A peel-off anti-counterfeiting label and its manufacturing method
By using a specially formulated hot melt adhesive and composite process in anti-counterfeiting labels, the problems of insufficient adhesion, heat resistance and water resistance of existing anti-counterfeiting labels are solved, and the labels can still maintain good adhesion at high temperatures and underwater.
Patent Information
- Application Number
- CN202311314352.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-11
- Publication Date
- 2025-09-05
- Estimated Expiration
- 2043-10-11
AI Technical Summary
Existing anti-counterfeiting labels have poor adhesion to the objects they are attached to, and are insufficiently stable in terms of heat and water resistance, which affects their efficiency.
Printing equipment is used to perform color printing on the front side of the substrate surface, and a hot laminating machine is used to cover it with BOPP pre-coated film to form an oil layer and an anti-counterfeiting layer. Hot melt adhesive is applied by hot melt adhesive coating equipment, and the adhesive layer and the anti-counterfeiting layer are compounded. A specifically formulated hot melt adhesive is used, including EVA, a modified adjuster modified with doped flaky graphene, a rare earth-blended silane modifier, etc., to optimize the label's adhesion and heat resistance and waterproof stability.
After peeling off the surface layer of the printed material, the variable data information on the back can be clearly attached, with better adhesion. The product can still remain stable at high temperatures and underwater, and has high efficiency in use.
Smart Images

Figure CN117360104B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of anti-counterfeiting labels, and in particular to a peel-off anti-counterfeiting label and a manufacturing method thereof. Background Art
[0002] Anti-counterfeiting labels are labels that can be attached, printed, or transferred to the surface or packaging of labeled items, as well as to attached items (such as product tags, business cards, and security cards). Existing anti-counterfeiting labels have poor adhesion to the items they are attached to, and their heat and water resistance are poor, affecting their effectiveness. This present invention addresses these issues by further improving them. Summary of the Invention
[0003] In view of the defects of the prior art, the purpose of the present invention is to provide a peel-off anti-counterfeiting label and a manufacturing method thereof to solve the problems raised in the above background technology.
[0004] The present invention solves the technical problem by adopting the following technical solutions:
[0005] The present invention provides a method for manufacturing a peelable anti-counterfeiting label, comprising the following steps:
[0006] Step 1: Use printing equipment to print color on the front side of the substrate to form a printed coating, and then use a hot laminating machine to coat a layer of BOPP pre-coated film on the back side of the substrate;
[0007] Step 2: Apply oil to the bottom of the BOPP pre-coated film on the glazing equipment to form an oil layer;
[0008] Step 3: Spray mirrored variable data on the lower part of the oil layer on a digital printing press, and then print a color mirrored pattern on the printing press to form an anti-counterfeiting layer;
[0009] Step 4: Use hot melt adhesive coating equipment to apply hot melt adhesive to the surface paper of the substrate to form an adhesive layer;
[0010] The hot melt adhesive comprises the following raw materials in parts by weight:
[0011] 45-55 parts of EVA, 12-18 parts of modified stabilizer of doped flake graphene, 6-10 parts of rare earth blended silane modifier, 4-7 parts of rosin resin, 2-4 parts of paraffin wax, and 1-3 parts of antioxidant;
[0012] The front side of the adhesive layer is compounded with the anti-counterfeiting layer, and the back side of the adhesive layer is compounded with the glassine base paper to obtain the label of the present invention.
[0013] Preferably, the oil agent is prepared by mixing FS-UV100, FS-UV800 and silicone oil in a weight ratio of 4:1:0.1.
[0014] Preferably, the antioxidant is BHT; the VA content in the EVA is 28-32%; and the melt index of the EVA is 25-30 g / 10 min.
[0015] Preferably, the preparation method of the film modifier is:
[0016] The doped flaky graphene modified adjusting agent and rare earth blended silane modifier are first stirred and mixed, then washed with water and dried, and the dried product is added together with EVA, rosin resin, paraffin and antioxidant into a mixer for mixing at a mixing temperature of 90-95°C for 5-10 minutes, and then extruded into an extruder at an extrusion temperature of 120-130°C. After the extrusion is completed, the film modifier is obtained by cooling.
[0017] Preferably, the preparation method of the doped flake graphene modified adjusting agent is:
[0018] S01: mixing sodium lignin sulfonate and a phosphate buffer solution having a pH value of 5.0 at a weight ratio of 4:1 to obtain a mixture;
[0019] S02: The mixture is then added to deionized water at a weight ratio of 1:5, followed by addition of a 6% chitosan solution (4-8% by weight) and stearic acid (1-3% by weight) to the total amount of the mixture, and stirred thoroughly to obtain a pre-adjusted solution;
[0020] S03: The flake graphene is preheated at 48-52° C. for 5-10 minutes, and then ultrasonically modified in a pre-adjusted solution that is 5-10 times the total amount of the flake graphene. After the treatment is completed, the flake graphene is washed with water and dried to obtain a modified flake graphene agent;
[0021] S04: The modified flaky graphene agent and the doped silicon carbide whisker agent are ball milled in a ball mill at a weight ratio of (7-8):3 at a ball milling speed of 1000-1500 r / min for 1-2 hours. After the ball milling is completed, the agent is washed with water and dried to obtain a modified flaky graphene agent.
