Preparation method of pressure-sensitive adhesive glue and tape with wide temperature range response pyrolysis

Abstract

This invention relates to a method for preparing a wide-temperature-range responsive pyrolytic adhesive pressure-sensitive adhesive and tape. The aim is to design and propose a method for preparing the pyrolytic adhesive tape while ensuring both protective and debonding performance. This invention achieves a balance between the pyrolytic adhesive tape's pyrolytic bonding temperature range, pyrolytic bonding time, and pyrolytic peel force by adjusting the expanded microsphere system in the adhesive system and introducing microcrystalline polymers and special resins. The advantages of this invention are the combined use of different expansion temperatures and amounts of expanded microspheres, and the synergistic effect of microcrystalline polymers and special resins, thereby achieving a perfect balance between the temperature response range and adhesive strength of the pyrolytic adhesive tape. This method utilizes the combination of these materials to prepare a wide-temperature-range responsive pyrolytic adhesive pressure-sensitive adhesive and tape.

Description

Technical Field

[0001] This invention relates to a method for preparing a wide-temperature-range responsive pyrolytic pressure-sensitive adhesive and tape. Background Technology

[0002] Pyrolytic adhesive tape is a special type of functional tape that loses its adhesiveness and can be peeled off under heating conditions. Its special function relies primarily on the structure and formulation design of the adhesive layer. At room temperature, this type of tape holds objects in place through strong adhesion between the adhesive layer and the substrate. When heated (typically 60℃~200℃), the molecular structure of the adhesive layer changes, causing a sharp decrease or even loss of adhesion. Its core advantages are no residue and no damage to the bonded surface, solving the problems of residue and scratches caused by traditional tapes when removed.

[0003] This type of tape has applications across multiple fields: in the electronics industry, it's used to temporarily fix precision components during chip and flexible screen manufacturing processes, easily separating them after heating to avoid scratching circuits; in automotive manufacturing, it's used to attach interior parts (such as sound insulation cotton and trim strips), allowing for heat-removal without residue during repairs; in building decoration, it's used to fix decorative films and masking tape, allowing for complete removal without staining walls after application; in the cultural and creative handicraft field, it's used to transfer stickers and heat transfers, precisely positioning them before peeling off the backing paper without damaging the design; and in medical settings, it's used to temporarily fix auxiliary devices, reducing skin irritation for patients. Furthermore, it's suitable for scenarios with high surface integrity requirements, such as optical lenses and new energy battery components, becoming an indispensable "removable" solution in precision manufacturing and delicate operations.

[0004] However, conventional pyrolytic adhesive tapes face a series of problems, such as insufficient debonding, narrow debonding temperature range, excessive residual stress after debonding, and the industry-wide problem of debonding marks, which have always restricted the expansion and wide application of pyrolytic adhesive tapes. Summary of the Invention

[0005] This invention aims to design and propose a method for preparing a wide-temperature-range responsive thermally disintegrating pressure-sensitive adhesive and tape, while ensuring both protective and debonding performance. By adjusting the expanded microsphere system in the adhesive system and introducing microcrystalline polymers and special resins, this invention successfully achieves a balance between the thermal disintegration temperature range, thermal disintegration time, and thermal disintegration peel force of the thermally disintegrating adhesive tape.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0007] A method for preparing a wide-temperature-range responsive pyrolytic pressure-sensitive adhesive, the method being as follows:

[0008] Step 1: Weigh out 50-100 parts by weight of isooctyl acrylate and 200 parts by weight of ethyl acetate, and prepare an isooctyl acrylate solution; weigh out 30-70 parts by weight of butyl acrylate and 100 parts by weight of ethyl acetate, and prepare an butyl acrylate solution; weigh out 70-150 parts by weight of methyl methacrylate and 200 parts by weight of ethyl acetate, and prepare an methyl methacrylate solution; weigh out 15-50 parts by weight of isobornyl methacrylate and 100 parts by weight of ethyl acetate, and prepare an isobornyl methacrylate solution; weigh out 5-10 parts by weight of acrylic acid and 50 parts by weight of ethyl acetate, and prepare an acrylic acid solution.

[0009] Step 2: Weigh 10-30 parts of 70-100℃ expandable microspheres and 100 parts of toluene according to the mass ratio, and prepare expandable microsphere solution A; weigh 5-20 parts of 130-160℃ expandable microspheres and 50 parts of toluene according to the mass ratio, and prepare expandable microsphere solution B; the expandable microspheres are made of thermoplastic resin.

