CN113845861A - Low-climbing organic silicon protective film and preparation method thereof - Google Patents
Low-climbing organic silicon protective film and preparation method thereof Download PDFInfo
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- 230000001681 protective effect Effects 0.000 title claims abstract description 51
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 35
- 239000010703 silicon Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 36
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 33
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 31
- 229920001971 elastomer Polymers 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 25
- 239000003112 inhibitor Substances 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 229920002545 silicone oil Polymers 0.000 claims abstract description 22
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims abstract description 20
- 238000004873 anchoring Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 16
- 239000010410 layer Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 32
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000003292 glue Substances 0.000 claims description 28
- 229910004674 SiO0.5 Inorganic materials 0.000 claims description 20
- 229910052681 coesite Inorganic materials 0.000 claims description 16
- 229910052906 cristobalite Inorganic materials 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 229910052682 stishovite Inorganic materials 0.000 claims description 16
- 229910052905 tridymite Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 229920002799 BoPET Polymers 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 239000008096 xylene Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 6
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 6
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 2
- DSVRVHYFPPQFTI-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane;platinum Chemical group [Pt].C[Si](C)(C)O[Si](C)(C=C)C=C DSVRVHYFPPQFTI-UHFFFAOYSA-N 0.000 claims description 2
- 239000001530 fumaric acid Substances 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 2
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 230000009194 climbing Effects 0.000 abstract description 5
- 230000003993 interaction Effects 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 15
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 13
- 238000003851 corona treatment Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- 239000011889 copper foil Substances 0.000 description 8
- 239000012790 adhesive layer Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002688 maleic acid derivatives Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Classifications
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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
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- 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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a low-climbing organic silicon protective film and a preparation method thereof, wherein the low-climbing organic silicon protective film comprises a base material, an organic silicon pressure-sensitive adhesive layer and a release film, the organic silicon pressure-sensitive adhesive layer is positioned between the base material and the release film, and the organic silicon pressure-sensitive adhesive comprises the following components in parts by weight: 20-80 parts of non-polar end group raw rubber, 5-20 parts of non-polar end group MQ resin, 1-2 parts of high-viscosity vinyl silicone oil, 0.1-2 parts of a cross-linking agent, 0-1 part of an inhibitor, 0-1 part of an anchoring agent, 0.5-5 parts of a platinum catalyst and 100-400 parts of a solvent. The organic silicon pressure-sensitive adhesive is prepared by adopting materials such as non-polar end group raw rubber, non-polar end group MQ resin and the like through the establishment of an organic silicon system, the content of polar groups is reduced, the interaction between the organic silicon pressure-sensitive adhesive and an adhered object is reduced, and the reduction of climbing of stripping force is realized.
Description
Technical Field
The invention relates to the technical field of protective films, in particular to a low-climbing organic silicon protective film and a preparation method thereof.
Background
Protective films are commonly used for protecting screens and housings of electronic products, and are very common products in daily life. As a protective material for protecting articles, protective films are also commonly used in the die cutting industry. In the die cutting industry, the material of the protective film is generally selected according to different application modes and requirements. Some protective films are used by being attached to other products in the circulation process, play a role in protection, and are torn off and removed when the protective films are circulated to the next link or the process flow; still other protective films are applied to end products and are directly marketed, and the requirements are higher than those of the former; the organic silicon protective film is not selected in the field of electronic protective films by virtue of the advantages of high and low temperature resistance, weather resistance, exhaust and light transmittance. The protective film used in the die cutting process has a good effect when being adhered, but after long-time adhesion and other links or technological processes, the relative peeling force between the protective film and an adhered object is remarkably increased, so that the peeling difficulty occurs in the last link or technological process needing to be torn off. Therefore, we propose a low-climbing silicone protective film and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a low-climbing organic silicon protective film and a preparation method thereof, which aim to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the low-climbing organic silicon protective film comprises a base material, an organic silicon pressure-sensitive adhesive layer and a release film, wherein the organic silicon pressure-sensitive adhesive layer is positioned between the base material and the release film, and the organic silicon pressure-sensitive adhesive comprises the following components in parts by weight: 20-80 parts of non-polar end group raw rubber, 5-20 parts of non-polar end group MQ resin, 1-2 parts of high-viscosity vinyl silicone oil, 0.1-2 parts of a cross-linking agent, 0-1 part of an inhibitor, 0-1 part of an anchoring agent, 0.5-5 parts of a platinum catalyst and 100-400 parts of a solvent.
