adding emulsifying microcapsules to degreasing agent A, various water-soluble emulsifiers can be spontaneously embedded within the microcapsules and their release can be controlled at a manageable rate. This means that the emulsifying components can act on the grease more evenly and continuously, thereby further enhancing the degreasing efficiency of the degreasing agent on the surface of the titanium strip and improving the degreasing effect. Resin microspheres can serve as the wall material of the microcapsules during the preparation of emulsifying microcapsules, providing structural support and protection. The addition of sodium silicate solution can improve the stability of the emulsifying microcapsules and prevent the microcapsules from rupturing or agglomerating during preparation and storage. Penetrant JFC can serve as an auxiliary agent during the preparation process to improve reaction efficiency and degreasing effect. It has high permeability and can promote the faster diffusion and penetration of degreasing components into the interior of the titanium strip.
[0030] Furthermore, the method for preparing the emulsified microcapsules is as follows:
[0031] Divide the sodium silicate solution into 2-3 equal parts, and mix the silica sol, water and one part of the sodium silicate solution to obtain composite solution A. Then add resin microspheres to composite solution A at a solid-liquid ratio of 1:2.5-3 and ultrasonically disperse for 15-20 minutes to obtain suspension C.
[0032] Add silica dispersant and dextrin sequentially to the remaining sodium silicate solution, stir and mix at 80-90℃ to obtain composite solution B;
[0033] The composite solution B was homogenized and emulsified using a homogenizer at 8000-9000 rpm for 1-1.5 min, and then centrifuged at 1000-1500 rpm for 18-20 min to obtain an emulsion. Finally, the suspension C and the curing agent were mixed and added to the emulsion. Finally, the mixture was centrifuged and spray-dried at 16000-18000 rpm for 10-20 min to obtain emulsified microcapsules.
[0034] Note: Sodium silicate solution mixed with silica sol and water can form a colloidal solution with good suspension and dispersibility. This solution can be used to make coatings and adhesives. The concentration of sodium silicate solution affects the dispersibility and stability of microcapsules, while the addition of silica dispersant and dextrin may improve the morphology and size distribution of microcapsules. The addition of curing agent will cause the resin microspheres in the resin microsphere composite solution to undergo a curing reaction and form a stable structure. Adding the cured resin microsphere mixture to the emulsion can help the resin microspheres to be uniformly dispersed in the liquid, thereby obtaining emulsified microcapsules.
[0035] Further, in step S2-1, the air-absorbing powder is either titanium powder or zirconium powder, and the binder is polyoxymethylene;
[0036] Explanation: Titanium powder and zirconium powder, as getters, have the ability to react with gases such as carbon, hydrogen, nitrogen, and oxygen at high temperatures. This means that during the degreasing process, these powders can effectively absorb and remove residual gases from the powder, helping to reduce the adverse effects of gases on the degreasing effect and powder quality. As metal powders, titanium powder and zirconium powder also have good thermal conductivity, which helps to transfer heat more evenly during the degreasing process, improving the degreasing speed and effect. Polyoxymethylene, as a multi-component binder, can effectively fix the titanium strip roll powder particles, preventing the powder from falling off or deforming during the degreasing process, thereby ensuring the smooth progress of the degreasing process and effectively improving the degreasing performance of the titanium strip roll.
[0037] Furthermore, in step S3, the elongation rate during the straightening process is 0.2-0.5%;
[0038] Note: Appropriate elongation helps eliminate plate shape defects in titanium strip coils, such as waviness and warping, thereby significantly improving the plate shape quality of the strip. Controlling the elongation allows the strip to undergo appropriate deformation during the stretching, bending and straightening process, achieving the ideal flatness requirements.
[0039] Furthermore, in step S4, the surface smoothing treatment adopts a continuous grinding and polishing unit, and the process parameters are as follows: the operating speed of the continuous grinding and polishing unit is 5-7m / min, and the mesh size of the grinding head abrasive belt is 200-300 mesh;
[0040] Note: Appropriate operating speed and abrasive belt mesh size can ensure high production efficiency while maintaining polishing quality.
