Anion-cation type electric viscosity-reducing adhesive tape and manufacturing method thereof
By using the electro-adhesive tape prepared by anionic polymer material, the problem of the inability to recycle existing thermal and UV adhesive tapes is solved, and an efficient and environmentally friendly electrical adhesive effect is achieved, and it is suitable for the treatment of precision electronic components and thermally sensitive materials.
Patent Information
- Application Number
- CN202411664514.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2025-03-14
AI Technical Summary
The existing thermal and UV adhesive tape cannot be recycled after use, and there are problems such as light pollution and thermal damage, making it difficult to meet the needs of precision electronic components and thermally sensitive materials.
Anionic polymer materials are used to synthesize cationic acrylic monomers and anionic styrene monomers to prepare electrically detoxified functional layer glue and permanent adhesive layer glue to form reversible reusable electro detoxified tape.
The recycling of electrically detached tape is realized, avoiding the defects of heat and UV detached, and does not cause light pollution or thermal damage. It is suitable for the treatment of precision electronic components and thermally sensitive materials.
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Figure CN119614093A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of polymer materials, relates to anionic and cationic electrical debonding tapes, and also relates to a method for preparing the anionic and cationic electrical debonding tapes. Background Art
[0002] Adhesive tapes are widely used in daily life, among which functional anti-viscosity tapes bring convenience in use and post-processing. In terms of anti-viscosity methods, there are heat, UV, electricity and other anti-viscosity methods. It should be pointed out that thermal anti-viscosity tapes are not suitable for some precision electronic components and heat-sensitive materials. UV anti-viscosity causes light pollution, which is harmful to the human body. More importantly, thermal and UV anti-viscosity tapes are disposable and cannot be recycled for multiple times. Electric anti-viscosity is to energize the positive and negative sides of the tape, resulting in a decrease in the viscosity of the tape. In principle, there is electrical heat generation, electrical light generation, and then heat and light anti-viscosity. Not only is the process complicated, but the final effect is the same as thermal and UV anti-viscosity. Therefore, it is necessary to design an electric anti-viscosity tape that can avoid the defects of thermal and UV anti-viscosity and achieve recycling at the same time. Summary of the invention
[0003] The purpose of the present invention is to provide a method for preparing anionic and cationic electrical de-tackifying adhesive tape, wherein the adhesive tape prepared by the method can avoid thermal and UV de-tackifying and can be recycled.
[0004] Another object of the present invention is to provide anionic and cationic electrical debonding tapes.
[0005] The first technical solution adopted by the present invention is a method for preparing anionic and cationic electrical debonding tape, which specifically comprises the following steps: Step 1, synthesizing a cationic acrylic acid monomer; Step 2, synthesizing anionic styrene monomer; Step 3, preparing an electrical debonding functional layer glue according to the products obtained in step 1 and step 2; Step 4, preparing permanent adhesive layer glue; Step 5, preparing an electrical debonding tape according to the products obtained in steps 3 and 4.
[0006] The first technical solution of the present invention is also characterized in that: The specific process of step 1 is: Add 6-12 mL of 8-bromooctyl methacrylate to 20-40 mL of tetrahydrofuran solution and stir evenly; then dissolve 2.5-5 g of trimethylamine hydrochloride in 20-40 mL of ether solution; finally, add the ether solution drop by drop into the tetrahydrofuran solution. After the addition is completed, stir at room temperature for 1-1.5 hours under nitrogen protection, and then increase the reaction temperature to 45-60 oC continues to react for 1-1.5h; after the reaction is completed, cool to room temperature, spin dry the final mixed solution, and separate it through a column with a mixed solvent of ethyl acetate and petroleum ether to obtain an oily cationic acrylic acid monomer.
[0007] The specific process of step 2 is: Take 5.9-11.8 mL of 4-vinylaniline and add it to 20-40 mL of tetrahydrofuran solution and stir evenly; then dissolve 11-22 g of sebacic acid in 20-40 mL of tetrahydrofuran solution, continue to add 0.1-0.2 mL of trifluoroacetic acid and 0.2-0.4 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly; then add the 4-vinylaniline solution drop by drop into the sebacic acid solution, and stir the sebacic acid solution at a speed of 1000-1200 r / min during the addition. After the addition is completed, the reaction temperature is 80-100 under nitrogen protection. o C, and continue the reaction for 1-1.5 hours; after the reaction is completed, the mixed solution is cooled to room temperature and spin-dried, and separated by column with a mixed solvent of ethyl acetate and petroleum ether to obtain an oily anionic styrene monomer.
[0008] The specific process of step 3 is: Take 4-6 mL of cationic acrylic acid monomer, 1-1.5 mL of anionic styrene monomer, 2-3 mL of butyl acrylate, 2-3 mL of N-(hydroxymethyl) acrylamide, and 1-1.5 mL of isobornyl acrylate and add them to 10-15 mL of xylene solvent, then add 0.015-0.03 g of azobisisobutyronitrile, and raise the reaction temperature to 60-80 o C, react for 1-1.5h, and after the reaction is completed, continue to add 10-15mL of xylene to dilute, so as to obtain the electrical viscosity-reducing functional layer glue.
[0009] The specific process of step 4 is: Take 2-4 mL of acrylic acid, 4-8 mL of 2-isooctyl acrylate, 2-8 mL of butyl acrylate, 1-2 mL of hydroxyethyl acrylate, 1-2 mL of isobornyl acrylate, and 0.1-0.2 mL of trihydroxypropyl ether triacrylate, add them to 10-15 mL of xylene solvent, then add 0.015-0.03 g of azobisisobutyronitrile, and raise the reaction temperature to 60-80 o C, react for 1-1.5h, and after the reaction is completed, continue to add 10-15mL of xylene to dilute to obtain a permanent adhesive layer glue.