Further, the non-polar end-group crude rubber has a general formula: r1[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2R2
R1、R2Is a saturated alkyl group of 3 to 10 carbon atoms, a phenyl group or a benzyl group;n and m are positive integers; the molecular weight of the non-polar end group raw rubber is 60-80 ten thousand, and the mole fraction of the vinyl is 0.03-0.3%.
Specific examples of non-polar end-group gums may be, but are not limited to:
and the common crude rubber is R1[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2R2；R1、R2Is methyl or vinyl; n and m are positive integers.
Further, the non-polar end group MQ resin has the general formula: (RSiO)0.5)a(CH3SiO0.5)x-a(SiO2)y；
R is one or more of saturated alkyl with 3-10 carbon atoms, phenyl and benzyl; a. x is even number, and y is positive integer; the value of x/y is 0.5 to 0.9.
Specific examples of non-polar end group MQ resins can be, but are not limited to:
(PhSiO0.5)100(CH3SiO0.5)400(SiO2)1000；
(PhCH2SiO0.5)80(CH3SiO0.5)600(SiO2)1000；
(C3H7SiO0.5)100(CH3SiO0.5)800(SiO2)1000；
(PhSiO0.5)50(C3H7SiO0.5)100(CH3SiO0.5)400(SiO2)1000；
while the general formula of conventional MQ resins is: (CH)3SiO0.5)x(SiO2)y；
Further, the high-viscosity vinyl silicone oil can adjust viscosity and reduce interaction with an attached object. The viscosity of the high-viscosity vinyl silicone oil is 60000-12000 cps, and the mass part of vinyl is 0.3-1%.
Specific examples of the high-viscosity vinyl silicone oil may be, but are not limited to:
further, the cross-linking agent is high hydrogen-containing silicone oil, and the structural formula is as follows:
Furthermore, the mol ratio of SiH/SiVi in the raw materials of the organic silicon pressure-sensitive adhesive is 2.0-6.0. In the raw material components of the organic silicon pressure-sensitive adhesive, the molar ratio of the silicon-hydrogen bond to the silicon-vinyl group is 2.0-6.0.
Further, the inhibitor is one of an alkynol compound, maleic acid and a derivative thereof, and fumaric acid and a derivative thereof.
Further, the anchoring agent is one of 3-glycidyl ether oxypropyl triethoxysilane and 2- (3, 4-epoxycyclohexane) ethyltrimethoxysilane.
Further, the platinum catalyst is a divinyl tetramethyl disiloxane platinum complex, and the platinum content is 2000-8000 ppm.
Further, the solvent is one or a mixture of toluene, xylene and ethyl acetate.
A preparation method of a low-climbing organic silicon protective film comprises the following steps:
(1) putting the non-polar end group raw rubber, the non-polar end group MQ resin and the solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding the high-viscosity vinyl silicone oil, the cross-linking agent, the inhibitor and the anchoring agent, dispersing for 10min, adding the platinum catalyst, and dispersing for 10min to obtain the glue;
(2) and (3) taking the PET film as a base material, coating glue on the base material, curing, superposing a release film, and curing to obtain the protective film.
Further, the curing process in the step (2) is as follows: the curing temperature is 45-85 ℃, and the curing time is 4-72 h.
In the technical scheme, the base material is subjected to corona treatment, no or little anchoring agent is added, the existence of polar molecules in the organic silicon pressure-sensitive adhesive layer can be reduced, and the stability of the organic silicon pressure-sensitive adhesive layer is improved; the curing process is arranged, so that the adhesive layer of the protective film is fully cured, the residue of reactive groups is reduced, and the stability of the adhesive layer is ensured.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the low-climbing organic silicon protective film and the preparation method thereof, the organic silicon pressure-sensitive adhesive is prepared by establishing an organic silicon system and adopting the non-polar end group raw rubber, the non-polar end group MQ resin and the high-viscosity vinyl silicone oil, the content of polar groups is reduced, the interaction between the organic silicon pressure-sensitive adhesive and an adhered object is reduced, and the climbing reduction of stripping force is realized.
