CN111334214B - Novel protective film containing thermal viscosity-reducing adhesive and preparation method thereof - Google Patents
Novel protective film containing thermal viscosity-reducing adhesive and preparation method thereof Download PDFInfo
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- CN111334214B CN111334214B CN202010212554.3A CN202010212554A CN111334214B CN 111334214 B CN111334214 B CN 111334214B CN 202010212554 A CN202010212554 A CN 202010212554A CN 111334214 B CN111334214 B CN 111334214B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/35—Heat-activated
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/062—Copolymers with monomers not covered by C09D133/06
- C09D133/066—Copolymers with monomers not covered by C09D133/06 containing -OH groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2433/00—Presence of (meth)acrylic polymer
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2475/00—Presence of polyurethane
Abstract
The invention relates to the technical field of protective films, and particularly provides a novel protective film containing thermal viscosity-reducing adhesive and a preparation method thereof. The invention provides a novel protective film containing thermal viscosity-reducing adhesive, which comprises a base material layer and an adhesive layer; wherein the glue layer comprises the following raw materials: a resin, a curing agent, a thermal expansion material, and a solvent; the resin is selected from any one or combination of polyurethane resin, acrylic resin and epoxy resin. The anti-sticking protective film containing the specific glue layer is adopted, and the acrylic resin in the glue layer and the thermal expansion material act together to realize that the obtained protective film can achieve higher peeling strength before heat treatment, realize high sticking performance, and simultaneously realize peeling without residual glue at non-high temperature, so that the anti-sticking protective film is very convenient in the actual use process.
Description
Technical Field
The invention relates to the technical field of protective films, and particularly provides a novel protective film containing thermal viscosity-reducing adhesive and a preparation method thereof.
Background
When tiny components such as plastic parts, glass, metal plates and the like are processed, the components are usually required to be fixed in an auxiliary mode through adhesive tapes, and damage caused by movement of the components in a cutting process is avoided. In addition, when the local surface of a certain component needs to be polished in the etching, washing or coating process, in order to protect other parts which do not need to be processed from being affected, the parts which do not need to be processed are firstly covered by the adhesive tape, and then peeled off after the processing is finished. However, the adhesive strength of the tape used for fixing or shielding needs to be strictly controlled, and if the adhesive force is too strong, a situation that the component is damaged when the tape is removed is likely to occur, and if the adhesive force is too small, the component is likely to be not completely fixed/shielded, resulting in damage.
In the prior art, a viscosity-reducing protective film is generally adopted for processing, high viscosity is kept during fixing/shielding, the components are ensured to be fixed and stable, the viscosity is reduced by adopting a certain means after cutting is finished, and an adhesive tape is removed. However, the prior art still does not have very excellent easy-stripping performance, the situation of damaging components still occurs sometimes, high stripping strength during fixing is not easy to realize, and the technical effects of easy stripping and no adhesive residue are realized at lower temperature.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a novel protective film containing a thermal viscosity-reducing adhesive, including a substrate layer and an adhesive layer; wherein the glue layer comprises the following raw materials: a resin, a curing agent, a thermal expansion material, and a solvent; the resin is selected from any one or combination of polyurethane resin, acrylic resin and epoxy resin.
As a preferred technical scheme of the invention, the glue layer comprises the following raw materials in parts by weight: 35-55 parts of resin, 0.5-5 parts of curing agent, 2-10 parts of thermal expansion material and 30-50 parts of solvent.
As a preferred embodiment of the present invention, the curing agent is selected from 1, 3-phenylene diisocyanate, 4' -diphenyl diisocyanate, 1, 4-phenylene diisocyanate, 4' -diphenylmethane diisocyanate, 2, 4-toluene diisocyanate, 2, 6-toluene diisocyanate, 4' -toluidine diisocyanate, 2,4, 6-triisocyanate toluene, 1,3, 5-triisocyanate benzene, any one or combination of trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1, 2-propylene diisocyanate, 2, 3-butylene diisocyanate, 1, 3-butylene diisocyanate, dodecamethylene diisocyanate, and 2,4, 4-trimethylhexamethylene diisocyanate.