[0010] The specific process of step 5 is: Step 5.1, removing impurities from the surface of the aluminum foil and drying it; Step 5.2: Place the aluminum foil treated in step 5.1 into a 45-60 o C oven for 12-24h; then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, and place the coated aluminum foil at 60-80 o C oven, dry for 30-45 min; Step 5.3, a layer of electrical debonding functional layer glue is applied on the surface of the aluminum foil treated in step 5.2, and the coated aluminum foil is heated at 60-80°C. o C oven, dry for 30-45 min; Step 5.4, place a piece of polypropylene release paper on the upper surface and the lower surface of the aluminum foil treated in step 5.3, respectively, one piece of polypropylene release paper and the upper surface of the aluminum foil form a release layer I, and the other piece of polypropylene release paper and the lower surface of the aluminum foil form a release layer II, and roll the release layer I and the release layer II together into a roll at a rolling rate of 10-15 cm / min.
[0011] The specific process of step 5.1 is as follows: put the aluminum foil into 200-300 mL of anhydrous ethanol solvent, ultrasonically clean it for 10-15 minutes to remove surface impurities; then put the cleaned aluminum foil into 45-60 o C oven for 12-24h.
[0012] In step 5.2, the coating thickness of the permanent adhesive layer glue above the aluminum foil is 10-15 um; the coating thickness of the permanent adhesive layer glue below the aluminum foil is 30-35 um.
[0013] The second technical solution adopted by the present invention is that the anionic and cationic electrical debonding tape is made by adopting the manufacturing method of the anionic and cationic electrical debonding tape.
[0014] The beneficial effects of the present invention are as follows: 1) The present invention realizes the contact (accessibility) between the anionic and cationic polymer functional groups (anions, cations, neutrals) and the metal layer through the anionic and cationic polymers, the molar ratio of anionic and cationic polymerization monomers, and the length of the anionic and cationic monomer branches and the neutral monomer branches. After the tape is electrified, the anions and cations in the polymer branches migrate to the positive and negative electrodes, and the neutral functional group branches are short, thereby realizing the reversible and reusable electrical de-viscosity function.
[0015] 2) By designing anionic and cationic polymers, the prepared tape can make good use of the migration of anions and cations, the length of anionic and cationic monomer side chains and neutral monomer side chains when powered on, so as to achieve the function of electrical tape viscosity reduction. After power is cut off, the anions and cations in the tape can be restored to their original viscosity due to the electrostatic force, thus achieving reversible recycling. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 It is a schematic diagram of the structure of the anionic and cationic electrical debonding tape of the present invention; Figure 2 It is a schematic diagram of the power-on and power-off cycle performance of the electric debonding tape produced by Example 1 of the method for producing anionic and cationic electric debonding tapes of the present invention. DETAILED DESCRIPTION
[0017] The present invention is described in detail below with reference to the accompanying drawings and specific embodiments.
[0018] The method for preparing the anionic and cationic electrical debonding tape of the present invention specifically comprises the following steps: Step 1, synthesis of cationic acrylic acid monomer, specifically: Add 6-12 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) to 20-40 mL of tetrahydrofuran solution and stir evenly. Then dissolve 2.5-5 g of trimethylamine hydrochloride in 20-40 mL of ether solution. Finally, add the ether solution drop by drop (addition time is 30-60 min) to the tetrahydrofuran solution. After the addition is completed, stir at room temperature for 1-1.5 hours under nitrogen protection, and then increase the reaction temperature to 45-60 o C and continue the reaction for 1-1.5 hours. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (volume ratio 1:10) to obtain an oily cationic acrylic acid monomer.
[0019] Step 2, the synthesis of anionic styrene monomer, is specifically: Take 5.9-11.8 mL of 4-vinylaniline and add it to 20-40 mL of tetrahydrofuran solution and stir evenly. Then dissolve 11-22 g of sebacic acid in 20-40 mL of tetrahydrofuran solution, and continue to add 0.1-0.2 mL of trifluoroacetic acid and 0.2-0.4 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add 4-vinylaniline solution drop by drop (addition time is 30-45min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1000-1200r / min). After the addition is completed, the reaction temperature is 80-100 under nitrogen protection. o C, and the reaction was continued for 1-1.5 hours. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (volume ratio 1:10) to obtain an oily anionic styrene monomer.
[0020] Step 3, preparation of the electrical debonding functional layer glue, specifically: Take 4-6 mL of cationic acrylic acid monomer, 1-1.5 mL of anionic styrene monomer, 2-3 mL of butyl acrylate, 2-3 mL of N-(hydroxymethyl) acrylamide, and 1-1.5 mL of isobornyl acrylate and add them to 10-15 mL of xylene solvent, then add 0.015-0.03 g of azobisisobutyronitrile, and raise the reaction temperature to 60-80 o C, react for 1-1.5h. After the reaction is completed, continue to add 10-15mL of xylene to dilute and set aside.