[0010] Step 3: Weigh 5-20 parts of the microcrystalline polymer and 50 parts of ethyl acetate according to their respective weights, and prepare a microcrystalline polymer solution; weigh 3-15 parts of the special resin and 20 parts of toluene according to their respective weights, and prepare a special resin solution; weigh 1-5 parts of the initiator and 10 parts of ethyl acetate according to their respective weights, and prepare an initiator solution.

[0011] Step 4: Weigh out 20-50 parts of isooctyl acrylate solution, 10-30 parts of butyl acrylate solution, 20-50 parts of methyl methacrylate solution, 10-25 parts of isobornyl methacrylate solution, 5-10 parts of acrylic acid solution, and 1.5-5 parts of initiator solution according to the mass ratio. Mix them evenly and add them to a four-necked flask. Heat to 78-88℃ and react for 3-6 hours with a stirring speed of 80-200 rpm.

[0012] Step 5: After the reaction is complete, add 5-10 parts by weight of expanded microsphere solution A, 8-25 parts by weight of expanded microsphere solution B, 5-25 parts by weight of microcrystalline polymer solution and 3-15 parts by weight of special resin solution to the reaction system. Continue stirring at 50-200 rpm for 5-20 minutes to obtain a wide temperature range responsive pyrolytic pressure-sensitive adhesive.

[0013] Furthermore, in step three, the microcrystalline polymer is one or more of polyamide, polycarbonate, and polycaprolactone.

[0014] Furthermore, in step three, the special resin is one or more of cyclopentadiene resin, terpene phenolic resin, and tert-butylphenolic resin.

[0015] Furthermore, in step three, the initiator is one or more of azobisisobutyronitrile, benzoyl peroxide, diisopropylbenzene peroxide, and azobisisobutyronitrile.

[0016] A method for preparing tape using the wide-temperature-range responsive pyrolytic pressure-sensitive adhesive prepared by the above preparation method, wherein the method is as follows: the adhesive is coated on a PET film with a coating thickness of 20~40μm, and after the coating process is completed, it is placed in a vacuum drying oven for drying, thereby obtaining the wide-temperature-range responsive pyrolytic adhesive tape.

[0017] Furthermore, in step six, the drying temperature is 70~90℃ and the drying time is 2~6 minutes.

[0018] The present invention aims to design a method for preparing a wide-temperature-range responsive pyrolytic adhesive pressure-sensitive adhesive and tape, and to prepare it through a free radical copolymerization reaction, thereby solving the problems of narrow debonding temperature window and complicated debonding operation of conventional pyrolytic adhesive tapes.

[0019] The advantages of this invention compared to existing technologies are as follows: The combined use of microspheres with different expansion temperatures and dosages, and the synergistic effect of microcrystalline polymers and special resins, achieves a perfect balance between the temperature response range and adhesive strength of the pyrolytic adhesive tape. Through the combined use of these materials, a method for preparing a wide-temperature-range responsive pyrolytic pressure-sensitive adhesive and tape can be developed. Attached Figure Description

[0020] Figure 1 Digital photographs of the pressure-sensitive adhesive of the pyrolysis adhesive tape at 80℃~110℃;

[0021] Figure 2 Digital photographs of adhesive tape that has undergone pyrolysis at 100℃~140℃;

[0022] Figure 3 GPC diagram of pressure-sensitive adhesive tape pyrolyzed at 80℃~110℃;

[0023] Figure 4 GPC diagram of pressure-sensitive adhesive tape pyrolyzed at 100℃~140℃;

[0024] Figure 5 Infrared spectrum of pressure-sensitive adhesive tape pyrolyzed at 80℃~110℃;

[0025] Figure 6 Thermogravimetric analysis (TGA) of the pressure-sensitive adhesive tape pyrolyzed at 100℃~140℃. Detailed Implementation

[0026] The present invention will be further described below with reference to the embodiments; however, the scope of the present invention is not limited to these embodiments.