As a preferred technical scheme of the invention, the expansion material is expansion microspheres of an Expancel series.
As a preferred technical scheme of the invention, the particle size of the expanded microspheres of the Expancel series is 8-30 μm.
As a preferred technical scheme of the invention, the thermal expansion temperature of the Expancel series is 80-200 ℃.
As a preferred technical scheme of the invention, the thickness of the glue layer is 20-45 μm.
As a preferable technical scheme of the invention, the thickness of the base material layer is 30-60 mu m.
As a preferred technical scheme of the present invention, the preparation method of the adhesive layer comprises: firstly, stirring the expansion material and the solvent for 20-30 min, then adding the curing agent and the resin, and stirring for 20-30 min to obtain the epoxy resin.
The second aspect of the invention provides a preparation method of the novel protective film containing the thermal viscosity-reducing adhesive, which comprises the steps of coating an adhesive layer on the surface of a base material layer, and drying to obtain the protective film.
Has the advantages that: the anti-sticking protective film containing the specific glue layer is adopted, and the acrylic resin in the glue layer and the thermal expansion material act together to realize that the obtained protective film can achieve higher peeling strength before heat treatment, realize high sticking performance, and simultaneously realize peeling without residual glue at non-high temperature, and is very convenient in the actual use process.
Detailed Description
The technical features of the technical solutions provided by the present invention will be further clearly and completely described below with reference to the specific embodiments, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one element or action from another element or action without necessarily requiring or implying any actual such relationship or order between such elements or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or composition that comprises a list of elements does not include those elements but may include other elements not expressly listed or inherent to such process, method, or composition.
The words "preferred", "preferably", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention. It should be understood that other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about".
The invention provides a novel protective film containing thermal viscosity-reducing adhesive, which comprises a base material layer and an adhesive layer; wherein the glue layer comprises the following raw materials: a resin, a curing agent, a thermal expansion material, and a solvent; the resin is selected from any one or combination of polyurethane resin, acrylic resin and epoxy resin; preferably, the glue layer comprises the following raw materials in parts by weight: 35-55 parts of resin, 0.5-5 parts of curing agent, 2-10 parts of thermal expansion material and 30-50 parts of solvent; further preferably, the glue layer comprises the following raw materials in parts by weight: 41-49 parts of resin, 1-4 parts of curing agent, 5-8 parts of thermal expansion material and 37-46 parts of solvent; more preferably, the glue layer comprises the following raw materials in parts by weight: 46 parts of resin, 3.5 parts of curing agent, 7 parts of thermal expansion material and 42 parts of solvent.
The resin can be any one or combination of more of polyurethane resin, acrylic resin and epoxy resin; preferably an acrylic resin; the raw materials for preparing the acrylic resin comprise an acrylate monomer and a dicarboxylic acid substance; more preferably, the molar ratio of the acrylate monomer to the dicarboxylic acid is 1: (0.5 to 0.8); more preferably, the molar ratio of acrylate monomer to dicarboxylic acid is 1: 0.75.
the acrylate monomer comprises any one or more of isooctyl acrylate, butyl acrylate, acrylic acid, lauric acid acrylate, stearic acid acrylate, 6-hydroxyhexyl acrylate, 2, 3-dihydroxypropyl acrylate and 2, 4-dihydroxypropyl methacrylate; preferably 2, 3-dihydroxypropyl acrylate with butyl acrylate; further preferably, the molar ratio of 2, 3-dihydroxypropyl acrylate to butyl acrylate is 1: (3-5); more preferably, the molar ratio of 2, 3-dihydroxypropyl acrylate to butyl acrylate is 1: 4.5.
the dicarboxylic acid of the present invention is not particularly limited, and refers to a compound having two carboxyl groups, and in one embodiment, the dicarboxylic acid is 1, 4-succinic acid.