[0021] Step 4, preparation of permanent adhesive layer glue, specifically: Take 2-4 mL of acrylic acid, 4-8 mL of 2-isooctyl acrylate, 2-8 mL of butyl acrylate, 1-2 mL of hydroxyethyl acrylate, 1-2 mL of isobornyl acrylate, and 0.1-0.2 mL of glycerol trihydroxypropyl ether triacrylate, add them to 10-15 mL of xylene solvent, then add 0.015-0.03 g of azobisisobutyronitrile, and raise the reaction temperature to 60-80 o C, react for 1-1.5h. After the reaction is completed, continue to add 10-15mL of xylene to dilute and set aside.
[0022] Step 5, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10-15 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45-60 o C oven for 12-24h. Then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, with coating thickness of 10-15 um and 30-35 um respectively. o C oven and dried for 30-45 min. Then a layer of electrical debonding functional layer glue (coating thickness is 30-35 um) is coated on the surface of the aluminum foil. o C oven, and dry for 30-45 min. Finally, two pieces of polypropylene release paper are placed on the upper and lower sides of the aluminum foil, and rolled together with the upper surface of the aluminum foil (forming release layer I) and the lower surface of the aluminum foil (forming release layer II) at a rate of 10-15 cm / min.
[0023] Use and testing of electrical adhesive tape Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10-15N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10-15N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0024] Example 1 The method for preparing the anionic and cationic electrical debonding tape of the present invention specifically comprises the following steps: Step 1, synthesis of cationic acrylic acid monomer, specifically: 6 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 20 mL of tetrahydrofuran solution and stirred evenly. Then 2.5 g of trimethylamine hydrochloride was dissolved in 20 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 30 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1 h under nitrogen protection, and the reaction temperature was raised to 45 o C and continue to react for 1 hour. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0025] Step 2, the synthesis of anionic styrene monomer, is specifically: Take 5.9 mL of 4-vinylaniline and add it to 20 mL of tetrahydrofuran solution and stir evenly. Then dissolve 11 g of sebacic acid in 20 mL of tetrahydrofuran solution, and continue to add 0.1 mL of trifluoroacetic acid and 0.2 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 30 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1000 r / min). After the addition is completed, the reaction temperature is 80 °C under nitrogen protection. o C, and the reaction was continued for 1 hour. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0026] Step 3, preparation of the electrical debonding functional layer glue, specifically: Take 4 mL of cationic acrylic acid monomer, 1 mL of anionic styrene monomer, 2 mL of butyl acrylate, 2 mL of N-(hydroxymethyl)acrylamide, and 1 mL of isobornyl acrylate and add them to 10 mL of xylene solvent. Then add 0.015 g of azobisisobutyronitrile and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0027] Step 4, preparation of permanent adhesive layer glue, specifically: Take 2 mL of acrylic acid, 4 mL of 2-isooctyl acrylate, 2 mL of butyl acrylate, 1 mL of hydroxyethyl acrylate, 1 mL of isobornyl acrylate, and 0.1 mL of trihydroxypropyl ether triacrylate, add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0028] Step 5, preparation of the electrical debonding tape, specifically: like Figure 1 (a) shows the structure of the electrical debonding tape. First, take a 50cmx5cm aluminum foil, put it into 200 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45 o C oven for 12 h. Then, a permanent adhesive layer was applied to the upper and lower surfaces of the aluminum foil with a coating thickness of 10 um and 30 um respectively. o C oven and dried for 30 min. A layer of electrical debonding functional layer glue (coating thickness of 30 μm) was further coated on the surface of the aluminum foil. o C oven and dried for 30 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 10 cm / min.
[0029] Use and testing of electrical adhesive tape Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10N). Figure 1 As shown in (b), the metal layer and the aluminum foil layer are connected to the positive and negative power supplies respectively. The tensile force required to disconnect the glass and aluminum alloy plates when the power supply is disconnected and powered on is detected.
[0030] Comparative Example 1 (In the process of preparing the adhesive for the electrical debonding functional layer, the amount of anionic and cationic monomers was exchanged, and the pulling force required for electrical debonding became larger) Step 1, synthesis of cationic acrylic acid monomer, specifically: 6 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 20 mL of tetrahydrofuran solution and stirred evenly. Then 2.5 g of trimethylamine hydrochloride was dissolved in 20 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 30 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1 h under nitrogen protection, and the reaction temperature was raised to 45 o C and continue to react for 1 hour. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0031] Step 2, the synthesis of anionic styrene monomer, is specifically: Take 5.9 mL of 4-vinylaniline and add it to 20 mL of tetrahydrofuran solution and stir evenly. Then dissolve 11 g of sebacic acid in 20 mL of tetrahydrofuran solution, and continue to add 0.1 mL of trifluoroacetic acid and 0.2 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 30 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1000 r / min). After the addition is completed, the reaction temperature is 80 °C under nitrogen protection. o C, and the reaction was continued for 1 hour. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0032] Step 3, preparation of the electrical debonding functional layer glue, specifically: Take 1 mL of cationic acrylic acid monomer, 4 mL of anionic styrene monomer, 2 mL of butyl acrylate, 2 mL of N-(hydroxymethyl)acrylamide, and 1 mL of isobornyl acrylate and add them to 10 mL of xylene solvent. Then add 0.015 g of azobisisobutyronitrile and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0033] Step 4, preparation of permanent adhesive layer glue, specifically: Take 2 mL of acrylic acid, 4 mL of 2-isooctyl acrylate, 2 mL of butyl acrylate, 1 mL of hydroxyethyl acrylate, 1 mL of isobornyl acrylate, and 0.1 mL of trihydroxypropyl ether triacrylate, add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0034] Step 5, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45 o C oven for 12 hours. Then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, with coating thickness of 10 um and 30 um respectively. o C oven and dried for 30-45 min. Then a layer of electrical debonding functional layer glue (coating thickness of 30 um) was coated on the surface of the aluminum foil. o C oven and dried for 30 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 10 cm / min.