[0022] Preferably, the ultrasonic improvement treatment has an ultrasonic power of 350-400W and an ultrasonic time of 1-2h.
[0023] Preferably, the preparation method of the doped silicon carbide whisker agent is:
[0024] 4-7 parts of silicon carbide whiskers and 2-5 parts of lanthanum sulfate solution are added to 10-15 parts of sodium citrate solution, and then 1-3 parts of sodium ethylenediamine ethanesulfonate and 2-4 parts of nano-silica sol are added, and stirred to obtain a doped silicon carbide whisker agent.
[0025] Preferably, the mass fraction of the lanthanum sulfate solution is 3-5%; the mass fraction of the sodium citrate solution is 15-20%.
[0026] Preferably, the preparation method of the rare earth blended silane modifier is:
[0027] S101: adding 3-5 parts of yttrium nitrate solution and 2-4 parts of silane coupling agent to 8-12 parts of ethanol solvent and mixing them evenly, then adding 1-3 parts of sodium dodecylbenzenesulfonate and stirring to obtain a modifier;
[0028] S102: Wollastonite is first dispersed evenly in a 2% by mass hydrochloric acid solution, then washed with water and dried. 5-8 parts of the dried wollastonite is then added to the S101 modifier and stirred thoroughly to obtain a rare earth blended silane modifier.
[0029] Preferably, the mass fraction of the yttrium nitrate solution is 2-5%; and the silane coupling agent is silane coupling agent KH560.
[0030] The present invention also provides a peel-away anti-counterfeiting label manufactured by a manufacturing method thereof.
[0031] Compared with the prior art, the present invention has the following beneficial effects:
[0032] The present invention realizes a self-adhesive label by independently synthesizing label materials and glazing with a special formula oil. After the surface layer of the printed substrate is peeled off, the surface layer of the printed substrate is immediately destroyed and cannot be restored. The variable data printed graphic information on the back can be clearly and completely attached to the object being attached. The anti-counterfeiting layer with variable graphics on the back has better adhesion to the object being attached. The product has heat resistance and waterproof stability. The anti-counterfeiting layer with variable graphics on the back still has good adhesion under high temperature and water immersion conditions, and the product has high use efficiency.
[0033] The hot melt adhesive used in the present invention is prepared by mutually blending EVA, rosin resin, paraffin, a setting agent modified by doping flaky graphene, and a rare earth-adjusted silane modifier, which can optimize the adhesion of label products and improve the heat resistance and waterproof stability of the products. The setting agent modified by doping flaky graphene, the rare earth-adjusted silane modifier and the two are coordinated with each other and work together to significantly improve the performance of the product. The setting agent modified by doping flaky graphene is formulated with sodium lignin sulfonate, phosphate buffer solution, chitosan solution and stearic acid, and then the graphene is preheated and the raw materials in the pre-adjusted liquid are coordinated and coordinated to optimize the ball milling improvement effect of the graphene and the doped silicon carbide whisker agent, thereby further synergizing the raw materials and enhancing the performance of the product through the flaky stone. Graphene and whisker-like structures are matched with each other and distributed in the system to support the system structure and improve the stability of the system structure. At the same time, through the mutual coordination between silicon carbide whiskers, lanthanum sulfate solution, sodium citrate solution, sodium ethylenediamine ethanesulfonate and nano-silica sol, through the mutual synergy between the raw materials, the joint combination, the synergistic effect of doped silicon carbide whisker agent and graphene is enhanced, the adhesion of the label product is optimized, and the heat resistance and waterproof stability of the product are improved; the synergy of wollastonite treated with hydrochloric acid solution is improved by the modifier composed of yttrium nitrate solution, silane coupling agent and sodium dodecylbenzenesulfonate, and the synergistic effect of the modified adjusting agent modified with doped flaky graphene can be further enhanced in the improved wollastonite reinforcement system, thereby further improving the performance of the product system. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Figure 1 Schematic diagram of the layered structure of the anti-counterfeiting label of the present invention. DETAILED DESCRIPTION
[0035] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0036] A method for manufacturing a peelable anti-counterfeiting label according to this embodiment includes the following steps:
[0037] Step 1: Use a printing device to perform color printing on the front side of the substrate surface layer 6 to form a printed coating 7, and then use a hot laminating machine to coat a layer of BOPP pre-coated film 5 on the back side of the substrate surface layer 6;
[0038] Step 2: Apply oil to the bottom of the BOPP pre-coated film on a glazing device to form an oil layer 4;
[0039] Step 3: spraying mirrored variable data on the lower part of the oil layer 4 on a digital printing press, and then printing a color mirrored pattern on the printing press to form the anti-counterfeiting layer 3;
[0040] Step 4: Use hot melt adhesive coating equipment to apply hot melt adhesive to the surface paper of the substrate to form adhesive layer 2;
[0041] The hot melt adhesive comprises the following raw materials in parts by weight:
[0042] 45-55 parts of EVA, 12-18 parts of modified stabilizer of doped flake graphene, 6-10 parts of rare earth blended silane modifier, 4-7 parts of rosin resin, 2-4 parts of paraffin wax, and 1-3 parts of antioxidant;
[0043] The front side of the adhesive layer 2 is compounded with the anti-counterfeiting layer 3, and the back side of the adhesive layer 2 is compounded with the glassine backing paper 1 to obtain the label of the present invention.