The curing agent of the present invention may be a curing agent material for a resin of a person skilled in the art, such as, but not limited to: any one or more combinations of 1, 3-phenylene diisocyanate, 4,4' -diphenyldiisocyanate, 1, 4-phenylene diisocyanate, 4,4' -diphenylmethane diisocyanate, 2, 4-toluene diisocyanate, 2, 6-toluene diisocyanate, 4,4' -toluidine diisocyanate, 2,4, 6-triisocyanate toluene, 1,3, 5-triisocyanate benzene, trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1, 2-propylene diisocyanate, 2, 3-butylene diisocyanate, 1, 3-butylene diisocyanate, dodecamethylene diisocyanate, and 2,4, 4-trimethylhexamethylene diisocyanate.
The type of solvent used in the present invention is not particularly limited, and examples thereof include, but are not limited to: any one or more of acetone, cyclohexanone, ethyl acetate, butyl acetate, butanone, methanol, ethanol, propanol, isopropanol, isobutanol, n-butanol, methyl isobutyl ketone, isophorone, toluene, xylene, propylene glycol methyl ether, and dipropylene glycol methyl ether; preferably ethyl acetate.
The thermal expansion material can generate gas under the action of thermal decomposition in the heating treatment process or under the condition of high temperature, so that the contact area between the protective film and an adhered object is reduced, and the effect of easy stripping is realized.
In one embodiment, the expanded microspheres of the Expancel series have a particle size of 8 to 30 μm.
In one embodiment, the thermal expansion temperature is 80-200 ℃; preferably 051DU40, 031DU40, and 053DU 40.
The thermal anti-sticking protective film is frequently used in the process of processing a semiconductor wafer, but the thermal anti-sticking condition of the protective film obtained at present is harsh, and the applicant finds that under the combined action of acrylic resin formed by dicarboxylic acid substances and acrylate monomers and a thermal expansion material, particularly when the acrylate monomers are 2, 3-dihydroxy propyl acrylate and butyl acrylate, expansion microspheres of an Expancel series are adopted as the thermal expansion material, the particle size of the expansion microspheres of the Expancel series is 8-30 mu m, the thermal expansion temperature is 80-200 ℃, the problem of residual glue anti-sticking at low temperature is realized, the technical effects of high peel strength before heating and low peel strength after heating are realized simultaneously, the acrylic resin is possibly used as a base material, the great increase of cohesive force and the migration of small molecules in the subsequent drying and curing processes are avoided, and the low peel strength before heating is not caused, high peel strength after heating; the thermal expansion material with the specific particle size and other molecules in the system act together to form a uniform system, so that the peeling strength is not greatly influenced, the volume change before heating treatment can be reduced, the contact area between the anti-adhesion layer and the adhered object under the heating treatment is reduced, and the technical effect of peeling without adhesive residue is realized.
The preparation method of the adhesive layer comprises the following steps: firstly, stirring the expansion material and the solvent for 20-30 min, then adding the curing agent and the resin, and stirring for 20-30 min to obtain the epoxy resin.
Preferably, the preparation method of the adhesive layer comprises the following steps:
(1) firstly, mixing an acrylate monomer, a dicarboxylic acid substance and a half weight of solvent, and stirring at 70-75 ℃ for 6-8 hours;
(2) and (3) stirring the expansion material and the rest half of the solvent for 20-30 min, adding the curing agent and the substance obtained in the step (1), and stirring for 20-30 min to obtain the composite material.
In one embodiment, the thickness of the adhesive layer is 20 to 45 μm.
In one embodiment, the thickness of the substrate layer is 30 to 60 μm.