[0027] Example 1: Preparation method of pyrolytic adhesive tape at 80℃~110℃

[0028] First, weigh 75 parts of isooctyl acrylate and 200 parts of ethyl acetate, and prepare an isooctyl acrylate solution; weigh 36 parts of butyl acrylate and 100 parts of ethyl acetate, and prepare a butyl acrylate solution; weigh 76 parts of methyl methacrylate and 200 parts of ethyl acetate, and prepare a methyl methacrylate solution; weigh 27 parts of isobornyl methacrylate and 100 parts of ethyl acetate, and prepare an isobornyl methacrylate solution; weigh 5.5 parts of acrylic acid and 50 parts of ethyl acetate, and prepare an acrylic acid solution. Acid solution; weigh 15 parts of 80℃ expanded microspheres and simultaneously weigh 100 parts by weight of toluene, and prepare expanded microsphere solution A; weigh 8 parts of 140℃ expanded microspheres and simultaneously weigh 50 parts by weight of toluene, and prepare expanded microsphere solution B; weigh 8 parts of polycarbonate and simultaneously weigh 50 parts by weight of ethyl acetate, and prepare polycarbonate solution; weigh 5.8 parts of dicyclopentadiene resin and simultaneously weigh 20 parts by weight of toluene, and prepare dicyclopentadiene resin solution; weigh 1.5 parts by weight of azobisisoheptanenitrile and simultaneously weigh 10 parts by weight of ethyl acetate, and prepare azobisisoheptanenitrile solution.

[0029] Next, according to the mass ratio, weigh out 33 parts of isooctyl acrylate solution, 24 parts of butyl acrylate solution, 45 parts of methyl methacrylate solution, 13 parts of isobornyl methacrylate solution, 6 parts of acrylic acid solution, and 2 parts of azobisisobutyronitrile solution. Mix them evenly and add them to a four-necked flask. Heat to 82°C and react for 3.5 hours at a stirring speed of 120 rpm. After the reaction is completed, add 9 parts of expanded microsphere solution A, 8.5 parts of expanded microsphere solution B, 12.5 parts of polycarbonate solution, and 11 parts of dicyclopentadiene resin solution to the reaction system according to the mass ratio. Continue stirring at 85 rpm for 15 minutes to obtain a pyrolytic pressure-sensitive adhesive that can be heated to 80°C~110°C.

[0030] Finally, the adhesive is applied to the PET film with a coating thickness of 25μm. After the coating process is completed, it is placed in a vacuum drying oven for drying at a temperature of 80℃ for 5 minutes, thereby obtaining a pyrolytic adhesive tape at 80℃~110℃.

[0031] Figure 1 This demonstrates the successful preparation of wide-temperature-range responsive pyrolytic adhesives and tapes. Figure 3 It can be demonstrated that the pyrolytic adhesive with a wide temperature range response has a narrow molecular weight distribution. Figure 5The spectral data can directly prove the successful synthesis of a wide-temperature-range responsive pyrolytic adhesive.

[0032] Example 2: Preparation method of pyrolytic adhesive tape at 100℃~140℃

[0033] First, weigh 61 parts of isooctyl acrylate and 200 parts of ethyl acetate, and prepare an isooctyl acrylate solution; weigh 35 parts of butyl acrylate and 100 parts of ethyl acetate, and prepare a butyl acrylate solution; weigh 101 parts of methyl methacrylate and 200 parts of ethyl acetate, and prepare a methyl methacrylate solution; weigh 35 parts of isobornyl methacrylate and 100 parts of ethyl acetate, and prepare an isobornyl methacrylate solution; weigh 8.5 parts of acrylic acid and 50 parts of ethyl acetate, and prepare an acrylic acid solution. Solutions: Weigh 15 parts of 90℃ expanded microspheres and simultaneously weigh 100 parts by weight of toluene to prepare expanded microsphere solution A; weigh 9 parts of 150℃ expanded microspheres and simultaneously weigh 50 parts by weight of toluene to prepare expanded microsphere solution B; weigh 17 parts of polycaprolactone and simultaneously weigh 50 parts by weight of ethyl acetate to prepare polycaprolactone solution; weigh 3.5 parts of tert-butylphenolic resin and simultaneously weigh 20 parts by weight of toluene to prepare tert-butylphenolic resin solution; weigh 2.5 parts by weight of benzoyl peroxide and simultaneously weigh 10 parts by weight of ethyl acetate to prepare benzoyl peroxide solution.

[0034] Next, according to the mass ratio, weigh 28 parts of isooctyl acrylate solution, 21 parts of butyl acrylate solution, 26 parts of methyl methacrylate solution, 18 parts of isoborneol methacrylate solution, 5.5 parts of acrylic acid solution, and 2.5 parts of benzoyl peroxide solution. Mix them evenly and add them to a four-necked flask. Heat to 82°C and react for 5 hours at a stirring speed of 120 rpm. After the reaction is completed, add 6.5 parts of expanding microsphere solution A, 19 parts of expanding microsphere solution B, 8.8 parts of polycaprolactone solution, and 12 parts of tert-butylphenol resin solution to the reaction system according to the mass ratio. Continue stirring at 180 rpm for 15 minutes to obtain a pyrolytic pressure-sensitive adhesive that can be heated to 100°C~140°C.

