A method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging

Abstract

This invention provides a method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, belonging to the field of ink preparation technology. This method incorporates rare earth water-resistant additives, including lanthanum adipic acid-aluminum complexes and aminourea adipic acid-aluminum complexes. The improved water resistance of the ink is primarily due to the chemical substances produced during the reaction interacting with water molecules, preventing water molecules from interacting with other components in the ink, thus preventing water molecule penetration and damage to the ink's structure; thereby enhancing the ink's water resistance. The room-temperature curing ink for pure aluminum foil pharmaceutical packaging prepared by this invention exhibits excellent adhesion to aluminum foil, provides strong and clear printing of text and patterns, rapid solvent release, good heat resistance, good gloss, and non-toxic pigments. It will not contaminate the packaged medicine due to the migration of chemical components within the ink.

Description

Technical Field

[0001] This invention relates to the field of ink preparation technology, and more specifically, to a method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging. Background Technology

[0002] PTP aluminum foil is mainly used for blister packaging in pharmaceutical packaging. Blister packaging is primarily made of polyvinyl chloride (PVC) sheets and 0.02mm thick aluminum foil. Blister packaging has become the most common packaging method for Western medicine tablets and capsules.

[0003] Currently, there are many types and brands of printing inks on the market. However, considering the printing process of pharmaceutical aluminum foil and the special requirements of pharmaceutical packaging, printing inks for aluminum foil must have good adhesion to the aluminum foil, ensure that printed text and patterns are firm and clear, release solvents quickly, have good heat resistance, excellent abrasion resistance, good gloss, and non-toxic pigments. The ink must not cause the migration of chemical components that could contaminate the packaged medicine. The practical viscosity should meet the requirements of the aluminum foil printing process.

[0004] Chinese Patent CN105602340B: A two-component high-temperature resistant pharmaceutical aluminum foil gravure ink comprises a resin binder, a curing agent, a pigment paste, and a diluent; wherein the resin binder is prepared by mixing the following components in the following weight ratio: 20-30% n-propyl acetate, 20-40% ethyl acetate, 5-10% methyl ethyl ketone, 15-25% ternary chloroacetic acid resin, 5-10% modified cellulose, 5-10% polyketide resin, and 1-3% fumed silica. This ink has the following advantages: it can be directly printed on the aluminum foil surface, and one-time drying saves energy and solvent consumption; no protective agent is needed after printing, ensuring the ink's heat resistance and adhesion; the ink layer printed on the aluminum foil surface has a high surface tension, greater than 40 dynes, allowing for subsequent surface printing; under heat sealing conditions of 250℃ and 0.4MPa, the ink layer on the aluminum foil surface does not exhibit plastic flow and still maintains strong adhesion to the aluminum foil.

[0005] Chinese Patent CN102732097B relates to the field of ink printing, specifically a method for preparing aluminum foil ink, comprising: a step of preparing a ternary chloroacetic acid resin solution; a step of preparing an acrylic resin solution; a step of preparing a polyketide resin solution; a step of mixing the above three resin solutions to obtain a polymer resin mixture; and a step of thoroughly mixing 15%-35% by mass of the polymer resin mixture, 0%-25% of dye, 35%-70% of organic solvent, and 1%-10% of additives to obtain the aluminum foil ink. Compared with existing technologies, the aluminum foil ink produced by this method has rapid solvent evaporation, very little odor, strong ink adhesion, excellent weather resistance, water resistance, abrasion resistance, and rubbing resistance. It is an ink with high transparency and high gloss, good leveling, strong transferability, and adaptability to various high-speed and low-speed machines.