[0044] The oil agent of this embodiment is prepared by mixing FS-UV100, FS-UV800 and silicone oil in a weight ratio of 4:1:0.1.
[0045] The antioxidant in this embodiment is BHT; the VA content in the EVA is 28-32%; and the melt index of the EVA is 25-30 g / 10 min.
[0046] The preparation method of the film modifier of this embodiment is:
[0047] The doped flaky graphene modified adjusting agent and rare earth blended silane modifier are first stirred and mixed, then washed with water and dried, and the dried product is added together with EVA, rosin resin, paraffin and antioxidant into a mixer for mixing at a mixing temperature of 90-95°C for 5-10 minutes, and then extruded into an extruder at an extrusion temperature of 120-130°C. After the extrusion is completed, the film modifier is obtained by cooling.
[0048] The preparation method of the modified doped graphene sheet of this embodiment is as follows:
[0049] S01: mixing sodium lignin sulfonate and a phosphate buffer solution having a pH value of 5.0 at a weight ratio of 4:1 to obtain a mixture;
[0050] S02: The mixture is then added to deionized water at a weight ratio of 1:5, followed by addition of a 6% chitosan solution (4-8% by weight) and stearic acid (1-3% by weight) to the total amount of the mixture, and stirred thoroughly to obtain a pre-adjusted solution;
[0051] S03: The flake graphene is preheated at 48-52° C. for 5-10 minutes, and then ultrasonically modified in a pre-adjusted solution that is 5-10 times the total amount of the flake graphene. After the treatment is completed, the flake graphene is washed with water and dried to obtain a modified flake graphene agent;
[0052] S04: The modified flaky graphene agent and the doped silicon carbide whisker agent are ball milled in a ball mill at a weight ratio of (7-8):3 at a ball milling speed of 1000-1500 r / min for 1-2 hours. After the ball milling is completed, the agent is washed with water and dried to obtain a modified flaky graphene agent.
[0053] The ultrasonic power of the ultrasonic improvement treatment in this embodiment is 350-400W, and the ultrasonic time is 1-2h.
[0054] The preparation method of the doped silicon carbide whisker agent of this embodiment is:
[0055] 4-7 parts of silicon carbide whiskers and 2-5 parts of lanthanum sulfate solution are added to 10-15 parts of sodium citrate solution, and then 1-3 parts of sodium ethylenediamine ethanesulfonate and 2-4 parts of nano-silica sol are added, and stirred to obtain a doped silicon carbide whisker agent.
[0056] The mass fraction of the lanthanum sulfate solution in this embodiment is 3-5%; the mass fraction of the sodium citrate solution is 15-20%.
[0057] The preparation method of the rare earth blended silane modifier of this embodiment is as follows:
[0058] S101: adding 3-5 parts of yttrium nitrate solution and 2-4 parts of silane coupling agent to 8-12 parts of ethanol solvent and mixing them evenly, then adding 1-3 parts of sodium dodecylbenzenesulfonate and stirring to obtain a modifier;
[0059] S102: Wollastonite is first dispersed evenly in a 2% by mass hydrochloric acid solution, then washed with water and dried. 5-8 parts of the dried wollastonite is then added to the S101 modifier and stirred thoroughly to obtain a rare earth blended silane modifier.
[0060] The mass fraction of the yttrium nitrate solution in this embodiment is 2-5%; the silane coupling agent is silane coupling agent KH560.
[0061] The peel-away anti-counterfeiting label is manufactured by a manufacturing method of a peel-away anti-counterfeiting label in this embodiment.
[0062] Example 1.
[0063] A method for manufacturing a peelable anti-counterfeiting label according to this embodiment includes the following steps:
[0064] Step 1: Use a printing device to perform color printing on the front side of the substrate surface layer 6 to form a printed coating 7, and then use a hot laminating machine to coat a layer of BOPP pre-coated film 5 on the back side of the substrate surface layer 6;
[0065] Step 2: Apply oil to the bottom of the BOPP pre-coated film on a glazing device to form an oil layer 4;
[0066] Step 3: spraying mirrored variable data on the lower part of the oil layer 4 on a digital printing press, and then printing a color mirrored pattern on the printing press to form the anti-counterfeiting layer 3;
[0067] Step 4: Use hot melt adhesive coating equipment to apply hot melt adhesive to the surface paper of the substrate to form adhesive layer 2;
[0068] The hot melt adhesive comprises the following raw materials in parts by weight:
[0069] 45 parts of EVA, 12 parts of a modified stabilizer of doped flake graphene, 6 parts of a rare earth blended silane modifier, 4 parts of rosin resin, 2 parts of paraffin wax, and 1 part of an antioxidant;
[0070] The front side of the adhesive layer 2 is compounded with the anti-counterfeiting layer 3, and the back side of the adhesive layer 2 is compounded with the glassine backing paper 1 to obtain the label of the present invention.