2. According to the low-climbing organic silicon protective film and the preparation method thereof, the formula is adjusted through the arrangement of the organic silicon protective film and the proportion thereof, the dosage of the hydrogen-containing silicone oil is controlled, the ratio of SiH to SiVi in the system is limited, the full curing of the organic silicon pressure-sensitive adhesive can be promoted, the residual of reactive groups is reduced, and the stability of the adhesive layer is ensured; after the organic silicon pressure-sensitive adhesive layer is cured, the content of active hydrogen is low, and the interaction between the adhesive layer and a base material can be reduced; the anchoring agent is not added or is added in a small amount, so that the amount of polar molecules in the adhesive layer is reduced, and the interaction between the adhesive layer and the base material is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood 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.
The parts of the components described in the following examples and comparative examples are parts by weight.
Example 1
(1) Adding 20 parts of non-polar end group raw rubber, 10 parts of non-polar end group MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 1 part of high-viscosity vinyl silicone oil, 3 parts of cross-linking agent and 0.1 part of inhibitor, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 2.1;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 70 ℃ for 48 hours to obtain the protective film.
Wherein the solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is an alkynol compound, and the platinum content of the platinum catalyst is 8000 ppm;
the molecular structure of the non-polar end-group crude rubber is C10H21[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2-Ph, molecular weight 60 ten thousand, vinyl mole fraction 0.04%;
the molecular structure of the non-polar end group MQ resin is (PhSiO)0.5)100(CH3SiO0.5)400(SiO2)1000。
Example 2
(1) Adding 20 parts of non-polar end group raw rubber, 10 parts of non-polar end group MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 1 part of high-viscosity vinyl silicone oil, 3 parts of cross-linking agent, 0.1 part of inhibitor and 1 part of anchoring agent, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 2.1;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 70 ℃ for 48 hours to obtain the protective film.
Wherein the solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is an alkynol compound, the anchoring agent is 3-glycidyl ether oxypropyl triethoxysilane, and the platinum content of the platinum catalyst is 8000 ppm;
the molecular structure of the non-polar end-group crude rubber is C10H21[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2-Ph, molecular weight 60 ten thousand, vinyl mole fraction 0.04%;
the molecular structure of the non-polar end group MQ resin is (PhSiO)0.5)100(CH3SiO0.5)400(SiO2)1000。
Example 3
(1) Adding 20 parts of non-polar end group raw rubber, 10 parts of non-polar end group MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 1 part of high-viscosity vinyl silicone oil, 8 parts of cross-linking agent, 0.1 part of inhibitor and 1 part of anchoring agent, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 5.8;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 70 ℃ for 48 hours to obtain the protective film.
Wherein the solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is alkynol compound, and the anchoring agent is 3-glycidyl ether oxypropyl triethoxysilane. The platinum content of the platinum catalyst is 8000 ppm;
the molecular structure of the non-polar end-group crude rubber is C10H21[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2-Ph, molecular weight 60 ten thousand, vinyl mole fraction 0.04%;
the molecular structure of the non-polar end group MQ resin is (PhSiO)0.5)100(CH3SiO0.5)400(SiO2)1000。
Example 4
(2) Adding 20 parts of non-polar end group raw rubber, 10 parts of non-polar end group MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 2 parts of high-viscosity vinyl silicone oil, 5 parts of cross-linking agent and 0.1 part of inhibitor, dispersing for 10min, adding 5 parts of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 3.2;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 45 ℃ for 72 hours to obtain the protective film.
Wherein the solvent is toluene; the inhibitor is maleic acid derivative, and the platinum content of the platinum catalyst is 2000 ppm;
the molecular structure of the non-polar end-group crude rubber is PhCH2[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2-Ph, molecular weight 80 ten thousand, vinyl mole fraction 0.04%;
the molecular structure of the non-polar end group MQ resin is (PhSiO)0.5)50(C3H7SiO0.5)100(CH3SiO0.5)400(SiO2)1000。
Comparative example 1
(1) Adding 20 parts of common raw rubber, 10 parts of common MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 1 part of high-viscosity vinyl silicone oil, 3 parts of cross-linking agent and 0.1 part of inhibitor, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 2.1;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 70 ℃ for 48 hours to obtain the protective film.
Wherein the molecular structure of the common raw rubber is CH3[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2CH3Molecular weight is 60 ten thousand, and vinyl mole fraction is 0.04%; molecular structure of ordinary MQ resinIs (CH)3SiO0.5)500(SiO2)1000；
The solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is an alkynol compound, and the platinum content of the platinum catalyst is 8000 ppm.