[0006] Chinese Patent CN102286229B discloses a water-based aluminum foil ink using pure acrylic emulsion as a base material and its preparation method. The ink composition, by mass ratio, is as follows: 35-50% pure acrylic emulsion, 10-30% pigment, 5-30% deionized water, 5-20% ethanol, 3-5% triethylamine, 0-2% wetting agent, 0-2% defoamer, 0.1-0.5% leveling agent, 1-3% film-forming aid, and 0.3-1% adhesion promoter. The above raw materials are added to a reaction vessel according to the mass ratio, stirred at room temperature, and ground in a sand mill. The pH is then adjusted to 7.0-8.5 with 0-1% pH adjuster to obtain the water-based aluminum foil ink.

[0007] However, inks prepared with existing technology exhibit ink piling or peeling when printed on large areas of aluminum foil; the inks have poor water resistance, freeze resistance, and adhesion; printed text and patterns are unclear, have poor heat resistance, and are prone to fading. Summary of the Invention

[0008] The primary objective of this invention is to provide a room-temperature curing ink for pharmaceutical packaging made of pure aluminum foil, which exhibits excellent adhesion to aluminum foil, provides strong and clear printing of text and patterns, rapid solvent release, good heat resistance, good gloss, and non-toxic pigments.

[0009] The second objective of this invention is to provide a method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, which adds rare earth water-resistant additives to prevent water molecules from penetrating and damaging the structure of the ink, thereby improving the water resistance of the ink.

[0010] To achieve the above objectives, the present invention is implemented using the following technical solution:

[0011] A method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, comprising the following steps:

[0012] Weigh 10-20 parts by weight of color paste and add it to 70-100 parts by weight of resin binder. Stir for 20-50 minutes to obtain pure aluminum foil pharmaceutical packaging room temperature curing ink.

[0013] Furthermore, in another embodiment of the present invention, the method for preparing the color paste is as follows:

[0014] Weigh 25-40 parts of transparent yellow and add it to 30-50 parts of ethanol and 10-20 parts of butanol, stir well, and obtain the color paste.

[0015] Furthermore, in another embodiment of the present invention, the method for preparing the resin binder is as follows:

[0016] Weigh out 1-3 parts by weight of silicone resin binder, 5-10 parts of acrylic resin, 50-68 parts of cotton liquid, 0.5-2 parts of wax powder, 0.1-1 parts of rare earth water-resistant additive, 0.1-1 parts of polyamide resin, 0.1-1 parts of ethyl methacrylate resin, 2-7 parts of ethyl acetate, 0.5-2 parts of ethanol, 5-12 parts of acetone, and 0.1-1 parts of antioxidant liquid, and stir for 40-60 minutes to obtain the resin binder.

[0017] Furthermore, in another embodiment of the present invention, the silicone resin adhesive is KX-605 or AH-062.

[0018] Furthermore, in another embodiment of the present invention, the method for preparing the cotton solution is as follows:

[0019] Weigh 15-20 parts by weight of nitrocellulose and 16-22 parts by weight of ethanol and add them to the reaction vessel. Soak for 5-10 minutes, then add 18-24 parts by weight of toluene and 7-15 parts by weight of isopropanol. Stir for 20-40 minutes, then add 7-15 parts by weight of butyl acetate and 1-4 parts by weight of cyclohexanone. Continue stirring for 10-30 minutes to obtain the cotton solution.

[0020] Furthermore, in another embodiment of the present invention, the method for preparing the antioxidant liquid is as follows:

[0021] Weigh 7-15 parts by weight of antioxidant and add them to 60-90 parts by weight of toluene solvent. Stir until transparent to obtain antioxidant solution.

[0022] Furthermore, in another embodiment of the present invention, the antioxidant is 168, 1010, or 264.

[0023] Furthermore, in another embodiment of the present invention, the preparation method of the rare earth water-resistant additive is as follows:

[0024] D1: By weight, add 0.9-2.5 parts aluminum chloride, 1.6-3.2 parts L-2-aminohexanoic acid, 0.03-0.07 parts acetic acid, and 100-120 parts DMF to the reactor, purge with nitrogen, and stir at 50-70°C for 100-150 minutes.

