CN114940877A - High-stability low-small-molecule-migration silica gel protective film - Google Patents
High-stability low-small-molecule-migration silica gel protective film Download PDFInfo
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- CN114940877A CN114940877A CN202210638924.9A CN202210638924A CN114940877A CN 114940877 A CN114940877 A CN 114940877A CN 202210638924 A CN202210638924 A CN 202210638924A CN 114940877 A CN114940877 A CN 114940877A
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- protective film
- vinyl
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- silica gel
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- 230000001681 protective effect Effects 0.000 title claims abstract description 66
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000741 silica gel Substances 0.000 title claims abstract description 42
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 42
- 238000013508 migration Methods 0.000 title claims abstract description 27
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 43
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 40
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 40
- 229920002545 silicone oil Polymers 0.000 claims abstract description 34
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000005012 migration Effects 0.000 claims abstract description 24
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 60
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 30
- 229920005989 resin Polymers 0.000 claims description 28
- 239000011347 resin Substances 0.000 claims description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 22
- 229910052710 silicon Inorganic materials 0.000 claims description 22
- 239000010703 silicon Substances 0.000 claims description 22
- 150000003384 small molecules Chemical class 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 15
- 239000007822 coupling agent Substances 0.000 claims description 14
- 239000003112 inhibitor Substances 0.000 claims description 14
- 229910052697 platinum Inorganic materials 0.000 claims description 14
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- -1 polymethylsiloxane Polymers 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- UEXCJVNBTNXOEH-UHFFFAOYSA-N Ethynylbenzene Chemical group C#CC1=CC=CC=C1 UEXCJVNBTNXOEH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000178 monomer Substances 0.000 claims description 3
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 125000003545 alkoxy group Chemical group 0.000 claims description 2
- NEEDEQSZOUAJMU-UHFFFAOYSA-N but-2-yn-1-ol Chemical compound CC#CCO NEEDEQSZOUAJMU-UHFFFAOYSA-N 0.000 claims description 2
- 125000003700 epoxy group Chemical group 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- HJFRLXPEVRXBQZ-UHFFFAOYSA-N pent-3-yn-2-ol Chemical compound CC#CC(C)O HJFRLXPEVRXBQZ-UHFFFAOYSA-N 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 abstract description 28
- 230000008859 change Effects 0.000 abstract description 22
- 239000004820 Pressure-sensitive adhesive Substances 0.000 abstract description 20
- 238000000576 coating method Methods 0.000 abstract description 18
- 238000004132 cross linking Methods 0.000 abstract description 16
- 238000003825 pressing Methods 0.000 abstract description 8
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000003085 diluting agent Substances 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 description 43
- 238000003756 stirring Methods 0.000 description 37
- 239000000463 material Substances 0.000 description 30
- 238000012360 testing method Methods 0.000 description 26
- 239000000243 solution Substances 0.000 description 19
- 239000011248 coating agent Substances 0.000 description 15
- 239000000499 gel Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000002390 adhesive tape Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 229920001971 elastomer Polymers 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 description 10
- 239000005020 polyethylene terephthalate Substances 0.000 description 10
- 230000002431 foraging effect Effects 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
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- 230000002829 reductive effect Effects 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920001558 organosilicon polymer Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- LTFTWJYRQNTCHI-UHFFFAOYSA-N -1-Hexyn-3-ol Natural products CCCC(O)C#C LTFTWJYRQNTCHI-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000011127 biaxially oriented polypropylene Substances 0.000 description 1
- 229920006378 biaxially oriented polypropylene Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 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
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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 silica gel protective film with high stability and low micromolecule migration; the invention adopts macromolecular siloxane to improve the whole molecular weight distribution of the pressure-sensitive adhesive and reduce the risk of micromolecules, and the vinyl silicone oil with low volatile content and high vinyl content is used as a diluent, and the coating process can be flexibly adjusted through reasonable change of the molecular weight, so that on one hand, the residual quantity of DMC micromolecules can be controlled, and on the other hand, the existence of a large amount of vinyl can ensure that the crosslinking degree of the main glue is compact enough, and the flowing property of the micromolecules in the pressure-sensitive adhesive is prevented as far as possible. The compound cross-linking agent is utilized to further improve the reticular cross-linking density of the dough pressing glue, and the characteristics of the reticular structure of the compound cross-linking agent greatly improve the three-dimensional reticular density of the glue.