Comparative example 2
(1) Adding 20 parts of end phenyl raw rubber, 10 parts of ordinary MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 1 part of high-viscosity vinyl silicone oil, 3 parts of cross-linking agent and 0.1 part of inhibitor, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 2.1;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 70 ℃ for 48 hours to obtain the protective film.
Wherein the molecular structure of the end phenyl crude rubber is Ph [ Si (CH)3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2Ph, molecular weight 60 ten thousand, vinyl mole fraction 0.04%; the molecular structure of the common MQ resin is (CH)3SiO0.5)500(SiO2)1000；
The solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is an alkynol compound, and the platinum content of the platinum catalyst is 8000 ppm.
Comparative example 3
(1) Adding 20 parts of non-polar end group raw rubber, 10 parts of non-polar end group MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 10 parts of high-viscosity vinyl silicone oil, 3 parts of cross-linking agent and 0.1 part of inhibitor, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 7.5;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 70 ℃ for 48 hours to obtain the protective film.
Wherein the solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is an alkynol compound, and the platinum content of the platinum catalyst is 8000 ppm;
the molecular structure of the non-polar end-group crude rubber is C10H21[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2-Ph, molecular weight 60 ten thousand, vinyl mole fraction 0.04%;
the molecular structure of the non-polar end group MQ resin is (PhSiO)0.5)100(CH3SiO0.5)400(SiO2)1000。
Comparative example 4
(1) Adding 20 parts of non-polar end group raw rubber, 10 parts of non-polar end group MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 1 part of high-viscosity vinyl silicone oil, 3 parts of cross-linking agent, 0.1 part of inhibitor and 5 parts of anchoring agent, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 2.1;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing a release film, and curing at 70 ℃ for 48 hours to obtain the protective film.
Wherein the solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is an alkynol compound, and the anchoring agent is 3-glycidyl ether oxypropyl triethoxysilane; the platinum content of the platinum catalyst is 8000ppm
The molecular structure of the non-polar end-group crude rubber is C10H21[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2-Ph, molecular weight 60 ten thousand, vinyl mole fraction 0.04%;
the molecular structure of the non-polar end group MQ resin is (PhSiO)0.5)100(CH3SiO0.5)400(SiO2)1000。
Comparative example 5
(2) Adding 20 parts of non-polar end group raw rubber, 10 parts of non-polar end group MQ resin and 100 parts of solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding 1 part of high-viscosity vinyl silicone oil, 3 parts of cross-linking agent, 0.1 part of inhibitor and 1 part of anchoring agent, dispersing for 10min, adding 1 part of platinum catalyst, and dispersing for 10min to obtain glue, wherein the value of SiH/SiVi in the system is 2.1;
(2) and (3) carrying out corona treatment on the PET film to obtain a base material, coating glue on the base material, curing, superposing the release film, and carrying out no curing to obtain the protective film.
Wherein the solvent is a mixture of toluene, xylene and ethyl acetate; the inhibitor is alkynol compound, and the anchoring agent is 3-glycidyl ether oxypropyl triethoxysilane. The platinum content of the platinum catalyst is 8000 ppm;
the molecular structure of the non-polar end-group crude rubber is C10H21[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2-Ph, molecular weight 60 ten thousand, vinyl mole fraction 0.04%;
the molecular structure of the non-polar end group MQ resin is (PhSiO)0.5)100(CH3SiO0.5)400(SiO2)1000。
Experiment of
Taking the protective films obtained in the examples 1-4 and the comparative examples 1-5, removing the release film to obtain samples, respectively detecting the performances of the copper foil and the glass, and recording the detection results:
wherein: 1. and (3) testing the peeling force: refer to GB/T2792-1998 pressure-sensitive adhesive tape 180 degree peel strength test method;
2. the copper foil used for the test is 25um electrolytic copper foil;
3. testing the peeling force of the copper foil at 85 ℃ for 3 d: placing the sample laminated copper foil into an oven at 85 ℃, taking out after 3d, cooling to the environmental temperature of a laboratory, and then testing the stripping force; the peel force test was similar for copper foil at 85 ℃ for 15 d.