[0025] D2: Add 0.003-0.03 parts of lanthanum acrylate and 2-4 parts of sodium tert-butoxide by weight, stir at 50-70℃ for 20-50 minutes, then add 12-23 parts of 4-propenylthioaminourea, keep warm and continue stirring for 20-50 minutes, and remove DMF by distillation to obtain rare earth water-resistant additives.

[0026] Reaction mechanism:

[0027] Aluminum chloride and L-2-aminoadipic acid form an aminoadipic acid-aluminum complex; the aminoadipic acid-aluminum complex undergoes an addition reaction with lanthanum acrylate under sodium tert-butoxide catalysis; the aminoadipic acid-aluminum complex undergoes an addition reaction with 4-propenylthioaminourea under sodium tert-butoxide catalysis; the two are mixed to obtain a rare earth water-resistant additive.

[0028] Technical effects:

[0029] The present invention provides a method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging. Compared with the prior art, the present invention has the following significant advantages:

[0030] 1. This invention adds rare earth water-resistant additives, including lanthanum adipic acid-aluminum complex and aminourea adipic acid-aluminum complex. The water resistance of the ink is improved mainly because the chemical substances produced by these additives in the reaction can interact with water molecules, preventing water molecules from interacting with other components in the ink, thereby preventing water molecules from penetrating and damaging the structure of the ink; thus improving the water resistance of the ink.

[0031] 2. The pure aluminum foil pharmaceutical packaging room temperature curing ink prepared by this invention has good adhesion to aluminum foil, prints text and patterns firmly and clearly, releases solvent quickly, has good heat resistance, good gloss, and the pigments are non-toxic. It will not contaminate the packaged medicine due to the migration of chemical components in the ink. Detailed Implementation

[0032] To make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are described clearly and completely below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer are used. Where the manufacturer of the reagents or instruments is not specified, all are conventional products that can be purchased commercially.

[0033] The following is a detailed description of the room-temperature curing ink for pure aluminum foil pharmaceutical packaging and its preparation method, according to embodiments of the present invention.

[0034] Example 1

[0035] A method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, comprising the following steps:

[0036] Weigh 10g of color paste and add it to 70g of resin binder. Stir for 20 minutes to obtain pure aluminum foil pharmaceutical packaging room temperature curing ink.

[0037] The method for preparing the color paste is as follows:

[0038] Weigh 25g of transparent yellow and add it to 30g of ethanol and 10g of butanol. Stir well to obtain a color paste.

[0039] The preparation method of the resin binder is as follows:

[0040] Weigh out 1g of silicone resin binder, 5g of acrylic resin, 50g of cotton liquid, 0.5g of wax powder, 0.1g of rare earth water-resistant additive, 0.1g of polyamide resin, 0.1g of ethyl methacrylate resin, 2g of ethyl acetate, 0.5g of ethanol, 5g of acetone, and 0.1g of antioxidant liquid, and stir for 40 minutes to obtain the resin binder.

[0041] The silicone resin adhesive is KX-605.

[0042] The method for preparing the cotton solution is as follows:

[0043] Weigh 15g of nitrocellulose and 16g of ethanol and add them to the reaction vessel. Soak for 5 minutes, then add 18g of toluene and 7g of isopropanol. Stir for 20 minutes, then add 7g of butyl acetate and 1g of cyclohexanone. Continue stirring for 10 minutes to obtain the cotton solution.

[0044] The method for preparing the antioxidant liquid is as follows:

[0045] Weigh 7g of antioxidant and add it to 60g of toluene solvent. Stir until transparent to obtain antioxidant solution.

[0046] The antioxidant mentioned is 168.

[0047] The preparation method of the rare earth water-resistant additive is as follows:

[0048] D1: Add 0.9g aluminum chloride, 1.6g L-2-aminohexanoic acid, 0.03g acetic acid, and 100g DMF to a reaction vessel, purge with nitrogen, and stir at 50°C for 100 minutes.