[0035] Use and test of electrical debonding tape: Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0036] Comparative Example 2 (the side chain length of the cationic acrylic monomer is shortened, 8-bromooctyl methacrylate is replaced by 1-bromomethyl methacrylate, and the electrical viscosity reduction tensile force is increased) Step 1, synthesis of cationic acrylic acid monomer, specifically: 6 mL of 1-bromomethyl methacrylate (cas: 88520-66-5) was added to 20 mL of tetrahydrofuran solution and stirred evenly. Then 2.5 g of trimethylamine hydrochloride was dissolved in 20 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 30 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1 h under nitrogen protection, and the reaction temperature was raised to 45 o C and continue to react for 1 hour. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0037] Step 2, the synthesis of anionic styrene monomer, is specifically: Take 5.9 mL of 4-vinylaniline and add it to 20 mL of tetrahydrofuran solution and stir evenly. Then dissolve 11 g of sebacic acid in 20 mL of tetrahydrofuran solution, and continue to add 0.1 mL of trifluoroacetic acid and 0.2 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 30 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1000 r / min). After the addition is completed, the reaction temperature is 80 °C under nitrogen protection. o C, and the reaction was continued for 1 hour. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0038] Step 3, preparation of the electrical debonding functional layer glue, specifically: Take 4 mL of cationic acrylic acid monomer, 1 mL of anionic styrene monomer, 2 mL of butyl acrylate, 2 mL of N-(hydroxymethyl)acrylamide, and 1 mL of isobornyl acrylate and add them to 10 mL of xylene solvent. Then add 0.015 g of azobisisobutyronitrile and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0039] Step 4, preparation of permanent adhesive layer glue, specifically: Take 2 mL of acrylic acid, 4 mL of 2-isooctyl acrylate, 2 mL of butyl acrylate, 1 mL of hydroxyethyl acrylate, 1 mL of isobornyl acrylate, and 0.1 mL of trihydroxypropyl ether triacrylate, add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0040] Step 5, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45 o C oven for 12 hours. Then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, with coating thickness of 10 um and 30 um respectively. o C oven and dried for 30-45 min. Then a layer of electrical debonding functional layer glue (coating thickness of 30 um) was coated on the surface of the aluminum foil. o C oven and dried for 30 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 10 cm / min.
[0041] Use and test of electrical debonding tape: Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0042] Comparative Example 3 (the side chain of the anionic styrene monomer becomes shorter, and the anionic styrene monomer is replaced with 4-vinylbenzoic acid, and the electrical viscosity reduction tension becomes larger) Step 1, synthesis of cationic acrylic acid monomer, specifically: 6 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 20 mL of tetrahydrofuran solution and stirred evenly. Then 2.5 g of trimethylamine hydrochloride was dissolved in 20 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 30 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1 h under nitrogen protection, and the reaction temperature was raised to 45 o C and continue to react for 1 hour. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0043] Step 2, preparation of the electrical debonding functional layer glue, specifically: Take 4 mL of cationic acrylic acid monomer, 1 mL of 4-vinylbenzoic acid, 2 mL of butyl acrylate, 2 mL of N-(hydroxymethyl)acrylamide, and 1 mL of isobornyl acrylate and add them to 10 mL of xylene solvent. Then add 0.015 g of azobisisobutyronitrile and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0044] Step 3, preparation of permanent adhesive layer glue, specifically: Take 2 mL of acrylic acid, 4 mL of 2-isooctyl acrylate, 2 mL of butyl acrylate, 1 mL of hydroxyethyl acrylate, 1 mL of isobornyl acrylate, and 0.1 mL of trihydroxypropyl ether triacrylate, add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0045] Step 4, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45 o C oven for 12 hours. Then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, with coating thickness of 10 um and 30 um respectively. o C oven and dried for 30-45 min. Then a layer of electrical debonding functional layer glue (coating thickness of 30 um) was coated on the surface of the aluminum foil. o C oven and dried for 30 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 10 cm / min.
[0046] Use and testing of electrical adhesive tape: Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0047] Comparative Example 4 (the neutral monomer side chain becomes longer, butyl acrylate and N-(hydroxymethyl) acrylamide are replaced by decyl acrylate and hydroxy-PEG3-acrylate respectively, and the electrical viscosity reduction tensile force becomes larger) Step 1, synthesis of cationic acrylic acid monomer, specifically: 6 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 20 mL of tetrahydrofuran solution and stirred evenly. Then 2.5 g of trimethylamine hydrochloride was dissolved in 20 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 30 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1 h under nitrogen protection, and the reaction temperature was raised to 45 o C and continue to react for 1 hour. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0048] Step 2, the synthesis of anionic styrene monomer, is specifically: Take 5.9 mL of 4-vinylaniline and add it to 20 mL of tetrahydrofuran solution and stir evenly. Then dissolve 11 g of sebacic acid in 20 mL of tetrahydrofuran solution, and continue to add 0.1 mL of trifluoroacetic acid and 0.2 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 30 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1000 r / min). After the addition is completed, the reaction temperature is 80 °C under nitrogen protection. o C, and the reaction was continued for 1 hour. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0049] Step 3, preparation of the electrical debonding functional layer glue, specifically: Take 4 mL of cationic acrylic acid monomer, 1 mL of anionic styrene monomer, 2 mL of decyl acrylate, 2 mL of hydroxy-PEG3-acrylate, and 1 mL of isobornyl acrylate and add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0050] Step 4, preparation of permanent adhesive layer glue, specifically: Take 2 mL of acrylic acid, 4 mL of 2-isooctyl acrylate, 2 mL of butyl acrylate, 1 mL of hydroxyethyl acrylate, 1 mL of isobornyl acrylate, and 0.1 mL of trihydroxypropyl ether triacrylate, add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0051] Step 5, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45 o C oven for 12 hours. Then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, with coating thickness of 10 um and 30 um respectively. o C oven and dried for 30-45 min. Then a layer of electrical debonding functional layer glue (coating thickness of 30 um) was coated on the surface of the aluminum foil. o C oven and dried for 30 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 10 cm / min.