[0071] The oil agent of this embodiment is prepared by mixing FS-UV100, FS-UV800 and silicone oil in a weight ratio of 4:1:0.1.
[0072] The antioxidant in this embodiment is BHT; the VA content in the EVA is 28%; and the melt index of the EVA is 25 g / 10 min.
[0073] The preparation method of the film modifier of this embodiment is:
[0074] The doped flaky graphene modified adjusting agent and rare earth blended silane modifier are first stirred and mixed, then washed with water and dried, and the dried product is added together with EVA, rosin resin, paraffin and antioxidant into a mixer for mixing at a mixing temperature of 90°C for 5 minutes, and then extruded into an extruder at an extrusion temperature of 120°C. After the extrusion is completed, the film modifier is obtained by cooling.
[0075] The preparation method of the modified doped graphene sheet of this embodiment is as follows:
[0076] S01: mixing sodium lignin sulfonate and a phosphate buffer solution having a pH value of 5.0 at a weight ratio of 4:1 to obtain a mixture;
[0077] S02: The mixture is then added to deionized water at a weight ratio of 1:5, followed by addition of 6% chitosan solution (4-8% by weight) and 1% stearic acid (1% by weight) of the total mixture, and stirred thoroughly to obtain a pre-adjusted solution;
[0078] S03: The flake graphene is preheated at 48°C for 5 minutes, and then ultrasonically modified in a pre-adjusted solution that is 5 times the total amount of the flake graphene. After the treatment is completed, the flake graphene is washed with water and dried to obtain a modified flake graphene agent;
[0079] S04: The modified flaky graphene agent and the doped silicon carbide whisker agent are ball-milled in a ball mill at a weight ratio of 7:3 at a ball milling speed of 1000 r / min for 1 hour. After the ball milling is completed, the agent is washed with water and dried to obtain a doped flaky graphene modified adjusting agent.
[0080] The ultrasonic power of the ultrasonic improvement treatment in this embodiment is 350W, and the ultrasonic time is 1 hour.
[0081] The preparation method of the doped silicon carbide whisker agent of this embodiment is:
[0082] 4 parts of silicon carbide whiskers and 2 parts of lanthanum sulfate solution are added to 10 parts of sodium citrate solution, and then 1 part of sodium ethylenediamine ethanesulfonate and 2 parts of nano-silica sol are added, and stirred to mix well to obtain a doped silicon carbide whisker agent.
[0083] The mass fraction of the lanthanum sulfate solution in this embodiment is 3%; the mass fraction of the sodium citrate solution is 15%.
[0084] The preparation method of the rare earth blended silane modifier of this embodiment is as follows:
[0085] S101: adding 3 parts of yttrium nitrate solution and 2 parts of silane coupling agent to 8 parts of ethanol solvent and mixing them evenly, then adding 1 part of sodium dodecylbenzenesulfonate and stirring to obtain a modifier;
[0086] S102: Wollastonite is first dispersed evenly in a 2% by mass hydrochloric acid solution, then washed with water and dried. Then, 5 parts of the dried wollastonite is added to the S101 modifier and stirred thoroughly to obtain a rare earth blended silane modifier.
[0087] The mass fraction of the yttrium nitrate solution in this embodiment is 2%; the silane coupling agent is silane coupling agent KH560.
[0088] The peel-away anti-counterfeiting label is manufactured by a manufacturing method of a peel-away anti-counterfeiting label in this embodiment.
[0089] Example 2.
[0090] A method for manufacturing a peelable anti-counterfeiting label according to this embodiment includes the following steps:
[0091] Step 1: Use a printing device to perform color printing on the front side of the substrate surface layer 6 to form a printed coating 7, and then use a hot laminating machine to coat a layer of BOPP pre-coated film 5 on the back side of the substrate surface layer 6;
[0092] Step 2: Apply oil to the bottom of the BOPP pre-coated film on a glazing device to form an oil layer 4;
[0093] Step 3: spraying mirrored variable data on the lower part of the oil layer 4 on a digital printing press, and then printing a color mirrored pattern on the printing press to form the anti-counterfeiting layer 3;
[0094] Step 4: Use hot melt adhesive coating equipment to apply hot melt adhesive to the surface paper of the substrate to form adhesive layer 2;
[0095] The hot melt adhesive comprises the following raw materials in parts by weight:
[0096] 55 parts of EVA, 18 parts of a modified stabilizer modified with doped flake graphene, 10 parts of a rare earth blended silane modifier, 7 parts of rosin resin, 4 parts of paraffin wax, and 3 parts of an antioxidant;
[0097] The front side of the adhesive layer 2 is compounded with the anti-counterfeiting layer 3, and the back side of the adhesive layer 2 is compounded with the glassine backing paper 1 to obtain the label of the present invention.