[0041] The beneficial effects of this invention are:
[0042] (1) This invention effectively optimizes the degreasing process for titanium strip rolls without unwinding them. It can achieve surface treatment of titanium strip rolls with an open length of up to thousands of meters and wrapped into a ring shape without unwinding. The wet area ratio after degreasing can reach 99.5-100%, which is similar to the degreasing effect after unwinding in traditional degreasing processes. At the same time, using this process for degreasing also helps to maintain the integrity and stability of the titanium strip roll. During the degreasing process, both the inside and outside of the titanium strip roll can be effectively treated, avoiding problems such as local deformation that may occur after unwinding.
[0043] (2) In this invention, the titanium strip roll is first pretreated with an alkaline solution with progressively increasing alkaline point. The alkaline solution treatment can increase the surface roughness of the titanium substrate and generate nanoscale micropores on its surface. This microstructure, due to its rougher surface, can usually better adsorb and remove contaminants such as grease. At the same time, a porous sodium titanate structure will be formed on the surface of the titanium substrate after alkaline treatment. Then, the titanium strip roll is further treated locally by powder degreasing and electrolytic degreasing processes. For local areas of the titanium strip roll, the surface of the titanium strip roll after alkaline treatment contains negatively charged Ti-OH groups, which can serve as active sites for electrochemical reactions, promoting the evolution of hydrogen and oxygen during electrolysis. The evolution of these gases will generate a strong stirring effect, which helps to peel off the oil and impurities on the surface of the titanium strip roll and carry them into the solution, further promoting the electrolytic degreasing treatment effect. Through the synergistic effect of these two degreasing processes, powder degreasing and electrolytic degreasing, a deep cleaning of the surface of the titanium strip roll can be achieved, removing stubborn grease and contaminants that are difficult to remove by conventional methods.
[0044] (3) This invention further promotes the degreasing effect of the degreasing agent on the surface of titanium strip by preparing a specific degreasing agent A containing emulsified microcapsules. By embedding the emulsifier in the emulsified microcapsules, the release rate of the emulsifier can be effectively controlled. When the emulsifier is embedded in the emulsified microcapsules, its dispersibility and stability are enhanced, which helps to react more effectively with oil during the degreasing process, thereby improving the separation efficiency of the degreasing agent. By first preparing the resin microspheres into a suspension, it can be ensured that the microspheres are uniformly dispersed in the system, avoiding agglomeration or sedimentation. Then, this suspension is mixed with the curing agent and then combined with the emulsion to form a more stable emulsified microcapsule system. Through the preparation of emulsified microcapsules, the resin microsphere suspension and the curing agent can be more uniformly coated in the emulsion, thereby further improving the emulsification effect of the emulsified microcapsules on oil. Attached Figure Description
[0045] Figure 1 This is a process flow diagram of the present invention;
[0046] Figure 2 This is a graph showing the changes in the degreasing performance of titanium strip rolls in Examples 1-12 and Control Groups 1-3 of the present invention;
[0047] Figure 3 This is a graph showing the changes in the degreasing performance of titanium strip rolls in Examples 1, 12-21, and Control Groups 4-5 of the present invention;
[0048] Figure 4 This is a graph showing the changes in the degreasing performance of titanium strip rolls in Examples 1, 22-30, and Control Groups 6-7 of the present invention. Detailed Implementation
[0049] To further illustrate the methods and effects of this invention, the technical solution of this invention will be clearly and completely described below in conjunction with experiments.
[0050] Example 1: A processing method for improving the degreasing performance of titanium strip coils, comprising the following steps:
[0051] S1, Pre-degreasing
[0052] The titanium strip coil was sequentially passed through a first alkaline bath, an immersion bath, a second alkaline bath, a rinsing bath, a third alkaline bath, and a cleaning bath, and ultrasonically treated for 8 minutes each to obtain a pre-degreased titanium strip coil. The alkalinity of the first alkaline bath was 4%, and then the alkalinity of the alkaline bath in each subsequent bath was increased by 4%. The alkaline bath was a sodium hydroxide solution at a temperature of 22°C. The rinsing bath contained a solution of 18 g / L nitric acid and 40 g / L hydrofluoric acid mixed in a mass ratio of 2.3:1.
[0053] In step S1, during the rinsing process, shot blasting is performed using spherical cast steel sand with a particle size of 1-3 mm. The shot blasting speed is 120 m / min, the spray angle is 40°, the amount of shot blasting sand is 700 kg / min, and the shot blasting time is 75 s.