[0049] D2: Add 0.003g lanthanum acrylate and 2g sodium tert-butoxide, stir at 50℃ for 20 minutes, then add 12g 4-propenylthiourea, keep warm and continue stirring for 20 minutes, and distill to remove DMF to obtain rare earth water-resistant additive.

[0050] Example 2

[0051] A method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, comprising the following steps:

[0052] Weigh 13g of color paste and add it to 80g of resin binder. Stir for 30 minutes to obtain pure aluminum foil pharmaceutical packaging room temperature curing ink.

[0053] The method for preparing the color paste is as follows:

[0054] Weigh 30g of transparent yellow and add it to 35g of ethanol and 13g of butanol. Stir well to obtain a color paste.

[0055] The preparation method of the resin binder is as follows:

[0056] Weigh out 2g of silicone resin binder, 6g of acrylic resin, 55g of cotton liquid, 1g of wax powder, 0.5g of rare earth water-resistant additive, 0.5g of polyamide resin, 0.5g of ethyl methacrylate resin, 3g of ethyl acetate, 1g of ethanol, 7g of acetone, and 0.5g of antioxidant liquid, and stir for 45 minutes to obtain the resin binder.

[0057] The silicone resin adhesive is KX-605.

[0058] The method for preparing the cotton solution is as follows:

[0059] Weigh 16g of nitrocellulose and 18g of ethanol and add them to the reaction vessel. Soak for 6 minutes, then add 20g of toluene and 10g of isopropanol. Stir for 25 minutes, then add 10g of butyl acetate and 2g of cyclohexanone. Continue stirring for 15 minutes to obtain the cotton solution.

[0060] The method for preparing the antioxidant liquid is as follows:

[0061] Weigh 10g of antioxidant and add it to 70g of toluene solvent. Stir until transparent to obtain antioxidant solution.

[0062] The antioxidant mentioned is 1010.

[0063] The preparation method of the rare earth water-resistant additive is as follows:

[0064] D1: Add 1.6g aluminum chloride, 2.2g L-2-aminohexanoic acid, 0.2g acetic acid, and 105g DMF to the reaction vessel, purge with nitrogen, and stir at 55°C for 110 minutes.

[0065] D2: Add 0.01g lanthanum acrylate and 3g sodium tert-butoxide, stir at 55℃ for 30 minutes, then add 17g 4-propenylthiourea, keep warm and continue stirring for 30 minutes, and distill to remove DMF to obtain rare earth water-resistant additive.

[0066] Example 3

[0067] A method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, comprising the following steps:

[0068] Weigh 18g of color paste and add it to 90g of resin binder. Stir for 40 minutes to obtain pure aluminum foil pharmaceutical packaging room temperature curing ink.

[0069] The method for preparing the color paste is as follows:

[0070] Weigh 35g of transparent yellow and add it to 45g of ethanol and 180g of butanol. Stir well to obtain a color paste.

[0071] The preparation method of the resin binder is as follows:

[0072] Weigh out 2g of silicone resin binder, 9g of acrylic resin, 60g of cotton liquid, 1.5g of wax powder, 0.8g of rare earth water-resistant additive, 0.8g of polyamide resin, 0.18g of ethyl methacrylate resin, 6g of ethyl acetate, 1.5g of ethanol, 10g of acetone, and 0.8g of antioxidant liquid, and stir for 55 minutes to obtain the resin binder.

[0073] The silicone resin adhesive is AH-062.

[0074] The method for preparing the cotton solution is as follows:

[0075] Weigh 19g of nitrocellulose and 20g of ethanol and add them to the reaction vessel. Soak for 8 minutes, then add 22g of toluene and 13g of isopropanol. Stir for 35 minutes, then add 13g of butyl acetate and 3g of cyclohexanone. Continue stirring for 25 minutes to obtain the cotton solution.