[0052] Use and test of electrical debonding tape: Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0053] Table 1 Electrical detackification performance of Example 1 and Comparative Examples 1-4
[0054] As shown in Table 1, compared with Example 1, the pulling force of Comparative Examples 2 and 3 when the power is off is reduced, which is because the side chains of the anionic styrene monomer and the cationic acrylic monomer are shortened, the side chains are reduced in entanglement, friction, and viscosity. On the contrary, the neutral monomer side chains of Comparative Example 4 are longer, and its pulling force when the power is off is increased compared with Example 1.
[0055] When the power is on, the tensile force of Example 1 is only 0.4, which is nearly 60 times smaller than that when the power is off, indicating that the adhesive tape of Example 1 has a good viscosity reduction effect under the action of current. In the preparation process of the adhesive layer of the electrical viscosity reduction functional layer of Comparative Example 1, the amount of anionic and cationic monomers is exchanged, such as Figure 1 As shown on the right, after power is applied, under the action of voltage, the positive and negative charges on the polymer side chains migrate separately, and the force between the metal layer and the anionic side chains of the electrical debonding layer determines the magnitude of the pulling force. If the amount of anionic and cationic monomers is swapped, the content of anionic side chains increases, resulting in a poor electrical debonding effect.
[0056] In Comparative Example 2, the side chain length of the cationic acrylic monomer is shortened, and 8-bromooctyl methacrylate is replaced by 1-bromomethyl methacrylate. After power is applied, the cationic side chain migration is shorter, the volume expansion is smaller, and the electrical viscosity reduction effect is relatively weakened.
[0057] In Comparative Example 3, the anionic styrene monomer side chain is shortened, and the anionic styrene monomer is replaced with 4-vinylbenzoic acid, and the electric viscosity reduction tension becomes larger. On the one hand, after power is turned on, the anionic side chain migrates shorter and the volume expansion is smaller. On the other hand, the anionic side chain is shorter than the neutral monomer side chain, and the force between the neutral monomer and the metal layer cannot be stripped.
[0058] At the same time, in Comparative Example 4, the neutral monomer branch becomes, although the anionic branch migrates faster after power is applied, which can cause the volume expansion of the adhesive layer. However, there is still a force between the anionic branch and the metal layer that is shorter than the neutral monomer branch and cannot be peeled off. Therefore, the pulling force when power is applied is higher than that of Example 1 and lower than that of Comparative Example 3.
[0059] like Figure 2 As shown, the mechanical properties of the electrical debonding tape of Example 1 after cyclic power-on and power-off, the time interval between power-on and power-off is 1h. After three power-on and power-off treatments, the tension can still be reduced to 0.7N, and the tension can still reach 27N after power-off. The electrical debonding effect is well achieved.
[0060] Comparative Example 5 (the adhesive of the electrical debonding functional layer does not contain cationic acrylic acid, the electrical debonding effect is poor and cannot be recycled) Step 1, the synthesis of anionic styrene monomer, is specifically: Take 5.9 mL of 4-vinylaniline and add it to 20 mL of tetrahydrofuran solution and stir evenly. Then dissolve 11 g of sebacic acid in 20 mL of tetrahydrofuran solution, and continue to add 0.1 mL of trifluoroacetic acid and 0.2 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 30 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1000 r / min). After the addition is completed, the reaction temperature is 80 °C under nitrogen protection. o C, and the reaction was continued for 1 hour. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0061] Step 2, preparation of the electrical debonding functional layer glue, specifically: 1 mL of anionic styrene monomer, 2 mL of butyl acrylate, 2 mL of N-(hydroxymethyl) acrylamide, and 1 mL of isobornyl acrylate were added to 10 mL of xylene solvent, and then 0.015 g of azobisisobutyronitrile was added. The reaction temperature was raised to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0062] Step 3, preparation of permanent adhesive layer glue, specifically: Take 2 mL of acrylic acid, 4 mL of 2-isooctyl acrylate, 2 mL of butyl acrylate, 1 mL of hydroxyethyl acrylate, 1 mL of isobornyl acrylate, and 0.1 mL of trihydroxypropyl ether triacrylate, add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0063] Step 4, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45 o C oven for 12 hours. Then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, with coating thickness of 10 um and 30 um respectively. o C oven and dried for 30-45 min. Then a layer of electrical debonding functional layer glue (coating thickness of 30 um) was coated on the surface of the aluminum foil. oC oven and dried for 30 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 10 cm / min.
