Grain refinement medicine foil based on multi-parameter composite regulation and control

Abstract

The invention discloses a grain refinement medicine foil based on multi-parameter composite regulation and control. A preparation method comprises the steps of raw material selection, casting, heat treatment, cold rolling, finished product annealing, surface treatment and the like. By accurately controlling alloy components, adding Fe, Si, Mg and aluminum-titanium-boron wires as grain refiners and combining semi-continuous casting and electromagnetic stirring technologies, grain refinement of the aluminum alloy is realized. In the heat treatment process, a homogenizing annealing and multi-stage heat treatment process is adopted, so that the strength and toughness of the material are further improved. In the cold rolling process, the technological parameters of primary rolling, intermediate annealing and finish rolling are optimized, so that the aluminum foil has good surface quality and dimensional precision. The surface treatment adopts alkali washing, acid pickling, passivation and coating treatment, and an epoxy resin coating is selected, so that the corrosion resistance of the aluminum foil and the adhesive force of the coating are remarkably improved. The medicine foil has excellent mechanical performance, corrosion resistance and surface quality, and is suitable for the fields of medicine packaging and the like. Through a multi-parameter composite regulation and control process, aluminum foil grains are remarkably refined, and the requirement of modern medicine packaging for high-performance materials is met.

Description

Technical Field

[0001] The invention relates to the field of preparation of medicine foil, and more specifically to a grain-refining medicine foil based on multi-parameter composite regulation. Background Art

[0002] Medicinal aluminum foil is an important material in the field of pharmaceutical packaging. It has good barrier properties, light-shielding properties and corrosion resistance, and can effectively protect drugs from the external environment. It is widely used in the packaging of tablets, capsules and other drugs. Traditional medicinal aluminum foil is usually made of pure aluminum or ordinary aluminum alloy. Although it has certain mechanical properties and protective functions, it still has deficiencies in grain refinement, strength and toughness, and it is difficult to meet the needs of modern pharmaceutical packaging for high performance, long-term storage and safety.

[0003] In practical applications, the degree of grain refinement of pharmaceutical packaging materials directly affects their mechanical properties and corrosion resistance. Grain-refined aluminum foil not only has better strength and toughness, but also can maintain high integrity and uniformity during the thinning process, thereby reducing material loss in pharmaceutical packaging. Therefore, it is of great significance to prepare a grain-refined pharmaceutical foil based on multi-parameter composite regulation. Summary of the invention

[0004] In order to solve the problems existing in the prior art, the present invention provides a grain-refining foil based on multi-parameter composite control, and the specific scheme is as follows:

[0005] A grain-refining foil based on multi-parameter composite control, specifically comprising the following steps:

[0006] S1. Raw material selection and alloy component control: Aluminum ingot is used as raw material, and alloy components are added and optimized to the following percentages: Fe 0.6-1.0%; Si 0.5-0.8%; Mg 0.05-0.1%; aluminum titanium boron wire is added;

[0007] S2, casting: the molten liquid aluminum is semi-continuously cast and electromagnetically stirred;

[0008] S3, heat treatment: including homogenization annealing and multi-stage heat treatment;

[0009] S4, cold rolling: including initial rolling, intermediate annealing and finishing rolling;

[0010] S5, finished product annealing;

[0011] S6. Surface treatment: Apply epoxy resin coating on the surface of aluminum foil.

[0012] Furthermore, the parameters of the semi-continuous casting in S2 are as follows: casting temperature is 720°C to 740°C; cooling rate is 15°C / s to 25°C / s; mold preheating temperature: 200°C to 250°C.

[0013] Furthermore, the parameters of electromagnetic stirring in S2 are: electromagnetic field intensity: 10mT to 50mT; stirring frequency: 10Hz to 50Hz; stirring time: 80% to 100% of the entire casting process.

[0014] Furthermore, the annealing temperature is 480°C to 520°C; the holding time is 12 hours to 24 hours; the furnace is cooled to 300°C and then air-cooled.