[0098] The oil agent of this embodiment is prepared by mixing FS-UV100, FS-UV800 and silicone oil in a weight ratio of 4:1:0.1.
[0099] The antioxidant in this embodiment is BHT; the VA content in the EVA is 32%; and the melt index of the EVA is 30 g / 10 min.
[0100] The preparation method of the film modifier of this embodiment is:
[0101] The doped flaky graphene modified adjusting agent and rare earth blended silane modifier are first stirred and mixed, then washed with water and dried, and the dried product is added together with EVA, rosin resin, paraffin and antioxidant into a mixer for mixing at a mixing temperature of 95°C for 10 minutes, and then extruded into an extruder at an extrusion temperature of 130°C. After the extrusion is completed, the product is cooled to obtain a film modifier.
[0102] The preparation method of the modified doped graphene sheet of this embodiment is as follows:
[0103] S01: mixing sodium lignin sulfonate and a phosphate buffer solution having a pH value of 5.0 at a weight ratio of 4:1 to obtain a mixture;
[0104] S02: The mixture is then added to deionized water at a weight ratio of 1:5, and then 6% chitosan solution (8% by weight) and 3% stearic acid (3% by weight) are added, and the mixture is stirred thoroughly to obtain a pre-adjusted solution;
[0105] S03: The flake graphene is preheated at 52° C. for 10 minutes, and then ultrasonically modified in a pre-adjusted solution that is 10 times the total amount of the flake graphene. After the treatment is completed, the flake graphene is washed with water and dried to obtain a modified flake graphene agent;
[0106] S04: The modified flaky graphene agent and the doped silicon carbide whisker agent are ball-milled in a ball mill at a weight ratio of 8:3 at a ball milling speed of 1500 r / min for 2 h. After the ball milling is completed, the agent is washed with water and dried to obtain a modified adjusting agent doped with flaky graphene.
[0107] The ultrasonic power of the ultrasonic improvement treatment in this embodiment is 400W, and the ultrasonic time is 2h.
[0108] The preparation method of the doped silicon carbide whisker agent of this embodiment is:
[0109] 7 parts of silicon carbide whiskers and 5 parts of lanthanum sulfate solution are added to 15 parts of sodium citrate solution, and then 3 parts of sodium ethylenediamine ethanesulfonate and 4 parts of nano-silica sol are added, and stirred to mix well to obtain a doped silicon carbide whisker agent.
[0110] The mass fraction of the lanthanum sulfate solution in this embodiment is 5%; the mass fraction of the sodium citrate solution is 20%.
[0111] The preparation method of the rare earth blended silane modifier of this embodiment is as follows:
[0112] S101: adding 5 parts of yttrium nitrate solution and 4 parts of silane coupling agent to 12 parts of ethanol solvent and mixing them evenly, then adding 3 parts of sodium dodecylbenzenesulfonate and stirring to obtain a modifier;
[0113] S102: Wollastonite is first dispersed evenly in a 2% by mass hydrochloric acid solution, then washed with water and dried. Then, 8 parts of the dried wollastonite is added to the S101 modifier and stirred thoroughly to obtain a rare earth blended silane modifier.
[0114] The mass fraction of the yttrium nitrate solution in this embodiment is 5%; the silane coupling agent is silane coupling agent KH560.
[0115] The peel-away anti-counterfeiting label is manufactured by a manufacturing method of a peel-away anti-counterfeiting label in this embodiment.
[0116] Example 3.
[0117] A method for manufacturing a peelable anti-counterfeiting label according to this embodiment includes the following steps:
[0118] Step 1: Use a printing device to perform color printing on the front side of the substrate surface layer 6 to form a printed coating 7, and then use a hot laminating machine to coat a layer of BOPP pre-coated film 5 on the back side of the substrate surface layer 6;
[0119] Step 2: Apply oil to the bottom of the BOPP pre-coated film on a glazing device to form an oil layer 4;
[0120] Step 3: spraying mirrored variable data on the lower part of the oil layer 4 on a digital printing press, and then printing a color mirrored pattern on the printing press to form the anti-counterfeiting layer 3;
[0121] Step 4: Use hot melt adhesive coating equipment to apply hot melt adhesive to the surface paper of the substrate to form adhesive layer 2;
[0122] The hot melt adhesive comprises the following raw materials in parts by weight:
[0123] 50 parts of EVA, 15 parts of modified stabilizer of doped flake graphene, 8 parts of rare earth blended silane modifier, 5.5 parts of rosin resin, 3 parts of paraffin wax, and 2 parts of antioxidant;
[0124] The front side of the adhesive layer 2 is compounded with the anti-counterfeiting layer 3, and the back side of the adhesive layer 2 is compounded with the glassine backing paper 1 to obtain the label of the present invention.