[0054] In step S1, microwave-assisted heating is performed while the alkaline solution is being soaked in each tank; the microwave power is 19kW, the heating temperature is 32℃, and the microwave time is 15min.
[0055] The soaking tank contains water at a temperature of 45℃; the top of the cleaning tank is equipped with a spray nozzle for spraying degreasing agent A at a temperature of 55℃, and a brush roller is rotated above the cleaning tank; the brush roller is a nylon brush roller; degreasing agent A is a commercially available degreasing agent;
[0056] S2, Degreasing treatment
[0057] S2-1, Powder Degreasing:
[0058] The suction powder, binder, and degreasing agent A flowing from the bottom of the titanium strip roll were mixed at a mass ratio of 0.4:0.08:1 to obtain degreasing agent B, which was then divided into two equal portions. The pre-degreased titanium strip roll was then placed vertically, and one portion of degreasing agent B was sprayed through the gaps between the top layers of the titanium strip roll using a high-pressure rotary nozzle. The flow rate of the high-pressure nozzle was 1.8 m³ / s. 3 / h, nozzle pressure is 1.3MPa, and spray angle is 55°;
[0059] In step S2-1, the getter powder is titanium powder and the binder is polyoxymethylene;
[0060] S2-2, Electrolytic Degreasing
[0061] The titanium strip roll was placed in the electrolytic cell, serving as the cathode and the electrode plate as the anode. Electricity was then applied. The electrolyte in the electrolytic cell was a 0.18 mol / L potassium hydroxide solution. For every 8°C increase in electrolyte temperature, 1 / 6 of the remaining degreasing agent B and 0.6% (by mass) of a low-foaming surfactant were added, and the mixture was kept at this temperature for 6 minutes. After all the degreasing agent B had been added (i.e., 6 additions of 1 / 6 of the remaining degreasing agent B each time), the titanium strip roll was removed and rinsed with water spray at a pressure of 0.2 MPa and a temperature of 45°C. The current in the electrolytic cell was 2500 A, and the current density was 8 A / dm³. 2 The low-foaming surfactant is trisodium phosphate solid.
[0062] S3, Annealing treatment
[0063] The electrolytically degreased titanium strip is fed into a vacuum furnace at 775°C and heated at 35m. 3 Helium gas is introduced at a flow rate of / h for annealing, followed by tensile straightening; the elongation during the tensile straightening process is 0.3%.
[0064] S4. Leveling treatment
[0065] The titanium strip coil that has undergone tension straightening is then subjected to surface leveling treatment to obtain a leveled titanium strip coil. The surface leveling treatment is performed using a continuous grinding and polishing unit with the following process parameters: the operating speed of the continuous grinding and polishing unit is 6m / min, and the mesh size of the grinding head abrasive belt is 250 mesh.
[0066] Example 2: Unlike Example 1, in step S1, the alkali point of the first alkali tank is 3%, and then the alkali point of each tank is increased by 2.5%; the alkali temperature is 15°C.
[0067] Example 3: Unlike Example 1, in step S1, the alkali point of the first alkali tank is 5%, and then the alkali point of each tank is increased by 5%; the alkali temperature is 30°C.
[0068] Example 4: Unlike Example 1, in step S1, the rinsing tank contains a solution obtained by mixing nitric acid with a concentration of 15 g / L and hydrofluoric acid with a concentration of 30 g / L in a mass ratio of 2:1.
[0069] Example 5: Unlike Example 1, in step S1, the rinsing tank contains a solution obtained by mixing nitric acid with a concentration of 20 g / L and hydrofluoric acid with a concentration of 30-50 g / L in a mass ratio of 2.5:1.
[0070] Example 6: Unlike Example 1, in step S1, spherical cast steel sand with a particle size of 1-3 mm is used for shot blasting during the rinsing process. The shot blasting speed is 40 m / min, the spray angle is 30°, the amount of shot blasting sand is 600 kg / min, and the shot blasting time is 120 s.
[0071] Example 7: Unlike Example 1, in step S1, spherical cast steel sand with a particle size of 1-3 mm is used for shot blasting during the rinsing process. The shot blasting speed is 200 m / min, the spray angle is 50°, the amount of shot blasting sand is 800 kg / min, and the shot blasting time is 30 s.