[0015] Furthermore, the multi-stage heat treatment process in S3 includes a first-stage heat treatment and a second-stage heat treatment; the first-stage heat treatment parameters are a temperature of 350°C, a holding time of 2 hours, and then rapid cooling to room temperature; the second-stage heat treatment parameters are a temperature of 280°C, a holding time of 4 hours, and then slow cooling to room temperature.

[0016] Further, the cold rolling in S4 includes the following steps:

[0017] S401, initial rolling: the initial rolling temperature is room temperature; the reduction rate is 30% to 50%; the rolling speed is 10m / min to 20m / min;

[0018] S402, intermediate annealing: annealing temperature is 300℃~350℃; holding time is 2 hours~4 hours; cooling method is air cooling;

[0019] S403, finishing rolling: the finishing rolling temperature is room temperature; the reduction rate is 60-80%; the finishing speed is controlled at 20m / min-30m / min.

[0020] Furthermore, the parameters of the finished product annealing in S5 are: annealing temperature: 180°C to 220°C; holding time controlled to be 1 to 3 hours; cooling method is cooling in air.

[0021] Furthermore, S6 further includes the following steps:

[0022] S601, surface pretreatment: use 2% to 5% sodium hydroxide solution for alkaline washing, the temperature is controlled at 60℃ to 80℃, and the washing time is 1 to 3 minutes; use deionized water to thoroughly rinse the surface residue; then carry out acid washing, use 5% to 10% nitric acid solution, the temperature is controlled at 20℃ to 40℃, and the acid washing time is 30 to 90 seconds; rinse again with deionized water to ensure that there is no residual chemical substance on the surface;

[0023] S602, surface passivation treatment: using a passivation solution containing chromate and zirconium, the solution temperature is controlled at 20°C to 30°C, and the treatment time is 30 to 120 seconds; after passivation, it is washed with deionized water and then dried, the drying temperature is controlled at 80°C to 100°C, and the drying time is 2 to 5 minutes;

[0024] S603, coating preparation: select coating materials containing epoxy resin, and control the coating thickness to 1 to 5 microns; use solvent or water-based diluent to adjust the coating to a viscosity of 20 to 30 seconds;

[0025] S604, coating process: use roller coating or spraying to coat evenly, the coating speed is controlled at 50-150 m / min; the coating environment temperature is 20℃-25℃, and the humidity is controlled at 50%-70%;

[0026] S605, coating curing: the coating curing temperature is controlled at 150℃~200℃, and the curing time is 2~5 minutes to ensure that the coating is completely cured.

[0027] Beneficial effects:

[0028] The present invention provides a grain-refining foil based on multi-parameter composite control, which specifically includes the following advantages:

[0029] (1) By adopting precise alloy composition design combined with semi-continuous casting and electromagnetic stirring processes, the present invention can significantly refine the grain structure of aluminum alloy. Grain refinement enables aluminum foil to exhibit higher strength and toughness in mechanical properties, especially to maintain good integrity during thinning processing, effectively reducing material loss.

[0030] (2) After multi-stage heat treatment process optimization including homogenization annealing and two-stage heat treatment, the internal stress of the pharmaceutical aluminum foil is released and the grains are uniformly refined. This process makes the aluminum foil not only have good tensile strength and ductility, but also have excellent tear resistance, which can adapt to the multiple rolling and forming requirements required in the pharmaceutical packaging process.

[0031] (3) Through reasonable composition control and electromagnetic stirring process, the surface density and uniformity of aluminum alloy are significantly improved, which greatly enhances the corrosion resistance of pharmaceutical aluminum foil. In the subsequent surface passivation treatment and epoxy resin coating application, the coating and the substrate are more closely combined, which can effectively resist the corrosion of aluminum foil by chemical components in medicines and extend the service life of packaging materials.

[0032] (4) During the surface treatment process, the precise control of the pretreatment process and the passivation treatment ensures the cleanliness and activity of the aluminum foil surface, so that the coating material can be evenly attached to the aluminum foil surface. The applied epoxy resin coating not only has uniform thickness, but also has an adhesion that reaches the industry's high standards after curing, which can effectively improve the barrier and protective properties of the pharmaceutical aluminum foil.