[0125] The oil agent of this embodiment is prepared by mixing FS-UV100, FS-UV800 and silicone oil in a weight ratio of 4:1:0.1.
[0126] The antioxidant in this embodiment is BHT; the VA content in the EVA is 30%; and the melt index of the EVA is 28 g / 10 min.
[0127] The preparation method of the film modifier of this embodiment is:
[0128] The doped flaky graphene modified adjusting agent and rare earth blending silane modifier are first stirred and mixed, then washed with water and dried, and the dried product is added together with EVA, rosin resin, paraffin and antioxidant into a mixer for mixing at a mixing temperature of 92°C for 7.5 minutes, and then extruded into an extruder at an extrusion temperature of 125°C. After the extrusion is completed, the film modifier is obtained by cooling.
[0129] The preparation method of the modified doped graphene sheet of this embodiment is as follows:
[0130] S01: mixing sodium lignin sulfonate and a phosphate buffer solution having a pH value of 5.0 at a weight ratio of 4:1 to obtain a mixture;
[0131] S02: The mixture is then added to deionized water at a weight ratio of 1:5, and then 6% by mass of a chitosan solution and 2% by mass of stearic acid are added to the mixture, and stirred thoroughly to obtain a pre-adjusted solution;
[0132] S03: The flake graphene was preheated at 50°C for 7.5 minutes, and then ultrasonically modified in a pre-adjusted solution that was 7.5 times the total amount of the flake graphene. After the treatment, the flake graphene was washed with water and dried to obtain a modified flake graphene agent;
[0133] S04: The modified flaky graphene agent and the doped silicon carbide whisker agent are ball-milled in a ball mill at a weight ratio of 7.5:3 at a ball milling speed of 1250 r / min for 1.5 h. After the ball milling is completed, the agent is washed with water and dried to obtain a modified adjusting agent doped with flaky graphene.
[0134] The ultrasonic power of the ultrasonic improvement treatment in this embodiment is 370W, and the ultrasonic time is 1.5h.
[0135] The preparation method of the doped silicon carbide whisker agent of this embodiment is:
[0136] 5.5 parts of silicon carbide whiskers and 3.5 parts of lanthanum sulfate solution were added to 12.5 parts of sodium citrate solution, and then 2 parts of sodium ethylenediamine ethanesulfonate and 3 parts of nano-silica sol were added and stirred to obtain a doped silicon carbide whisker agent.
[0137] The mass fraction of the lanthanum sulfate solution in this embodiment is 4%; the mass fraction of the sodium citrate solution is 17.5%.
[0138] The preparation method of the rare earth blended silane modifier of this embodiment is as follows:
[0139] S101: adding 4 parts of yttrium nitrate solution and 3 parts of silane coupling agent to 10 parts of ethanol solvent and mixing them evenly, then adding 2 parts of sodium dodecylbenzenesulfonate and stirring to obtain a modifier;
[0140] S102: Wollastonite is first dispersed evenly in a 2% by mass hydrochloric acid solution, then washed with water and dried. 6.5 parts of the dried wollastonite is then added to the S101 modifier and stirred thoroughly to obtain a rare earth blended silane modifier.
[0141] The mass fraction of the yttrium nitrate solution in this embodiment is 3.5%; the silane coupling agent is silane coupling agent KH560.
[0142] The peel-away anti-counterfeiting label is manufactured by a manufacturing method of a peel-away anti-counterfeiting label in this embodiment.
[0143] Comparative Example 1.
[0144] The difference from Example 3 is that no adjusting agent modified by doped flaky graphene is added to the hot melt adhesive.
[0145] Comparative Example 2.
[0146] The difference from Example 3 is that no pre-adjusting liquid treatment is used in the preparation of the doped flaky graphene-modified adjusting agent.
[0147] Comparative Example 3.
[0148] The difference from Example 3 is that no chitosan solution or stearic acid was added during the preparation of the pre-adjusted solution.
[0149] Comparative Example 4.
[0150] The difference from Example 3 is the preparation method of the pre-adjusted liquid:
[0151] A phosphate buffer solution with a pH value of 5.0 was added to deionized water at a weight ratio of 1:5, and then a chitosan solution with a mass fraction of 6% of the total amount of the mixture was added, and stirred thoroughly to obtain a pre-adjusted solution.
[0152] Comparative Example 5.
[0153] The difference from Example 3 is that the doped silicon carbide whisker agent is not used in the preparation of the doped flaky graphene modified adjusting agent.
[0154] Comparative Example 6.
[0155] The difference from Example 3 is that no rare earth blending silane modifier is added to the hot melt adhesive.
[0156] Comparative Example 7.
[0157] The difference from Example 3 is that no modifier treatment is used in the preparation of the rare earth blended silane modifier.