[0072] Example 8: Unlike Example 1, in step S1, the microwave power is 18kW, the heating temperature is 25℃, and the microwave time is 25min during the microwave-assisted heating process.
[0073] Example 9: Unlike Example 1, in step S1, the microwave power is 20kW, the heating temperature is 40℃, and the microwave time is 5min during the microwave-assisted heating process.
[0074] Example 10: Unlike Example 1, in step S1, the soaking tank contains water at a temperature of 40°C; the top of the cleaning tank is equipped with a spray nozzle for spraying degreasing agent A at a temperature of 50°C.
[0075] Example 11: Unlike Example 1, in step S1, the soaking tank contains water at a temperature of 50°C; the top of the cleaning tank is equipped with a spray nozzle for spraying degreasing agent A at a temperature of 60°C.
[0076] Example 12: Unlike Example 1, in step S2-1, the air-absorbing powder, binder, and degreasing agent A flowing out from the bottom of the titanium strip roll are mixed in a mass ratio of 0.3:0.5:1 to obtain degreasing agent B.
[0077] Example 13: Unlike Example 1, in step S2-1, the air-absorbing powder, binder, and degreasing agent A flowing out from the bottom of the titanium strip roll are mixed in a mass ratio of 0.5:0.7:1 to obtain degreasing agent B.
[0078] Example 14: Unlike Example 1, in step S2-1, the flow rate of the high-pressure nozzle is 1.5 m³ / s. 3 / h, nozzle pressure is 0.8MPa, and spray angle is 45°.
[0079] Example 15: Unlike Example 1, in step S2-1, the flow rate of the high-pressure nozzle is 2m³ / h. 3 / h, nozzle pressure is 1.8MPa, and spray angle is 65°.
[0080] Example 16: Unlike Example 1, in step S2-2, the electrolyte in the electrolytic cell is a potassium hydroxide solution with a molar concentration of 0.15 mol / L. For every 5°C increase in electrolyte temperature, 1 / 8 of the remaining degreasing agent B and 0.5% of the mass percentage of degreasing agent B low-foaming surfactant are added (i.e., degreasing agent B is added 8 times, each time the amount added is 1 / 8 of the remaining degreasing agent B), and the temperature is maintained for 7 minutes.
[0081] Example 17: Unlike Example 1, in step S2-2, the electrolyte in the electrolytic cell is a potassium hydroxide solution with a molar concentration of 0.2 mol / L. For every 10°C increase in electrolyte temperature, 1 / 4 of the remaining degreasing agent B and a low-foaming surfactant accounting for 0.7% of the mass percentage of degreasing agent B are added (i.e., degreasing agent B is added 4 times, each time the amount added is 1 / 4 of the remaining degreasing agent B), and the temperature is maintained for 5 minutes.
[0082] Example 18: Unlike Example 1, in step S2-2, after the solution temperature in the electrolytic cell reaches 70°C, the titanium strip roll is taken out and rinsed with water spray at a pressure of 0.15MPa and a water temperature of 40°C.
[0083] Example 19: Unlike Example 1, in step S2-2, after the solution temperature in the electrolytic cell reaches 80°C, the titanium strip roll is taken out and rinsed with water spray at a pressure of 0.25 MPa and a water temperature of 50°C.
[0084] Example 20: Unlike Example 1, in step S2-2, the current in the electrolytic cell is 2400A and the current density is 5A / dm³. 2 .
[0085] Example 21: Unlike Example 1, in step S2-2, the current in the electrolytic cell is 2600A and the current density is 10A / dm³. 2 .
[0086] Example 22: Unlike Example 1, in step S3, the electrolytically degreased titanium strip roll is fed into a vacuum furnace at 750°C and heated at 25m... 3 Helium gas is introduced at a flow rate of / h for annealing, followed by straightening; the elongation during the straightening process is 0.2%.
[0087] Example 23: Unlike Example 1, in step S3, the electrolytically degreased titanium strip roll is fed into a vacuum furnace at 800°C and heated at 45m... 3 Helium gas is introduced at a flow rate of / h for annealing, followed by straightening; the elongation during the straightening process is 0.5%.
[0088] Example 24: Unlike Example 1, in step S4, the operating speed of the continuous grinding and polishing unit is 5 m / min.