[0033] (5) The precise control of the cold rolling process enables the thickness and surface quality of the aluminum foil to be stably controlled, avoiding the surface defect problem that occurs in the traditional aluminum foil during multiple rolling processes. At the same time, the processing parameters of the aluminum foil in the initial rolling, intermediate annealing and finishing rolling are optimized to ensure the reduction rate and rolling speed in each stage, and finally produce a pharmaceutical aluminum foil with consistent thickness and smooth surface. DETAILED DESCRIPTION

[0034] In order to deepen the understanding of the present invention, the present invention will be further described in detail below in conjunction with examples. The examples are only used to explain the present invention and do not constitute a limitation on the protection scope of the present invention.

[0035] Embodiment 1:

[0036] S1 Raw material selection and alloy composition control:

[0037] AA8011 series aluminum alloy was selected as the substrate, with the composition of Fe 0.8%, Si 0.7%, Mg 0.08%, and aluminum titanium boron wire accounting for 0.02% of the aluminum weight was added to enhance the grain refinement effect.

[0038] S2 Casting:

[0039] The aluminum alloy was melted and maintained at 730°C. Semi-continuous casting was used in the casting process, the cooling rate was controlled at 20°C / s, and the mold preheating temperature was 230°C.

[0040] The electromagnetic stirring parameters are: electromagnetic field intensity of 30 mT, stirring frequency of 30 Hz, and stirring time of 90% of the casting process.

[0041] S3 heat treatment:

[0042] First, homogenization annealing is performed at 500°C for 20 hours, then the furnace is cooled to 300°C and then air-cooled to room temperature.

[0043] Then a two-stage heat treatment is carried out. The first stage is kept at 350°C for 2 hours and then quickly cooled. The second stage is kept at 280°C for 4 hours and then slowly cooled to room temperature.

[0044] S4 Cold Rolled:

[0045] Initial rolling: Initial rolling was carried out at room temperature with a reduction rate of 40% and a rolling speed of 15 m / min.

[0046] Intermediate annealing: annealing temperature is 320℃, keep warm for 3 hours, cooling method is air cooling.

[0047] Finish rolling: Finish rolling was carried out at room temperature with a reduction rate of 70% and a rolling speed of 25 m / min.

[0048] S5 finished product annealing:

[0049] The annealing temperature was 200°C for 2 hours and then air-cooled to room temperature.

[0050] S6 Surface Treatment:

[0051] S601 surface pretreatment: use 3% sodium hydroxide solution, the temperature is 70℃, the cleaning time is 2 minutes. Pickling uses 7% nitric acid solution, the pickling temperature is 30℃, and the pickling time is 60 seconds.

[0052] S602 surface passivation treatment: using chromate solution, temperature 25℃, treatment time 60 seconds. Drying temperature is 90℃, drying time is 3 minutes.

[0053] S603 coating preparation: Select coating materials containing epoxy resin, the coating thickness is controlled at 3 microns, and the viscosity is 25 seconds (measured by Ford Cup No. 4).

[0054] S604 coating process: roller coating, coating speed is 100 m / min, ambient temperature is controlled at 22°C, humidity is 60%.

[0055] S605 coating curing: curing temperature is 180℃, curing time is 3 minutes.

[0056] Embodiment 2:

[0057] S1 Raw material selection and alloy composition control:

[0058] AA8021 aluminum alloy was selected, with the alloy composition of Fe 0.9%, Si 0.6%, Mg 0.06%, and aluminum titanium boron wire (0.03%) was added to improve the alloy grain structure.

[0059] S2 Casting:

[0060] The aluminum liquid temperature is controlled at 740℃, semi-continuous casting is adopted, the cooling rate is 25℃ / s, and the mold preheating temperature is 240℃.

[0061] The electromagnetic stirring parameters are: electromagnetic field intensity 40 mT, stirring frequency 40 Hz, and stirring time 95% of the entire casting process.

[0062] S3 Heat Treatment**:

[0063] The homogenization annealing temperature is 510°C, which is kept at this temperature for 24 hours and then furnace cooled to 300°C and then air cooled to room temperature.