[0064] Use and test of electrical debonding tape: Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0065] Comparative Example 6 (the glue of the electrical viscosity-reducing functional layer does not contain anionic styrene monomer and has no electrical viscosity-reducing function) Step 1, synthesis of cationic acrylic acid monomer, specifically: 6 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 20 mL of tetrahydrofuran solution and stirred evenly. Then 2.5 g of trimethylamine hydrochloride was dissolved in 20 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 30 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1 h under nitrogen protection, and the reaction temperature was raised to 45 o C and continue to react for 1 hour. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0066] Step 2, preparation of the electrical debonding functional layer glue, specifically: Take 4 mL of cationic acrylic acid monomer, 2 mL of butyl acrylate, 2 mL of N-(hydroxymethyl) acrylamide, and 1 mL of isobornyl acrylate and add them to 10 mL of xylene solvent. Then add 0.015 g of azobisisobutyronitrile and raise the reaction temperature to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0067] Step 3, preparation of permanent adhesive layer glue, specifically: Take 2 mL of acrylic acid, 4 mL of 2-isooctyl acrylate, 2 mL of butyl acrylate, 1 mL of hydroxyethyl acrylate, 1 mL of isobornyl acrylate, and 0.1 mL of trihydroxypropyl ether triacrylate, add them to 10 mL of xylene solvent, then add 0.015 g of azobisisobutyronitrile, and raise the reaction temperature to 60 oC, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0068] Step 4, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 45 o C oven for 12 hours. Then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, with coating thickness of 10 um and 30 um respectively. o C oven and dried for 30-45 min. Then a layer of electrical debonding functional layer glue (coating thickness of 30 um) was coated on the surface of the aluminum foil. o C oven and dried for 30 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 10 cm / min.
[0069] Use and test of electrical debonding tape: Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 10N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 10N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0070] Table 2 Comparative Examples 5-6 Electrical Detackification Performance
[0071] As shown in Table 2, compared with Example 1, the pulling force of Comparative Examples 5-6 when the power is off is reduced, which is due to the lack of cationic acrylic monomer and anionic styrene monomer components.
[0072] When the power is turned on, the tension of Comparative Example 5 increases significantly compared with that of Example 1. This is because the electric viscosity reduction functional layer lacks cationic side chains, and there is no cationic side chain migration when the power is turned on, resulting in a small volume expansion. In Example 1, since the anionic side chains migrate to the metal layer after the power is turned on, the anionic side chains are longer than the neutral side chains. After the migration, the effect of the medium side chains and the metal can be peeled off to achieve electrical viscosity reduction. However, Comparative Example 6 lacks anionic styrene monomer components and cannot achieve a viscosity reduction effect. Therefore, the tension does not change much before and after the power is turned on.
[0073] Example 2 The method for preparing the anionic and cationic electrical debonding tape of the present invention specifically comprises the following steps: Step 1, synthesis of cationic acrylic acid monomer, specifically: 7 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 30 mL of tetrahydrofuran solution and stirred evenly. Then 3 g of trimethylamine hydrochloride was dissolved in 30 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 40 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1.2 h under nitrogen protection, and the reaction temperature was raised to 55 o C was continued to react for 1.2 hours. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0074] Step 2, the synthesis of anionic styrene monomer, is specifically: Take 8 mL of 4-vinylaniline and add it to 30 mL of tetrahydrofuran solution and stir evenly. Then dissolve 15 g of sebacic acid in 30 mL of tetrahydrofuran solution, and continue to add 0.15 mL of trifluoroacetic acid and 0.3 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 35 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1100 r / min). After the addition is completed, the reaction temperature is 90 °C under nitrogen protection. o C, and the reaction was continued for 1.2 hours. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0075] Step 3, preparation of the electrical debonding functional layer glue, specifically: Take 5 mL of cationic acrylic acid monomer, 1.2 mL of anionic styrene monomer, 2.5 mL of butyl acrylate, 2.5 mL of N-(hydroxymethyl) acrylamide, and 1.2 mL of isobornyl acrylate and add them to 12 mL of xylene solvent. Then add 0.02 g of azobisisobutyronitrile and raise the reaction temperature to 70 o C, react for 1.2 h. After the reaction is completed, add 12 mL of xylene to dilute and set aside.
[0076] Step 4, preparation of permanent adhesive layer glue, specifically: Take 3 mL of acrylic acid, 6 mL of 2-isooctyl acrylate, 6 mL of butyl acrylate, 1.5 mL of hydroxyethyl acrylate, 1.5 mL of isobornyl acrylate, and 0.15 mL of trihydroxypropyl ether triacrylate, add them to 12 mL of xylene solvent, then add 0.02 g of azobisisobutyronitrile, and raise the reaction temperature to 70 o C, react for 1.2 h. After the reaction is completed, add 12 mL of xylene to dilute and set aside.
[0077] Step 5, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 260 mL of anhydrous ethanol solvent, and ultrasonically clean it for 12 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into 55 o C oven for 18 hours. Then, a permanent adhesive layer was applied to the upper and lower surfaces of the aluminum foil, with a coating thickness of 12 um and 32 um, respectively. o C oven and dried for 35 min. A layer of electrical debonding functional layer glue (coating thickness of 32 μm) was further coated on the surface of the aluminum foil. o C oven and dried for 35 min. Finally, the two polypropylene release papers were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 12 cm / min.