The substrate layer of the present invention may be selected from materials of resins of those skilled in the art, such as, but not limited to: one or more of polyolefins such as low-density polyethylene, medium-density polyethylene, high-density polyethylene, ultra-low-density polyethylene, random copolymer polypropylene, block copolymer polypropylene, homopolypropylene, polybutene, polymethylpentene, ethylene-vinyl acetate copolymer, ethylene-butene copolymer, ethylene-hexene copolymer, polyurethane, polyesters such as polyethylene terephthalate, polyimide, polyether ether ketone, polyvinyl chloride, and polyvinylidene chloride.
The second aspect of the invention provides a preparation method of the novel protective film containing the thermal viscosity-reducing adhesive, which comprises the steps of coating an adhesive layer on the surface of a base material layer, and drying to obtain the protective film; the drying temperature is preferably 65-85 ℃; the drying time is preferably 90-120 s, and the base material layer is preferably a material subjected to corona treatment.
Example 1
The embodiment 1 of the invention provides a novel protective film containing thermal viscosity-reducing adhesive, which comprises a substrate layer and an adhesive layer; the glue layer comprises the following raw materials in parts by weight: 36 parts of resin, 1 part of curing agent, 3 parts of thermal expansion material and 32 parts of solvent;
the resin is acrylate resin, and the preparation raw materials of the acrylate resin comprise acrylate monomers and dicarboxylic acid substances; the molar ratio of the acrylate monomer to the dicarboxylic acid is 1: 0.55;
the acrylate monomer is 2, 3-dihydroxypropyl acrylate and butyl acrylate, and the molar ratio of the 2, 3-dihydroxypropyl acrylate to the butyl acrylate is 1: 3.2;
the dicarboxylic acid is 1, 4-succinic acid;
the curing agent is 2, 4-toluene diisocyanate;
the solvent is ethyl acetate;
adopting expansion microspheres of an Expancel series as a thermal expansion material;
the expanded microspheres of the Expancel series are 051DU 40;
the preparation method of the adhesive layer comprises the following steps:
(1) firstly, mixing an acrylate monomer, a dicarboxylic acid substance and a half weight of solvent, and stirring at 70 ℃ for 6.5-7 hours;
(2) stirring the expansion material and the rest half of the solvent by weight for 25-28 min, adding the curing agent and the substance obtained in the step (1), and stirring for 25-26 min to obtain the composite material;
the thickness of the adhesive layer is 36 micrometers, and the thickness of the base material layer is 50 micrometers;
the preparation method of the novel protective film containing the thermal viscosity-reducing adhesive comprises the steps of coating an adhesive layer on the surface of a base material layer, and drying to obtain the protective film; the drying temperature is 70 ℃; the drying time is 110 s; the substrate layer is polyethylene terephthalate which is subjected to corona treatment.
Example 2
Embodiment 2 of the present invention provides a novel protective film containing a thermal viscosity-reducing adhesive, including a substrate layer and an adhesive layer; the glue layer comprises the following raw materials in parts by weight: 52 parts of resin, 4.8 parts of curing agent, 10 parts of thermal expansion material and 49 parts of solvent;
the resin is acrylate resin, and the preparation raw materials of the acrylate resin comprise acrylate monomers and dicarboxylic acid substances; the molar ratio of the acrylate monomer to the dicarboxylic acid is 1: 0.8;
the acrylate monomer is 2, 3-dihydroxypropyl acrylate and butyl acrylate, and the molar ratio of the 2, 3-dihydroxypropyl acrylate to the butyl acrylate is 1: 4.8;
the dicarboxylic acid is 1, 4-succinic acid;
the curing agent is 2, 4-toluene diisocyanate;
the solvent is ethyl acetate;
adopting expansion microspheres of an Expancel series as a thermal expansion material;
the expanded microspheres of the Expancel series are 051DU 40;
the preparation method of the adhesive layer comprises the following steps:
(1) firstly, mixing an acrylate monomer, a dicarboxylic acid substance and a half weight of solvent, and stirring at 70 ℃ for 6.5-7 hours;
(2) stirring the expansion material and the rest half of the solvent by weight for 25-28 min, adding the curing agent and the substance obtained in the step (1), and stirring for 25-26 min to obtain the composite material;
the thickness of the adhesive layer is 36 micrometers, and the thickness of the base material layer is 50 micrometers;
the preparation method of the novel protective film containing the thermal viscosity-reducing adhesive comprises the steps of coating an adhesive layer on the surface of a base material layer, and drying to obtain the protective film; the drying temperature is 70 ℃; the drying time is 110 s; the substrate layer is polyethylene terephthalate which is subjected to corona treatment.