[0158] Comparative Example 8.
[0159] The difference from Example 3 is that no yttrium nitrate solution is added during the preparation of the modifier.
[0160] The hot melt adhesives of the products of Examples 1-3 and Comparative Examples 1-8 were tested. Two substrates of the same size were bonded together using hot melt adhesives. The peel strength of the products was tested using a tensile testing machine. The products were tested under normal conditions, immersed in water for 1 hour (water resistance test), and placed at 70°C for 1 hour (temperature stability test). The performance measurement results are as follows:
[0161]
[0162]
[0163] From Examples 1-3 and Comparative Examples 1-8, it can be concluded that
[0164] The product of Example 3 of the present invention has excellent peel strength performance. At the same time, the product has excellent performance stability under water immersion and heat resistance conditions. The peel strength of Example 3 can reach up to 27.6N / 25mm under normal conditions. At the same time, the water resistance test and the heat stability test can reach up to 26.8N / 25mm and 27.3N / 25mm respectively.
[0165] As can be seen from Comparative Examples 1-5 and Example 3, the performance of the product deteriorated significantly when no doped flaky graphene-modified setting agent was added to the hot melt adhesive. The performance of the product showed a trend of deterioration when no pre-adjustment liquid treatment was used in the preparation of the doped flaky graphene-modified setting agent, chitosan solution and stearic acid were not added in the preparation of the pre-adjustment liquid, and the preparation methods of the pre-adjustment liquid were different. The performance of the product showed a trend of deterioration when no doped silicon carbide whisker agent was used in the preparation of the doped flaky graphene-modified setting agent. The performance of the product deteriorated significantly when the doped silicon carbide whisker agent treatment was used. The performance of the product showed a trend of greater influence on the performance of the product. The pre-adjustment liquid prepared by the method of the present invention and the specific process conditions of the present invention were used to obtain the doped flaky graphene-modified setting agent, and the performance effect of the product was the most significant.
[0166] It can be seen from Comparative Examples 6-8, Comparative Example 1 and Example 3 that when neither the rare earth-blended silane modifier nor the flaky graphene-modified modifier is added to the hot melt adhesive, the performance of the product tends to deteriorate significantly. Only when the two are coordinated and work together, the performance effect of the product is most significant. When the rare earth-blended silane modifier is not treated with a modifier and yttrium nitrate solution is not added in the preparation of the modifier, the performance of the product tends to deteriorate. Only when the rare earth-blended silane modifier is prepared by the method of the present invention, the performance effect of the product is most significant.
[0167] Based on the above tests, the present invention found that the doped silicon carbide whisker agent has a significant impact on the performance of the product. Based on this, the present invention further explored it.
[0168] The preparation method of the doped silicon carbide whisker agent is as follows:
[0169] 5.5 parts of silicon carbide whiskers and 3.5 parts of lanthanum sulfate solution were added to 12.5 parts of sodium citrate solution, and then 2 parts of sodium ethylenediamine ethanesulfonate and 3 parts of nano-silica sol were added and stirred to obtain a doped silicon carbide whisker agent.
[0170] The mass fraction of the lanthanum sulfate solution is 4%; the mass fraction of the sodium citrate solution is 17.5%.
[0171] Experimental Example 1.
[0172] The same as Example 3, except that silicon carbide whiskers are not added in the preparation of the doped silicon carbide whisker agent.
[0173] Experimental Example 2.
[0174] The same as Example 3, except that no lanthanum sulfate solution was added during the preparation of the doped silicon carbide whisker agent.
[0175] Experimental Example 3.
[0176] The same as Example 3, except that sodium ethylenediamine sulfonate is not added in the preparation of the doped silicon carbide whisker agent.
[0177] Experimental Example 4.
[0178] The same as Example 3, except that no nano-silica sol is added in the preparation of the doped silicon carbide whisker agent.
[0179] Experimental Example 5.
[0180] The same as Example 3, the only difference is that the silicon carbide whiskers are replaced by aluminum borate whiskers in the preparation of the doped silicon carbide whisker agent.
[0181]
[0182]
[0183] It can be seen from Experimental Examples 1-5 that silicon carbide whiskers were not added in the preparation of the doped silicon carbide whisker agent, and the performance of the product showed the greatest change trend in the preparation of the doped silicon carbide whisker agent. At the same time, lanthanum sulfate solution, sodium ethylenediamine ethanesulfonate, and nano-silica sol were not added in the preparation of the doped silicon carbide whisker agent, and aluminum borate whiskers were used instead of silicon carbide whiskers. The performance of the product showed a trend of deterioration. Only when the silicon carbide whiskers proprietary to the present invention were used in combination with the specific raw material ratio of the present invention, the performance effect of the product was the most significant. When other raw materials were used instead, the performance effect of the product was not as good as the doped silicon carbide whisker agent prepared by the method of the present invention.
[0184] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.
[0185] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.