4. The normal temperature in the test on the glass plate is the laboratory ambient temperature.
Table 1: examples 1-4 peel force test data for 25um electrodeposited copper foil
Table 2: comparative examples 1-5 peel force test data for 25um electrolytic copper foil
Table 3: examples 1-4 peel force test data on glass
Table 4: comparative examples 1-5 peel force test data on glass
From the data in the table above, it is clear that the following conclusions can be drawn:
the protective films obtained in examples 1 to 4 are compared with the protective films obtained in comparative examples 1 to 5, and the detection results show that the protective films obtained in examples 1 to 4 have small changes in the peeling force before and after aging, which fully indicates that the invention realizes the reduction of the climbing of the peeling force of the prepared protective films; the climbing of the copper foil and the glass plate is below 30 percent, which can meet the application of different objects to be pasted
Compared with the example 1, the glue is prepared by adopting common raw glue and MQ resin in the comparative example 1, and the glue is prepared by adopting phenyl-terminated raw glue and MQ resin in the comparative example 2; comparative example 3 SiH/SiVi was 8.0; the glue of comparative example 4 was added with an anchoring agent; the glue in the comparative example 5 is not cured, and the peeling force is obviously changed before and after aging, so that the composition and the preparation process thereof are set, and the decrease of the climbing of the peeling force of the prepared protective film can be promoted.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A low-climbing organic silicon protective film is characterized in that: the adhesive comprises a substrate, an organic silicon pressure-sensitive adhesive layer and a release film, wherein the organic silicon pressure-sensitive adhesive layer is positioned between the substrate and the release film, and comprises the following components in parts by weight: 20-80 parts of non-polar end group raw rubber, 5-20 parts of non-polar end group MQ resin, 1-2 parts of high-viscosity vinyl silicone oil, 0.1-2 parts of a cross-linking agent, 0-1 part of an inhibitor, 0-1 part of an anchoring agent, 0.5-5 parts of a platinum catalyst and 100-400 parts of a solvent.
2. A low climb in accordance with claim 1Organosilicon protection film, its characterized in that: the general formula of the non-polar end-group raw rubber is as follows: r1[Si(CH3)2O]n[Si(CH3)(C2H3)O]mSi(CH3)2R2；
R1、R2Is a saturated alkyl group of 3 to 10 carbon atoms, a phenyl group or a benzyl group; n and m are positive integers; the molecular weight of the non-polar end group raw rubber is 60-80 ten thousand, and the mole fraction of the vinyl is 0.03-0.3%.
3. The low-climb silicone protective film according to claim 1, characterized in that: the general formula of the non-polar terminal MQ resin is as follows: (RSiO)0.5)a(CH3SiO0.5)x-a(SiO2)y；
R is one or more of saturated alkyl with 3-10 carbon atoms, phenyl and benzyl; a. x is even number, and y is positive integer; the value of x/y is 0.5 to 0.9.
4. The low-climb silicone protective film according to claim 1, characterized in that: the viscosity of the high-viscosity vinyl silicone oil is 60000-12000 cps, and the mass part of vinyl is 0.3-1%.
5. The low-climbing silicone protective film according to claim 4, wherein: the cross-linking agent is high hydrogen-containing silicone oil; the mol ratio of SiH/SiVi in the raw materials of the organic silicon pressure-sensitive adhesive is 2.0-6.0.
6. The low-climb silicone protective film according to claim 1, characterized in that: the inhibitor is one of alkynol compound, maleic acid and derivatives thereof, and fumaric acid and derivatives thereof.
7. The low-climb silicone protective film according to claim 1, characterized in that: the anchoring agent is one of 3-glycidyl ether oxypropyl triethoxysilane and 2- (3, 4-epoxy cyclohexane) ethyl trimethoxysilane.
8. The low-climb silicone protective film according to claim 1, characterized in that: the platinum catalyst is a divinyl tetramethyl disiloxane platinum complex, and the platinum content is 2000-8000 ppm;
the solvent is one or more of toluene, xylene and ethyl acetate.
9. A preparation method of a low-climbing organic silicon protective film is characterized by comprising the following steps: the method comprises the following steps:
1) putting the non-polar end group raw rubber, the non-polar end group MQ resin and the solvent into a three-neck flask, heating and refluxing for 0.5h under stirring, cooling to room temperature, pouring into a mixing bottle, adding the high-viscosity vinyl silicone oil, the cross-linking agent, the inhibitor and the anchoring agent, dispersing for 10min, adding the platinum catalyst, and dispersing for 10min to obtain the glue;
(2) and taking the PET film as a base material, coating glue on the PET film, curing, superposing a release film, and curing to obtain the protective film.
10. The method for preparing a low-climbing silicone protective film according to claim 9, wherein: the curing process in the step (2) comprises the following steps: the curing temperature is 45-85 ℃, and the curing time is 4-72 h.
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