Example 3
Embodiment 3 of the present invention provides a novel protective film containing a thermal viscosity-reducing adhesive, including a substrate layer and an adhesive layer; the glue layer comprises the following raw materials in parts by weight: 46 parts of resin, 3.5 parts of curing agent, 7 parts of thermal expansion material and 42 parts of solvent;
the resin is acrylate resin, and the preparation raw materials of the acrylate resin comprise acrylate monomers and dicarboxylic acid substances; the molar ratio of the acrylate monomer to the dicarboxylic acid is 1: 0.75;
the acrylate monomer is 2, 3-dihydroxypropyl acrylate and butyl acrylate, and the molar ratio of the 2, 3-dihydroxypropyl acrylate to the butyl acrylate is 1: 4.5;
the dicarboxylic acid is 1, 4-succinic acid;
the curing agent is 2, 4-toluene diisocyanate;
the solvent is ethyl acetate;
adopting expansion microspheres of an Expancel series as a thermal expansion material;
the expanded microspheres of the Expancel series are 051DU 40;
the preparation method of the adhesive layer comprises the following steps:
(1) firstly, mixing an acrylate monomer, a dicarboxylic acid substance and a half weight of solvent, and stirring at 70 ℃ for 6.5-7 hours;
(2) stirring the expansion material and the rest half of the solvent by weight for 25-28 min, adding the curing agent and the substance obtained in the step (1), and stirring for 25-26 min to obtain the composite material;
the thickness of the adhesive layer is 36 micrometers, and the thickness of the base material layer is 50 micrometers;
the preparation method of the novel protective film containing the thermal viscosity-reducing adhesive comprises the steps of coating an adhesive layer on the surface of a base material layer, and drying to obtain the protective film; the drying temperature is 70 ℃; the drying time is 110 s; the substrate layer is polyethylene terephthalate which is subjected to corona treatment.
Example 4
Example 4 of the present invention provides a novel thermal viscosity-reducing adhesive-containing protective film, which is similar to example 3, except that the dicarboxylic acid compound content is 0.
Example 5
Example 5 of the present invention provides a novel protective film comprising a thermal visbreaker, and the specific embodiment thereof is the same as example 3, except that the content of expanded microspheres in the Expancel series is 0.
Example 6
Example 6 of the present invention provides a novel protective film containing a thermal viscosity-reducing adhesive, which is similar to example 3, except that the expandable microspheres of Expancel series are 930DU 120.
Performance evaluation
The protective films obtained in examples 1 to 6 were cured at 40 ℃ for 72 hours, and then firmly attached to a glass plate, and the following tests were performed:
1. measuring 180-degree peel force of the protective film at room temperature;
2. and (3) heating the protective film at 100 ℃ for 5min, and observing whether residual glue exists.