[0035] Finally, the adhesive is applied to the PET film with a thickness of 35μm. After the coating process is completed, it is placed in a vacuum drying oven for drying at a temperature of 90℃ for 4 minutes, thereby obtaining a pyrolytic adhesive tape that can be heated to 100℃~140℃.

[0036] Figure 2 This demonstrates the successful preparation of wide-temperature-range responsive pyrolytic adhesives and tapes. Figure 4It can be demonstrated that the pyrolytic adhesive with a wide temperature range response has a narrow molecular weight distribution. Figure 6 The thermogravimetric data can directly prove the good thermal stability of the wide-temperature-range responsive pyrolytic adhesive below 140℃.

Claims

1. A method for preparing a wide-temperature-range responsive pyrolytic pressure-sensitive adhesive, characterized in that: The method is as follows: Step 1: Weigh out 50-100 parts by weight of isooctyl acrylate and 200 parts by weight of ethyl acetate, and prepare an isooctyl acrylate solution; weigh out 30-70 parts by weight of butyl acrylate and 100 parts by weight of ethyl acetate, and prepare an butyl acrylate solution; weigh out 70-150 parts by weight of methyl methacrylate and 200 parts by weight of ethyl acetate, and prepare an methyl methacrylate solution; weigh out 15-50 parts by weight of isobornyl methacrylate and 100 parts by weight of ethyl acetate, and prepare an isobornyl methacrylate solution; weigh out 5-10 parts by weight of acrylic acid and 50 parts by weight of ethyl acetate, and prepare an acrylic acid solution. Step 2: Weigh 10-30 parts of the 70-100℃ expandable microspheres according to the mass ratio, and simultaneously weigh 100 parts of toluene to prepare expandable microsphere solution A; weigh 5-20 parts of the 130-160℃ expandable microspheres, and simultaneously weigh 50 parts of toluene to prepare expandable microsphere solution B. Step 3: Weigh 5-20 parts of the microcrystalline polymer and 50 parts of ethyl acetate according to their respective weights, and prepare a microcrystalline polymer solution; weigh 3-15 parts of the special resin and 20 parts of toluene according to their respective weights, and prepare a special resin solution; weigh 1-5 parts of the initiator and 10 parts of ethyl acetate according to their respective weights, and prepare an initiator solution. Step 4: Weigh out 20-50 parts of isooctyl acrylate solution, 10-30 parts of butyl acrylate solution, 20-50 parts of methyl methacrylate solution, 10-25 parts of isobornyl methacrylate solution, 5-10 parts of acrylic acid solution, and 1.5-5 parts of initiator solution according to the mass ratio. Mix them evenly and add them to a four-necked flask. Heat to 78-88℃ and react for 3-6 hours with a stirring speed of 80-200 rpm. Step 5: After the reaction is complete, add 5-10 parts by weight of expanded microsphere solution A, 8-25 parts by weight of expanded microsphere solution B, 5-25 parts by weight of microcrystalline polymer solution and 3-15 parts by weight of special resin solution to the reaction system. Continue stirring at 50-200 rpm for 5-20 minutes to obtain a wide temperature range responsive pyrolytic pressure-sensitive adhesive.

2. The preparation method of the wide-temperature-range responsive pyrolytic pressure-sensitive adhesive according to claim 1, characterized in that: In step three, the microcrystalline polymer is one or more of polyamide, polycarbonate, and polycaprolactone.

3. The method for preparing the wide-temperature-range responsive pyrolytic pressure-sensitive adhesive according to claim 1, characterized in that: In step three, the special resin is one or more of cyclopentadiene resin, terpene phenolic resin, and tert-butylphenolic resin.

4. The method for preparing the wide-temperature-range responsive pyrolytic pressure-sensitive adhesive according to claim 1, characterized in that: In step three, the initiator is one or more of azobisisobutyronitrile, benzoyl peroxide, diisopropylbenzene peroxide, and azobisisobutyronitrile.

5. A method for preparing adhesive tape using the wide-temperature-range responsive pyrolytic pressure-sensitive adhesive prepared by any one of claims 1 to 4, characterized in that: The method is as follows: apply adhesive to a PET film with a coating thickness of 20~40μm, and after the coating process is completed, place it in a vacuum drying oven for drying to obtain a wide temperature range responsive pyrolytic adhesive tape.

6. The method for preparing the wide-temperature-range responsive pyrolytic pressure-sensitive adhesive according to claim 5, characterized in that: In step six, the drying temperature is 70~90℃ and the drying time is 2~6 minutes.

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