[0089] Example 25: Unlike Example 1, in step S4, the operating speed of the continuous grinding and polishing unit is 7 m / min.
[0090] Example 26: Unlike Example 1,
[0091] Degreasing agent A, by mass parts, includes: 4 parts acetone, 2 parts sodium carbonate, 10 parts benzotriazole, 3 parts emulsifying microcapsules, 5 parts penetrant JFC, and 50 parts deionized water;
[0092] The emulsified microcapsules, by weight percentage, comprise: 32% resin microspheres, 5% sodium silicate solution at a concentration of 30 g / L, 15% silica dispersant, 3% dextrin, 1.7% silica sol, 1% curing agent, and the balance being water; wherein, the curing agent is a commercially available conventional curing agent.
[0093] The preparation method of emulsified microcapsules is as follows:
[0094] The sodium silicate solution was divided into two equal parts, and the silica sol, water and one part of the sodium silicate solution were mixed to obtain composite solution A. Then, resin microspheres were added to composite solution A at a solid-liquid ratio of 1:2.8 and ultrasonically dispersed for 18 minutes to obtain suspension C.
[0095] Add silica dispersant and dextrin sequentially to the remaining sodium silicate solution, stir and mix at 85°C to obtain composite solution B;
[0096] The composite solution B was homogenized and emulsified for 1.3 min using a homogenizer at 8500 rpm, and then centrifuged at 1250 rpm for 19 min to obtain an emulsion. Finally, the suspension C and the curing agent were mixed and added to the emulsion. Finally, the mixture was centrifuged and spray-dried at 17000 rpm for 15 min to obtain emulsified microcapsules.
[0097] Example 27: Unlike Example 26, the degreasing agent A comprises, by mass parts: 2 parts acetone, 0.5 parts sodium carbonate, 8 parts benzotriazole, 3 parts emulsifying microcapsules, 4 parts penetrant JFC, and 35 parts deionized water;
[0098] The emulsified microcapsules, by weight percentage, comprise: 25% resin microspheres, 2% sodium silicate solution at a concentration of 25 g / L, 10% silica dispersant, 1% dextrin, 1.5% silica sol, 0.8% curing agent, and the balance being water.
[0099] Example 28: Unlike Example 26, the degreasing agent A comprises, by mass parts: 5 parts acetone, 3 parts sodium carbonate, 12 parts benzotriazole, 4 parts emulsifying microcapsules, 6 parts penetrant JFC, and 65 parts deionized water;
[0100] The emulsified microcapsules, by weight percentage, comprise: 40% resin microspheres, 8% sodium silicate solution at a concentration of 35 g / L, 20% silica dispersant, 5% dextrin, 2% silica sol, 1.2% curing agent, and the balance being water.
[0101] Example 29: Unlike Example 26, in the preparation method of the emulsified microcapsules,
[0102] The sodium silicate solution was divided into two equal parts, and the silica sol, water and one part of the sodium silicate solution were mixed to obtain composite solution A. Then, resin microspheres were added to composite solution A at a solid-liquid ratio of 1:2.5 and ultrasonically dispersed for 15 minutes to obtain suspension C.
[0103] After adding silica dispersant and dextrin to the remaining sodium silicate solution in sequence, stirring and mixing at 80°C, composite solution B is obtained.
[0104] The composite solution B was homogenized and emulsified for 1 min using a homogenizer at 8000 rpm, and then centrifuged at 1000 rpm for 20 min to obtain an emulsion. Finally, the suspension C and the curing agent were mixed and added to the emulsion. Finally, the mixture was centrifuged and spray-dried at 16000 rpm for 20 min to obtain emulsified microcapsules.
[0105] Example 30: Unlike Example 26, in the preparation method of the emulsified microcapsules,
[0106] The sodium silicate solution was divided into three equal parts, and the silica sol, water and one part of the sodium silicate solution were mixed to obtain composite solution A. Then, resin microspheres were added to composite solution A at a solid-liquid ratio of 1:3 and ultrasonically dispersed for 20 minutes to obtain suspension C.
[0107] After adding silica dispersant and dextrin to the remaining sodium silicate solution in sequence, stirring and mixing at 90°C, composite solution B was obtained.