[0076] The method for preparing the antioxidant liquid is as follows:

[0077] Weigh 13g of antioxidant and add it to 80g of toluene solvent. Stir until transparent to obtain antioxidant solution.

[0078] The antioxidant mentioned is 1010.

[0079] The preparation method of the rare earth water-resistant additive is as follows:

[0080] D1: Add 2.2g aluminum chloride, 2.8g L-2-aminohexanoic acid, 0.06g acetic acid, and 1150g DMF to a reaction vessel, purge with nitrogen, and stir at 65°C for 140 minutes.

[0081] D2: Add 0.02g lanthanum acrylate and 3g sodium tert-butoxide, stir at 65℃ for 40 minutes, then add 20g 4-propenylthiourea, keep warm and continue stirring for 40 minutes, and distill to remove DMF to obtain rare earth water-resistant additive.

[0082] Example 4

[0083] A method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, comprising the following steps:

[0084] Weigh 20g of color paste and add it to 100g of resin binder. Stir for 50 minutes to obtain pure aluminum foil pharmaceutical packaging room temperature curing ink.

[0085] The method for preparing the color paste is as follows:

[0086] Weigh 40g of transparent yellow and add it to 50g of ethanol and 20g of butanol. Stir well to obtain a color paste.

[0087] The preparation method of the resin binder is as follows:

[0088] Weigh out 3g of silicone resin binder, 10g of acrylic resin, 68g of cotton liquid, 2g of wax powder, 1g of rare earth water-resistant additive, 1g of polyamide resin, 1g of ethyl methacrylate resin, 7g of ethyl acetate, 2g of ethanol, 12g of acetone, and 1g of antioxidant liquid, and stir for 60 minutes to obtain the resin binder.

[0089] The silicone resin adhesive is AH-062.

[0090] The method for preparing the cotton solution is as follows:

[0091] Weigh 20g of nitrocellulose and 22g of ethanol and add them to the reaction vessel. Soak for 10 minutes, then add 24g of toluene and 15g of isopropanol. Stir for 40 minutes, then add 15g of butyl acetate and 4g of cyclohexanone. Continue stirring for 30 minutes to obtain the cotton solution.

[0092] The method for preparing the antioxidant liquid is as follows:

[0093] Weigh 15g of antioxidant and add it to 90g of toluene solvent. Stir until transparent to obtain antioxidant solution.

[0094] The antioxidant mentioned is 264.

[0095] The preparation method of the rare earth water-resistant additive is as follows:

[0096] D1: Add 2.5g aluminum chloride, 3.2g L-2-aminohexanoic acid, 0.07g acetic acid, and 120g DMF to a reaction vessel, purge with nitrogen, and stir at 70°C for 150 minutes.

[0097] D2: Add 0.03g lanthanum acrylate and 4g sodium tert-butoxide, stir at 70℃ for 50 minutes, then add 23g 4-propenylthiourea, keep warm and continue stirring for 50 minutes, and distill to remove DMF to obtain rare earth water-resistant additive.

[0098] Comparative Example 1

[0099] This example is identical to Example 1 except that no rare earth water-resistant additives are added.

[0100] Comparative Example 2

[0101] This example is identical to Example 1 except that L-2-aminohexanoic acid is not added.

[0102] Comparative Example 3

[0103] This example is identical to Example 1 except that 4-propenylthiourea is not added.

[0104] Example Evaluation Method:

[0105] Heat resistance test method: The ink is evenly coated on pure aluminum foil, and its adhesion is checked with polyester tape; its heat resistance is tested with a heat sealer at 230℃, 0.2MPa, and 1s.

[0106] Water resistance test method: Apply the ink evenly to pure aluminum foil, immerse it in water for 24 hours, rub it back and forth 100 times, and observe the surface condition of the ink.