Claims
1. A method for producing a peelable anti-counterfeiting label, characterized in that: The following steps are involved: Step 1: Perform color printing on the front side of the substrate surface layer (6) by a printing device to form a printed coating (7), and then use a hot laminating machine to coat a layer of BOPP pre-coated film (5) on the back side of the substrate surface layer (6); Step 2: Apply oil to the bottom of the BOPP pre-coated film on a glazing device to form an oil layer (4); Step 3: spraying mirrored variable data on the lower part of the oil layer (4) on a digital printing machine, and then printing a color mirrored pattern on the printing machine to form an anti-counterfeiting layer (3); Step 4: Use hot melt adhesive coating equipment to apply hot melt adhesive to the surface paper of the substrate to form an adhesive layer (2); The hot melt adhesive comprises the following raw materials in parts by weight: 45-55 parts of EVA, 12-18 parts of modified stabilizer of doped flake graphene, 6-10 parts of rare earth blended silane modifier, 4-7 parts of rosin resin, 2-4 parts of paraffin wax, and 1-3 parts of antioxidant; The front side of the adhesive layer (2) is compounded with the anti-counterfeiting layer (3), and the back side of the adhesive layer (2) is compounded with the glassine backing paper (1) to obtain a label; The preparation method of the hot melt adhesive is as follows: The doped flaky graphene modified setting agent and the rare earth blended silane modifier are first stirred and mixed, then washed with water and dried, and the dried product is added together with EVA, rosin resin, paraffin and antioxidant into a mixer for mixing at a mixing temperature of 90-95° C. for 5-10 minutes, and then extruded into an extruder at a temperature of 120-130° C. After extrusion is completed, the hot melt adhesive is obtained by cooling. The preparation method of the doped flaky graphene modified setting agent is as follows: S01: mixing sodium lignin sulfonate and a phosphate buffer solution having a pH value of 5.0 at a weight ratio of 4:1 to obtain a mixture; S02: The mixture is then added to deionized water at a weight ratio of 1:5, followed by addition of 6% chitosan solution (4-8% by weight) and 1-3% stearic acid (1% by weight) to the total amount of the mixture, and stirred thoroughly to obtain a pre-adjusted solution; S03: The flake graphene is preheated at 48-52° C. for 5-10 minutes, and then ultrasonically modified in a pre-adjusted solution that is 5-10 times the total amount of the flake graphene. After the treatment is completed, the flake graphene is washed with water and dried to obtain a modified flake graphene agent; S04: The modified flaky graphene agent and the doped silicon carbide whisker agent are ball-milled in a ball mill at a weight ratio of (7-8):3 at a ball milling speed of 1000-1500 r / min for 1-2 hours. After the ball milling is completed, the agent is washed with water and dried to obtain a modified adjusting agent doped with flaky graphene.
2. The method for making a peelable anti-counterfeiting label according to claim 1, characterized in that: The oil agent is prepared by mixing FS-UV100, FS-UV800 and silicone oil in a weight ratio of 4:1:0.1; The antioxidant is BHT; the VA content in the EVA is 28-32%; and the melt index of the EVA is 25-30 g / 10 min.
3. The method for making a peelable anti-counterfeiting label according to claim 2, characterized in that: The ultrasonic improvement treatment has an ultrasonic power of 350-400W and an ultrasonic time of 1-2h.
4. The method for making a peelable anti-counterfeiting label according to claim 3, characterized in that: The preparation method of the doped silicon carbide whisker agent is: 4-7 parts of silicon carbide whiskers and 2-5 parts of lanthanum sulfate solution are added to 10-15 parts of sodium citrate solution, and then 1-3 parts of sodium ethylenediamine ethanesulfonate and 2-4 parts of nano-silica sol are added, and stirred to obtain a doped silicon carbide whisker agent.
5. The method for making a peelable anti-counterfeit label according to claim 4, characterized in that: The mass fraction of the lanthanum sulfate solution is 3-5%; the mass fraction of the sodium citrate solution is 15-20%.
6. The method for making a peelable anti-counterfeit label according to claim 1, characterized in that: The preparation method of the rare earth blended silane modifier is: S101: adding 3-5 parts of yttrium nitrate solution and 2-4 parts of silane coupling agent to 8-12 parts of ethanol solvent and mixing them evenly, then adding 1-3 parts of sodium dodecylbenzenesulfonate and stirring to obtain a modifier; S102: First, disperse wollastonite evenly in a 2% by mass hydrochloric acid solution, then wash and dry it. Then, add 5-8 parts of the dried wollastonite to the S101 modifier and stir thoroughly to obtain a rare earth blended silane modifier.
7. The method for making a peelable anti-counterfeit label according to claim 6, characterized in that: The mass fraction of the yttrium nitrate solution is 2-5%; and the silane coupling agent is silane coupling agent KH560.
8. A peel-off anti-counterfeiting label manufactured by the method for manufacturing a peel-off anti-counterfeiting label according to any one of claims 1 to 7.
Citation Information
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