[0078] Use and testing of electrical adhesive tape Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 12N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 12N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0079] Example 3 The method for preparing the anionic and cationic electrical debonding tape of the present invention specifically comprises the following steps: Step 1, synthesis of cationic acrylic acid monomer, specifically: 12 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 40 mL of tetrahydrofuran solution and stirred evenly. Then 5 g of trimethylamine hydrochloride was dissolved in 40 mL of ether solution. Finally, the ether solution was added dropwise (addition time was 60 min) to the tetrahydrofuran solution. After the addition was completed, the mixture was stirred at room temperature for 1.5 h under nitrogen protection, and the reaction temperature was raised to 60o C was continued to react for 1.5 hours. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0080] Step 2, the synthesis of anionic styrene monomer, is specifically: Take 11.8 mL of 4-vinylaniline and add it to 40 mL of tetrahydrofuran solution and stir evenly. Then dissolve 22 g of sebacic acid in 40 mL of tetrahydrofuran solution, and continue to add 0.2 mL of trifluoroacetic acid and 0.4 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 45 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1200 r / min). After the addition is completed, the reaction temperature is 100 o C, and the reaction was continued for 1.5 hours. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0081] Step 3, preparation of the electrical debonding functional layer glue, specifically: Take 6 mL of cationic acrylic acid monomer, 1.5 mL of anionic styrene monomer, 3 mL of butyl acrylate, 3 mL of N-(hydroxymethyl) acrylamide, and 1.5 mL of isobornyl acrylate and add them to 15 mL of xylene solvent. Then add 0.03 g of azobisisobutyronitrile and raise the reaction temperature to 80 o C, react for 1.5 h. After the reaction is completed, add 15 mL of xylene to dilute and set aside.
[0082] Step 4, preparation of permanent adhesive layer glue, specifically: Take 4 mL of acrylic acid, 8 mL of 2-isooctyl acrylate, 8 mL of butyl acrylate, 2 mL of hydroxyethyl acrylate, 2 mL of isobornyl acrylate, and 0.2 mL of glycerol trihydroxypropyl ether triacrylate, add them to 15 mL of xylene solvent, then add 0.03 g of azobisisobutyronitrile, and raise the reaction temperature to 80 o C, react for 1.5 h. After the reaction is completed, add 15 mL of xylene to dilute and set aside.
[0083] Step 5, preparation of the electrical debonding tape, specifically: First, take a 50cmx5cm aluminum foil, put it into 300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 15 minutes to remove impurities such as dust and oil on the surface. Then put the cleaned aluminum foil into a 60 oC oven for 24h. Then, a permanent adhesive layer was applied on the upper and lower surfaces of the aluminum foil with a coating thickness of 15um and 35um respectively. o C oven and dried for 45 min. A layer of electrical debonding functional layer glue (coating thickness of 35 μm) was further coated on the surface of the aluminum foil. o C oven and dried for 45 min. The last two pieces of polypropylene release paper were rolled together with the upper surface (forming release layer I) and the lower surface (forming release layer II) of the aluminum foil at a rate of 15 cm / min.
[0084] Use and testing of electrical adhesive tape Take the prepared electrical debonding tape of 3cmx3cm, peel off the release layer II, stick the permanent adhesive layer on the surface of 5cmx5cm glass (thickness 3mm), and then roll the tape with a roller (pressure 15N). Then peel off the release layer I, stick the electrical debonding layer on the surface of 5cmx5cm aluminum alloy plate (thickness 3mm), and then roll the tape with a roller (pressure 15N). Connect the metal layer and aluminum foil layer to the positive and negative power supply respectively. Detect the pulling force required to disconnect the glass and aluminum alloy plate when the power is disconnected and powered on.
[0085] Example 4 Compared with Example 1, step 1, synthesis of cationic acrylic acid monomer, specifically: 9 mL of 8-bromooctyl methacrylate (cas: 128055-30-1) was added to 20 mL of tetrahydrofuran solution and stirred evenly. Then 2.5 g of trimethylamine hydrochloride was dissolved in 20 mL of ether solution. Finally, the ether solution was added dropwise (dropping time was 30 min) to the tetrahydrofuran solution. After the dropwise addition was completed, it was stirred at room temperature for 1 h under nitrogen protection, and then the reaction temperature was increased to 45 o C and continue to react for 1 hour. After the reaction is completed, the mixed solution is cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily cationic acrylic acid monomer.
[0086] The remaining steps are the same as those in Example 1.
[0087] Example 5 Compared with Example 1, step 2, the synthesis of anionic styrene monomer, is specifically as follows: Take 6.8 mL of 4-vinylaniline and add it to 20 mL of tetrahydrofuran solution and stir evenly. Then dissolve 11 g of sebacic acid in 20 mL of tetrahydrofuran solution, and continue to add 0.1 mL of trifluoroacetic acid and 0.2 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly. Then add the 4-vinylaniline solution drop by drop (addition time is 30 min) to the sebacic acid solution. During the addition process, the sebacic acid solution needs to be stirred rapidly (speed 1000 r / min). After the addition is completed, the reaction temperature is 80 °C under nitrogen protection. o C, and the reaction was continued for 1 hour. After the reaction was completed, the mixed solution was cooled to room temperature and dried by spin drying, and separated by column with a mixed solvent of ethyl acetate and petroleum ether (1:10) to obtain an oily anionic styrene monomer.
[0088] The remaining steps are the same as those in Example 1.
[0089] Example 6 Compared with Example 1, 4 mL of cationic acrylic acid monomer, 1.1 mL of anionic styrene monomer, 2 mL of butyl acrylate, 2 mL of N-(hydroxymethyl)acrylamide, and 1 mL of isobornyl acrylate were added to 14 mL of xylene solvent, and then 0.015 g of azobisisobutyronitrile was added. The reaction temperature was raised to 60 o C, react for 1 h. After the reaction is completed, add 10 mL of xylene to dilute and set aside.
[0090] The remaining steps are the same as those in Example 1.