[0107] Table 1 Evaluation Results of Examples

[0108] Water resistance Adhesion Heat resistance Example 1 The surface does not change color, fade, or lose color. It does not fall off or peel off. qualified Example 2 The surface does not change color, fade, or lose color. It does not fall off or peel off. qualified Example 3 The surface does not change color, fade, or lose color. It does not fall off or peel off. qualified Example 4 The surface does not change color, fade, or lose color. It does not fall off or peel off. qualified Comparative Example 1 Surface discoloration and fading Shedding Unqualified Comparative Example 2 Surface fading Partial peeling Unqualified Comparative Example 3 Surface fading Partial peeling Unqualified

[0109] Through comparison of the above embodiments and comparative examples, the rare earth water-resistant additive prepared by the present invention can effectively improve the water resistance of ink; the pure aluminum foil pharmaceutical packaging room temperature curing ink prepared by the present invention has good adhesion to aluminum foil, prints text and patterns firmly and clearly, and has good heat resistance.

[0110] The above are merely specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions, or modifications made based on the present invention to solve essentially the same technical problems and achieve essentially the same technical effects are all covered within the protection scope of the present invention.

Claims

1. A method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging, comprising the following steps: Weigh 10-20 parts by weight of color paste and add it to 70-100 parts by weight of resin binder. Stir for 20-50 minutes to obtain pure aluminum foil pharmaceutical packaging room temperature curing ink. The preparation method of the resin binder is as follows: Weigh out 1-3 parts by weight of silicone resin binder, 5-10 parts of acrylic resin, 50-68 parts of cotton liquid, 0.5-2 parts of wax powder, 0.1-1 parts of rare earth water-resistant additive, 0.1-1 parts of polyamide resin, 0.1-1 parts of ethyl methacrylate resin, 2-7 parts of ethyl acetate, 0.5-2 parts of ethanol, 5-12 parts of acetone, and 0.1-1 parts of antioxidant liquid, and stir for 40-60 minutes to obtain the resin binder. The method for preparing the cotton solution is as follows: Weigh 15-20 parts by weight of nitrocellulose and 16-22 parts by weight of ethanol and add them to the reaction vessel. Soak for 5-10 minutes, then add 18-24 parts by weight of toluene and 7-15 parts by weight of isopropanol. Stir for 20-40 minutes, then add 7-15 parts by weight of butyl acetate and 1-4 parts by weight of cyclohexanone. Continue stirring for 10-30 minutes to obtain cotton solution. The preparation method of the rare earth water-resistant additive is as follows: D1: By weight, add 0.9-2.5 parts aluminum chloride, 1.6-3.2 parts L-2-aminohexanoic acid, 0.03-0.07 parts acetic acid, and 100-120 parts DMF to the reactor, purge with nitrogen, and stir at 50-70°C for 100-150 minutes. D2: Add 0.003-0.03 parts of lanthanum acrylate and 2-4 parts of sodium tert-butoxide by weight, stir at 50-70℃ for 20-50 minutes, then add 12-23 parts of 4-propenylthioaminourea, keep warm and continue stirring for 20-50 minutes, and remove DMF by distillation to obtain rare earth water-resistant additives.

2. The method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging according to claim 1, characterized in that: The method for preparing the color paste is as follows: Weigh 25-40 parts of transparent yellow by weight and add it to 30-50 parts of ethanol and 10-20 parts of butanol. Stir well to obtain a color paste.

3. The method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging according to claim 1, characterized in that: The silicone resin adhesive is KX-605.

4. The method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging according to claim 1, characterized in that: The method for preparing the antioxidant liquid is as follows: Weigh 7-15 parts by weight of antioxidant and add them to 60-90 parts by weight of toluene solvent. Stir until transparent to obtain antioxidant solution.

5. The method for preparing a room-temperature curing ink for pure aluminum foil pharmaceutical packaging according to claim 4, characterized in that: The antioxidants mentioned are 168, 1010, and 264.