[0108] The composite solution B was homogenized and emulsified for 1.5 min using a homogenizer at 9000 rpm, and then centrifuged at 1500 rpm for 18 min to obtain an emulsion. Finally, the suspension C and the curing agent were mixed and added to the emulsion. Finally, the mixture was centrifuged and spray-dried at 18000 rpm for 10 min to obtain emulsified microcapsules.
[0109] Experimental Example: The description of this experimental example is based on the scheme described in Example 1, and aims to illustrate the practical application effect of the present invention.
[0110] Experimental Design: To elucidate the degreasing properties of the titanium strip coil prepared in this invention, the following experimental group was designed:
[0111] Control group 1: Unlike Example 1, the soaking tank contained degreasing agent A at a temperature of 45°C; the top of the cleaning tank was equipped with a spray nozzle for spraying water at a temperature of 55°C.
[0112] Control group 2: Unlike Example 1, the shot blasting step was missing in step S1 during the rinsing process.
[0113] Control group 3: Unlike Example 1, in step S1, the microwave-assisted heating process was not performed during the immersion of each alkaline solution tank.
[0114] Control group 4: Unlike Example 1, in step S2-1, degreasing agent A was directly sprayed and degreased along the gap between the top titanium strip roll layers using a high-pressure rotary nozzle.
[0115] Control group 5: Unlike Example 1, step S2-2 electrolysis treatment was not performed.
[0116] Control group 6: Unlike Example 26, the emulsified microcapsules in defatting agent A were replaced with a commercially available emulsifier.
[0117] Control Group 7: Unlike Example 26, in the preparation of emulsified microcapsules, the components were directly mixed and emulsified in a homogenizer, and finally centrifuged and spray-dried at 17,000 rpm for 15 min to obtain emulsified microcapsules.
[0118] Degreasing performance evaluation method: Titanium strip rolls were prepared using Examples 1-30 and Comparative Examples 1-7. After unwinding, the rolls were rinsed with deionized water. The surface of the titanium strip rolls was observed to see if a continuous water film could be formed, and the area ratio of the water film was recorded.
[0119] 1. Investigate the effects of the pre-degreasing operation sequence and method on the degreasing performance of titanium strip rolls.
[0120] Conclusion: From Figure 2A comparison of Examples 1-11 and Comparative Examples 1-3 shows that adjusting the order of pre-degreasing the titanium strip coil in Comparative Example 1 resulted in a decrease in the degreasing performance of the titanium strip coil. Immersing in alkaline solution of low concentration first and then high concentration can reduce the direct impact of high concentration alkaline solution on the titanium strip coil substrate, thereby reducing the risk of corrosion to the substrate. At the same time, although the acid cleaning step will cause some corrosion to the strip, in this process, since the acid cleaning is after the alkaline solution treatment, it can help remove some residues generated during the alkaline solution treatment and further clean the surface. Multiple immersion treatments can ensure that the oil stains react fully with the alkaline solution, thereby improving the degreasing efficiency. In addition, the degreasing agent rinsing, as the last step, can ensure that the residual oil stains on the surface of the titanium strip coil are completely removed. However, the wet area ratio after degreasing is still 99.0% after adjusting the order.
[0121] In Comparative Example 2, the lack of shot blasting during the acid rinsing process resulted in the prepared titanium strip roll having a wet area ratio of only 93% after degreasing. The absence of shot blasting significantly reduced the degreasing performance of the titanium strip roll. Shot blasting can give the titanium strip roll a more uniform and consistent surface roughness, which helps to improve the adhesion of the degreasing agent, thereby promoting the degreasing effect of the degreasing agent on the titanium strip roll. In Comparative Example 3, the lack of microwave-assisted heating during the alkaline soaking process also resulted in a significant decrease in the degreasing performance of the titanium strip roll. This is because microwave-assisted treatment can promote the cleanliness of the titanium strip roll surface by the alkaline solution, and since the titanium strip roll is not unwound, the microwave action can accelerate the decomposition and removal of grease and impurities in the crevices of the titanium strip roll surface, thereby improving the treatment effect of the alkaline solution on the titanium strip roll surface.
[0122] 2. Investigate the effect of degreasing treatment steps on the degreasing performance of titanium strip rolls.