[0064] The first stage heat treatment is kept at 350°C for 2 hours and then quickly cooled to room temperature; the second stage heat treatment is kept at 280°C for 4 hours and then slowly cooled.

[0065] S4 Cold Rolled:

[0066] Initial rolling: carried out at room temperature, with a reduction rate of 45% and a rolling speed of 12m / min.

[0067] Intermediate annealing: annealing temperature is 330℃, keep warm for 4 hours, and cool in air.

[0068] Finish rolling: the reduction ratio is 75%, the rolling speed is 30 m / min, and it is carried out at room temperature.

[0069] S5 finished product annealing:

[0070] The annealing temperature is 210°C, the temperature is kept for 2 hours, and the cooling method is air cooling.

[0071] S6 Surface Treatment:

[0072] S601 surface pretreatment: Use 2% sodium hydroxide solution at 65°C for 1 minute. Acid pickling uses 5% nitric acid solution at 25°C for 45 seconds.

[0073] S602 surface passivation treatment: zirconium passivation solution is used, the temperature is controlled at 25℃, the treatment time is 90 seconds. The drying temperature is 85℃, and the drying time is 4 minutes.

[0074] S603 coating preparation: coating material is epoxy resin, thickness 4 microns, viscosity 30 seconds (Ford Cup No. 4)

[0075] S604 coating process: spray coating, coating speed controlled at 80 m / min, ambient temperature 24°C, humidity 55%.

[0076] S605 coating curing: curing temperature is 190℃, curing time is 4 minutes.

[0077] Embodiment 3:

[0078] S1. Raw material selection and alloy composition control:

[0079] AA8011 aluminum alloy is used, with a composition of Fe 0.7%, Si 0.8%, and Mg 0.1%, and aluminum-titanium-boron wire (0.015%) is added to improve the alloy's grain refinement performance.

[0080] S2 Casting:

[0081] The molten aluminum temperature is 725°C, the semi-continuous casting process, the cooling rate is 18°C / s, and the mold preheating temperature is 220°C.

[0082] The electromagnetic stirring parameters are: electromagnetic field intensity 20 mT, stirring frequency 20 Hz, and stirring time 85% of the casting process.

[0083] S3 heat treatment:

[0084] The homogenization annealing temperature is 490°C, and after keeping at this temperature for 18 hours, the furnace is cooled to 300°C and then air-cooled.

[0085] The first stage heat treatment is kept at 350°C for 2 hours and then quickly cooled to room temperature; the second stage heat treatment is kept at 280°C for 4 hours and then slowly cooled to room temperature.

[0086] S4 Cold Rolled:

[0087] Initial rolling: carried out at room temperature, with a reduction rate of 50% and a rolling speed of 18m / min.

[0088] Intermediate annealing: annealing temperature is 310℃, keep warm for 3 hours, and use air cooling.

[0089] Finishing rolling: the reduction rate is 80%, and the finishing speed is 28m / min.

[0090] S5 finished product annealing:

[0091] The annealing temperature is 190°C, kept for 3 hours, and then air-cooled.

[0092] S6 Surface Treatment:

[0093] S601 surface pretreatment: Use 4% sodium hydroxide solution at 75°C for 3 minutes. Pickling uses 10% nitric acid solution at 35°C for 90 seconds.

[0094] S602 surface passivation treatment: using chromate solution, temperature 30℃, treatment time 60 seconds, drying temperature 95℃, time 3 minutes.

[0095] S603 coating preparation: The coating material is epoxy resin, with a thickness of 5 microns and a viscosity of 20 seconds;

[0096] S604 coating process: roller coating is adopted, the coating speed is controlled at 90 m / min, the ambient temperature is 23°C, and the humidity is 65%.

[0097] S605 coating curing: curing temperature is 200℃, curing time is 5 minutes.