TABLE 1
| Peel force (g/25mm) | Whether or not there is residual glue | |
| Example 1 | 897 | No adhesive residue |
| Example 2 | 903 | No adhesive residue |
| Example 3 | 911 | No adhesive residue |
| Example 4 | \ | With residual glue |
| Example 5 | \ | With residual glue |
| Example 6 | 817 | With residual glue |
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. The protective film containing the thermal-reduction adhesive is characterized by comprising a substrate layer and an adhesive layer; wherein the glue layer comprises the following raw materials in parts by weight: 35-55 parts of resin, 0.5-5 parts of curing agent, 2-10 parts of thermal expansion material and 30-50 parts of solvent;
the resin is acrylic resin, the preparation raw materials of the acrylic resin are composed of acrylate monomers and dicarboxylic acid substances, and the molar ratio of the acrylate monomers to the dicarboxylic acid substances is 1: (0.5-0.8), the acrylate monomer is 2, 3-dihydroxypropyl acrylate and butyl acrylate, and the molar ratio of the 2, 3-dihydroxypropyl acrylate to the butyl acrylate is 1: (3-5);
the expansion material is an Expancel series expansion microsphere;
the particle size of the expanded microspheres of the Expancel series is 8-30 mu m;
the thermal expansion temperature of the expansion microspheres of the Expancel series is 80-200 ℃;
the dicarboxylic acid substance is 1, 4-succinic acid;
the curing agent is selected from any one or combination of 1, 3-phenylene diisocyanate, 1, 4-phenylene diisocyanate, 4,4 '-diphenylmethane diisocyanate, 2, 4-toluene diisocyanate, 2, 6-toluene diisocyanate, 4,4' -toluidine diisocyanate, 2,4, 6-triisocyanate toluene, 1,3, 5-triisocyanate benzene, trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1, 2-propylene diisocyanate, 2, 3-butylene diisocyanate, 1, 3-butylene diisocyanate, dodecamethylene diisocyanate, and 2,4, 4-trimethylhexamethylene diisocyanate.
2. The protective film containing the thermal adhesive reducing agent according to claim 1, wherein the thickness of the adhesive layer is 20 to 45 μm.
3. The protective film containing the thermal adhesive reducing agent according to claim 1, wherein the thickness of the substrate layer is 30 to 60 μm.
4. The protective film containing the thermal adhesive reducing agent according to any one of claims 1 to 3, wherein the adhesive layer is prepared by a method comprising: firstly, stirring the expansion material and the solvent for 20-30 min, then adding the curing agent and the resin, and stirring for 20-30 min to obtain the epoxy resin.
5. A method for preparing a protective film containing thermal visbreaking glue according to any one of claims 1 to 4, wherein the protective film is obtained by coating a glue layer on the surface of a base material layer and drying.
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| CN114790371A (en) * | 2022-04-16 | 2022-07-26 | 广州星业新材料有限公司 | UV curing thermal expansion strippable pressure-sensitive adhesive tape |
| CN115725256B (en) * | 2022-11-18 | 2024-01-26 | 道生天合材料科技(上海)股份有限公司 | Detachable acrylate adhesive, preparation method thereof and detachable structural member |
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| JP2000239620A (en) * | 1999-02-19 | 2000-09-05 | Fujimori Kogyo Co Ltd | Thermal release self-adhesive and self-adhesive member using same |
| JP3941448B2 (en) * | 2000-10-13 | 2007-07-04 | 住友化学株式会社 | Laminated body in which resin composition and adherend are bonded together |
| CN105131869A (en) * | 2015-09-10 | 2015-12-09 | 深圳市美信电子有限公司 | Thermal viscosity loss pressure-sensitive adhesive, thermally peelable adhesive tape and preparation methods of thermal viscosity loss pressure-sensitive adhesive and thermally peelable adhesive tape |
| CN110684481B (en) * | 2019-09-19 | 2022-03-04 | 浙江耀阳新材料科技有限公司 | Controllable-viscosity adhesive tape and application method thereof |
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Address after: 512000 chlor alkali characteristic industrial base of hougongdu Economic Development Zone, Rucheng Town, Ruyuan County, Shaoguan City, Guangdong Province Patentee after: Guangdong Shuocheng Technology Co.,Ltd. Address before: 512000 chlor alkali characteristic industrial base of hougongdu Economic Development Zone, Rucheng Town, Ruyuan County, Shaoguan City, Guangdong Province Patentee before: GUANGDONG SHUOCHENG TECHNOLOGY Co.,Ltd. |