[0123] Conclusion: From Figure 3 The trend graphs of Examples 1, 12-23, and Control Groups 4-5 show that Control Group 4 lacks the preparation step of degreasing agent B. The absence of getter powder and binder also leads to a decrease in the degreasing performance of the titanium strip surface. This is because the components of degreasing agent B effectively promote electrolytic degreasing. During electrolytic degreasing, oil is peeled off from the steel strip surface by bubbles generated by electrolysis. Degreasing agent B, containing getter powder, enhances this peeling effect by adsorbing more oil particles, thereby improving degreasing efficiency. As shown in the graphs, electrolytic degreasing is a necessary step. The absence of this step weakens the degreasing effect on the titanium strip surface. In this application, following powder degreasing with electrolytic degreasing allows for further deep cleaning, removing more difficult-to-treat oil and residues. This combined degreasing method improves the thoroughness and efficiency of degreasing.
[0124] 3. Investigate the effects of annealing and leveling parameters, as well as the composition and preparation method of degreasing agent A, on the degreasing performance of titanium strip coils.
[0125] Conclusion: From Figure 4 The trends observed in Examples 1, 22-30, and Control Groups 6-7 show that the direct application of commercially available emulsifiers in Control Group 6 significantly impacted the degreasing efficiency of the titanium strip. This is because encapsulating the emulsifier in microcapsules allows for effective control of its release rate. Encapsulating the emulsifier enhances its dispersibility and stability, facilitating more effective interaction with oils during degreasing and thus improving the separation efficiency of the degreasing agent. In Control Group 7, the degreasing effect on the titanium strip surface prepared by directly homogenizing and emulsifying the components before centrifugal spray drying in the microcapsule preparation process also showed a significant decrease. Because the method of this application can first prepare resin microspheres into a suspension, which can ensure that the microspheres are uniformly dispersed in the system and avoid agglomeration or sedimentation, and then mix this suspension with the curing agent and then combine it with the emulsion, a more stable emulsion microcapsule system can be formed. Through the preparation of emulsion microcapsules, the resin microsphere suspension and the curing agent can be more uniformly coated in the emulsion, thereby further improving the emulsification effect of the emulsion microcapsules on oils. As can be seen from the comparison of Examples 1 and Examples 26-30, the degreasing agent A prepared by the method of this application has significantly improved the degreasing performance of titanium strip rolls, reaching 100%. Considering all factors, Example 26 is the optimal solution.
Claims
1. A processing method for improving the stripping performance of a titanium strip coil, characterized by, The method comprises the following steps: S1, pre-degreasing The titanium strip coil is sequentially passed through a first alkali tank, a soaking tank, a second alkali tank, a rinsing tank, a third alkali tank and a cleaning tank for ultrasonic treatment for 5-10 minutes, to obtain a pre-degreased titanium strip coil; the alkali concentration of the first alkali tank is 3-5%, and then the alkali concentration of each tank is increased by 2.5-5%; the rinsing tank contains a solution obtained by mixing 15-20 g / L nitric acid and 30-50 g / L hydrofluoric acid at a mass ratio of 2-2.5:1; the alkali temperature is 15-30℃; The soaking tank contains water at a temperature of 40-50℃; the cleaning tank is provided with a spraying port at the top for spraying degreasing agent A at a temperature of 50-60℃, and a brush roller is rotatably arranged above the cleaning tank; S2, degreasing treatment S2-1, powder degreasing The gettering powder and the binder, the debinding agent A flowing out along the bottom of the titanium strip roll are mixed in a mass ratio of 0.3-0.5:0.05-0.1:1 to obtain a debinding agent B, and are evenly divided into 2-3 parts; then the titanium strip roll after pre-debinding is vertically placed, and one part of the debinding agent B is sprayed along the gap between the top layers of the titanium strip roll by using a high-pressure rotary spray nozzle for spray debinding; wherein the flow rate of the high-pressure nozzle is 1.5-2 m 3 / h, the nozzle pressure is 0.8-1.8 MPa, and the spray angle is 45-65°. S2-2, electrolytic degreasing The titanium strip coil is put into an electrolytic cell, the titanium strip coil serves as a cathode, an electrode plate serves as an anode, then electricity is passed, the electrolyte in the electrolytic cell is a potassium hydroxide solution with a molar concentration of 0.15-0.2 mol / L, for every 5-10 ℃ increase in the temperature of the electrolyte, 1 / 8-1 / 4 of the remaining degreasing agent B and 0.5-0.7% of a low-foaming surfactant based on the mass percentage of the degreasing agent B are added, and the temperature is kept for 5-7 min; after the degreasing agent B is added, the titanium strip coil is taken out and washed by spraying water with a pressure of 0.15-0.25 MPa and a temperature of 40-50 ℃; wherein the current in the electrolytic cell is 2400-2600 A, and the current density is 5-10 A / dm 2 ; S3, annealing treatment The electrolytic degreased titanium strip coil is sent into a vacuum furnace at 750-800℃, helium is passed in at a flow rate of 25-45m 3 / h for annealing, and after annealing, the strip is straightened by drawing. S4, flattening treatment The titanium strip coil after the tension-straightening treatment is subjected to surface flattening treatment, to obtain a flattened titanium strip coil.