[0098] As a further improvement, the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A grain-refining foil based on multi-parameter composite control, characterized in that: The preparation method of the medicine foil specifically comprises the following steps: S1. Raw material selection and alloy component control: Aluminum ingot is used as raw material, and alloy components are added and optimized to the following percentages: Fe 0.6-1.0%; Si 0.5-0.8%; Mg 0.05-0.1%; aluminum titanium boron wire is added; S2, casting: the molten liquid aluminum is semi-continuously cast and electromagnetically stirred; S3, heat treatment: including homogenization annealing and multi-stage heat treatment; S4, cold rolling: including initial rolling, intermediate annealing and finishing rolling; S5, finished product annealing; S6. Surface treatment: Apply epoxy resin coating on the surface of aluminum foil.

2. The grain-refining foil based on multi-parameter composite control according to claim 1 is characterized in that: The parameters of the semi-continuous casting in S2 are as follows: the casting temperature is 720°C to 740°C; the cooling rate is 15°C / s to 25°C / s; and the mold preheating temperature is 200°C to 250°C.

3. The grain-refining foil based on multi-parameter composite control according to claim 1 is characterized in that: The parameters of electromagnetic stirring in S2 are: electromagnetic field intensity: 10mT to 50mT; stirring frequency: 10Hz to 50Hz; stirring time: 80% to 100% of the entire casting process.

4. The grain-refining foil based on multi-parameter composite control according to claim 1 is characterized in that: Annealing temperature: 480℃~520℃; Holding time: 12 hours~24 hours; Cool in the furnace to 300℃ and then air cool.

5. The grain-refining foil based on multi-parameter composite control according to claim 1 is characterized in that: The multi-stage heat treatment process in S3 includes a first stage heat treatment and a second stage heat treatment; the first stage heat treatment parameters are a temperature of 350°C, a holding time of 2 hours, and then rapid cooling to room temperature; the second stage heat treatment parameters are a temperature of 280°C, a holding time of 4 hours, and then slow cooling to room temperature.

6. The grain-refining foil based on multi-parameter composite control according to claim 1 is characterized in that: The cold rolling in S4 includes the following steps: S401, initial rolling: the initial rolling temperature is room temperature; the reduction rate is 30% to 50%; the rolling speed is 10m / min to 20m / min; S402, intermediate annealing: annealing temperature is 300℃~350℃; holding time is 2 hours~4 hours; cooling method is air cooling; S403, finishing rolling: the finishing rolling temperature is room temperature; the reduction rate is 60-80%; the finishing speed is controlled at 20m / min-30m / min.

7. The grain-refining foil based on multi-parameter composite control according to claim 1 is characterized in that: The parameters for the finished product annealing in S5 are: annealing temperature of 180°C to 220°C; holding time controlled to be 1 to 3 hours; and cooling method is cooling in air.

8. The grain-refining foil based on multi-parameter composite control according to claim 1 is characterized in that: S6 further includes the following steps: S601, surface pretreatment: use 2% to 5% sodium hydroxide solution for alkaline washing, the temperature is controlled at 60℃ to 80℃, and the washing time is 1 to 3 minutes; use deionized water to thoroughly rinse the surface residue; then carry out acid washing, use 5% to 10% nitric acid solution, the temperature is controlled at 20℃ to 40℃, and the acid washing time is 30 to 90 seconds; rinse again with deionized water to ensure that there is no residual chemical substance on the surface; S602, surface passivation treatment: using a passivation solution containing chromate and zirconium, the solution temperature is controlled at 20°C to 30°C, and the treatment time is 30 to 120 seconds; after passivation, it is washed with deionized water and then dried, the drying temperature is controlled at 80°C to 100°C, and the drying time is 2 to 5 minutes; S603, coating preparation: select coating materials containing epoxy resin, and control the coating thickness to 1 to 5 microns; use solvent or water-based diluent to adjust the coating to a viscosity of 20 to 30 seconds; S604, coating process: use roller coating or spraying to coat evenly, the coating speed is controlled at 50-150 m / min; the coating environment temperature is 20℃-25℃, and the humidity is controlled at 50%-70%; S605, coating curing: the coating curing temperature is controlled at 150℃~200℃, and the curing time is 2~5 minutes to ensure that the coating is completely cured.