Claims
1. The method for making anionic and cationic electric debonding tape is characterized by: The specific steps include: Step 1, synthesizing a cationic acrylic acid monomer; Step 2, synthesizing anionic styrene monomer; Step 3, preparing an electrical debonding functional layer glue according to the products obtained in step 1 and step 2; Step 4, preparing permanent adhesive layer glue; Step 5, preparing an electrical debonding tape according to the products obtained in steps 3 and 4.
2. The method for making anionic and cationic electrical debonding tape according to claim 1, characterized in that: The specific process of step 1 is as follows: Add 6-12 mL of 8-bromooctyl methacrylate to 20-40 mL of tetrahydrofuran solution and stir evenly; then dissolve 2.5-5 g of trimethylamine hydrochloride in 20-40 mL of ether solution; finally, add the ether solution drop by drop into the tetrahydrofuran solution. After the addition is completed, stir at room temperature for 1-1.5 hours under nitrogen protection, and then increase the reaction temperature to 45-60 o C continues to react for 1-1.5h; after the reaction is completed, cool to room temperature, spin dry the final mixed solution, and separate it through a column with a mixed solvent of ethyl acetate and petroleum ether to obtain an oily cationic acrylic acid monomer.
3. The method for making anionic and cationic electrical debonding tape according to claim 2, characterized in that: The specific process of step 2 is: Take 5.9-11.8 mL of 4-vinylaniline and add it to 20-40 mL of tetrahydrofuran solution and stir evenly; then dissolve 11-22 g of sebacic acid in 20-40 mL of tetrahydrofuran solution, continue to add 0.1-0.2 mL of trifluoroacetic acid and 0.2-0.4 g of 4-hydroxy-2,2,6,6-tetramethylpiperidinyl nitroxide free radical and stir evenly; then add the 4-vinylaniline solution drop by drop into the sebacic acid solution, and stir the sebacic acid solution at a speed of 1000-1200 r / min during the addition. After the addition is completed, the reaction temperature is 80-100 under nitrogen protection. o C, and continue the reaction for 1-1.5 hours; after the reaction is completed, the mixed solution is cooled to room temperature and spin-dried, and separated by column with a mixed solvent of ethyl acetate and petroleum ether to obtain an oily anionic styrene monomer.
4. The method for making anionic and cationic electrical debonding tape according to claim 3, characterized in that: The specific process of step 3 is as follows: Take 4-6 mL of cationic acrylic acid monomer, 1-1.5 mL of anionic styrene monomer, 2-3 mL of butyl acrylate, 2-3 mL of N-(hydroxymethyl) acrylamide, and 1-1.5 mL of isobornyl acrylate and add them to 10-15 mL of xylene solvent, then add 0.015-0.03 g of azobisisobutyronitrile, and raise the reaction temperature to 60-80 o C, react for 1-1.5h, and after the reaction is completed, continue to add 10-15mL of xylene to dilute, so as to obtain the electrical viscosity-reducing functional layer glue.
5. The method for making anionic and cationic electrical debonding tape according to claim 4, characterized in that: The specific process of step 4 is as follows: Take 2-4 mL of acrylic acid, 4-8 mL of 2-isooctyl acrylate, 2-8 mL of butyl acrylate, 1-2 mL of hydroxyethyl acrylate, 1-2 mL of isobornyl acrylate, and 0.1-0.2 mL of trihydroxypropyl ether triacrylate, add them to 10-15 mL of xylene solvent, then add 0.015-0.03 g of azobisisobutyronitrile, and raise the reaction temperature to 60-80 o C, react for 1-1.5h, and after the reaction is completed, continue to add 10-15mL of xylene to dilute to obtain a permanent adhesive layer glue.
6. The method for making anionic and cationic electrical debonding tape according to claim 5, characterized in that: The specific process of step 5 is as follows: Step 5.1, removing impurities from the surface of the aluminum foil and drying it; Step 5.2: Place the aluminum foil treated in step 5.1 into a 45-60 o C oven for 12-24h; then apply permanent adhesive layer glue on the upper and lower surfaces of the aluminum foil, and place the coated aluminum foil at 60-80 o C oven, dry for 30-45 min; Step 5.3, a layer of electrical debonding functional layer glue is applied on the surface of the aluminum foil treated in step 5.2, and the coated aluminum foil is heated at 60-80°C. o C oven, dry for 30-45 min; Step 5.4, place a piece of polypropylene release paper on the upper surface and the lower surface of the aluminum foil treated in step 5.3, respectively, one piece of polypropylene release paper and the upper surface of the aluminum foil form a release layer I, and the other piece of polypropylene release paper and the lower surface of the aluminum foil form a release layer II, and roll the release layer I and the release layer II together into a roll at a rolling rate of 10-15 cm / min.
7. The method for making anionic and cationic electrical debonding tape according to claim 6, characterized in that: The specific process of step 5.1 is as follows: put the aluminum foil into 200-300 mL of anhydrous ethanol solvent, and ultrasonically clean it for 10-15 minutes to remove surface impurities; then put the cleaned aluminum foil into 45-60 o C oven for 12-24h.
8. The method for making anionic and cationic electrical debonding tape according to claim 7, characterized in that: In the step 5.2, the coating thickness of the permanent adhesive layer glue above the aluminum foil is 10-15 um; the coating thickness of the permanent adhesive layer glue below the aluminum foil is 30-35 um.
9. Anionic and cationic electrical debonding tape, made according to the method for making anionic and cationic electrical debonding tape according to any one of claims 1 to 8.
Citation Information
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