2. The method of claim 1, wherein the titanium strip coil is lifted by a crane. In step S1, spherical cast steel sand with a particle size of 1-3 mm is used for shot blasting treatment during the rinsing process, the shot blasting speed is 40-200 m / min, the spraying angle is 30-50℃, the shot blasting sand amount is 600-800 Kg / min, and the shot blasting time is 30-120 s.
3. The processing method for improving the degreasing performance of titanium strip coils as described in claim 1, characterized in that, In step S1, the alkali solution in the first alkali tank, the second alkali tank and the third alkali tank is sodium hydroxide solution, and microwave-assisted heating is performed while the titanium strip coil is soaked in each alkali tank; the microwave power is 18-20 kW, the heating temperature is 25-40℃, and the microwave time is 5-25 min.
4. The processing method for improving the degreasing performance of titanium strip coils as described in claim 1, characterized in that, In step S1, the brush roller is one of a nylon brush roller, a non-woven fabric brush roller and a ceramic brush roller.
5. The processing method for improving the degreasing performance of titanium strip coils as described in claim 1, characterized in that, In step S1, the degreasing agent A comprises, by mass fraction: 2-5 parts of acetone, 0.5-3 parts of sodium carbonate, 8-12 parts of benzotriazole, 3-4 parts of emulsified microcapsules, 4-6 parts of penetrating agent JFC and 35-65 parts of deionized water. The emulsified microcapsules comprise, by mass percentage: 25-40% of resin microspheres, 2-8% of a sodium silicate solution with a concentration of 25-35 g / L, 10-20% of a white carbon black dispersant, 1-5% of dextrin, 1.5-2% of silica sol, 0.8-1.2% of a curing agent and the balance of water.
6. The method of claim 5, wherein the titanium strip coil is lifted by a crane. The preparation method of the emulsified microcapsules is as follows: The sodium silicate solution is equally divided into 2-3 parts, a composite solution A is obtained by uniformly mixing the silica sol, water and one part of the sodium silicate solution, then resin microspheres are added to the composite solution A at a solid-liquid ratio of 1:2.5-3 and ultrasonic dispersion is performed for 15-20 min to obtain a suspension C; The remaining sodium silicate solutions are sequentially added with the white carbon black dispersant and dextrin, stirred and uniformly mixed at 80-90℃ to obtain a composite solution B. The composite solution B is homogenized and emulsified by a homogenizer with a rotating speed of 8000-9000 rpm for 1-1.5 min, and then centrifuged at 1000-1500 rpm for 18-20 min to obtain an emulsion, and then the suspension C and the solidifying agent are mixed and added into the emulsion, and finally centrifugal spray drying is carried out at a rotating speed of 16000-18000 rpm for 10-20 min to obtain the emulsified microcapsules.
7. The method of claim 1, wherein the titanium strip coil is lifted by a crane. In step S2-1, the inhaled powder is one of titanium powder or zirconium powder, and the binder is polyformaldehyde.
8. The method of claim 1, wherein the titanium strip coil is lifted by a crane. In step S3, the elongation rate in the straightening process is 0.2-0.5%.
9. The method of claim 1, wherein the titanium strip coil is lifted by a crane.
9. The method of claim 1, wherein the titanium strip coil is lifted by a crane. In step S4, the surface flattening treatment adopts a continuous grinding and polishing machine group, and the process parameters are as follows: the running speed of the continuous grinding and polishing machine group is 5-7 m / min, and the grinding head sand belt mesh is 200-300 meshes.
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