Description
Technical Field
The invention relates to the technical field of silica gel protective films, in particular to a silica gel protective film with high stability and low micromolecule migration.
Background
The organic silicon pressure-sensitive adhesive is an adhesive suitable for coating films and fabrics and consists of polydimethylsiloxane silica gel, silicone resin, filler and organic solvent, wherein the polydimethylsiloxane silica gel (polymer) and the silicone resin (tackifying resin) mainly consist of the polydimethylsiloxane silica gel and the silicone resin. The adhesive has excellent viscosity, initial viscosity, high viscosity, moisture resistance, aging resistance, ultraviolet ray, oil resistance, acid and alkali resistance and the like, has good electrical performance, can be used for bonding materials with low surface tension, and can be used for coating textile materials. The glass transition temperature of siloxane is-120 ℃, so that the excellent low-temperature resistance of the siloxane is determined, and the organosilicon high polymer material has excellent temperature resistance and weather resistance due to the fact that the bond energy (450kJ/mol) of Si-O bonds is much higher than that of C-C bonds (350kJ/mol) and C-O bonds (360 kJ/mol). The organic silicon pressure-sensitive adhesive can be bonded with a low surface energy surface due to good high and low temperature resistance, chemical resistance and low dielectric property. The organic silicon pressure-sensitive adhesive tape can be widely applied to industrial production in the forms of splicing tapes, electrical tapes, plasma spraying tapes, machining tapes and the like. Silicone pressure sensitive adhesives and tapes thereof are commonly used in Printed Circuit Board (PCB) production and assembly processes. The organic silicon pressure-sensitive adhesive generally refers to a pressure-sensitive adhesive using an organic silicon polymer as a main body, or an acrylic acid and organic silicon modified rubber type pressure-sensitive adhesive modified by the organic silicon polymer. Compared with the traditional acrylate pressure-sensitive adhesive and rubber pressure-sensitive adhesive, the pressure-sensitive adhesive has excellent performances of chemical resistance, water resistance, oil resistance, solvent resistance, high temperature resistance, low temperature resistance, thermal degradation resistance, oxidative degradation resistance and the like, and can be bonded with various materials which are difficult to bond, such as polyolefin (BOPP, PET, PE and the like) fluoroplastics, polyimide, polycarbonate and the like which are not subjected to surface treatment.
At present, for some electronic products, in the process of manufacturing, shipping or using, the surface of the product is relatively easy to be polluted by contact of some chemical substances or scratched by grinding marks such as nails and the like; in order to reduce or prevent the surface of the electronic product from being damaged or contaminated during the use or manufacturing process, a protective film is usually attached to the surface for protection, and a silicone protective film is commonly used in the manufacturing process and shipment of the electronic product.
The organosilicon protective film is low-viscosity organosilicon silica gel glue coated on the surface of a base material, and the formula of the glue is characterized in that macromolecular siloxane is used as a main body, a small amount of MQ silicon resin is used for adjusting viscosity, and auxiliary agents such as a cross-linking agent, a coupling agent, a catalyst and the like are used for cross-linking to form a film. It is suitable for various screen protection, maintenance of computer keyboard in production process, and protection of low static electricity requirement. LCD, LCM screen appearance protection and antidetonation protection effect, use electronic screen, car appearance, shell etc., air conditioner appearance and various domestic appliance appearance protection, too tight belongs to board, optics piece, optics resin board etc. and the surface protection effect.
Although the silica gel protective film has various advantages which are not possessed by other types of protective films and can fully meet most scene applications, in part of process standards with extremely high requirements, silica gel also has a defect of the silica gel, namely, silicon transfer. In the using process of the common silica gel protective film, a layer of micromolecular silicone oil is remained on the surface of an attached object through a certain temperature and humidity process, and the common silica gel protective film is not influenced for general application, and for products requiring higher processes or needing subsequent surface processing, a plurality of quality problems are generated due to the fact that the micromolecular silicone oil is remained much, because the surface energy of siloxane is very low, the surface tension of dimethyl silicone oil is about 21 dynes, and compared with 38 dynes of an acrylic acid system, the surface tension is much lower, the remanufacturing process and coating of other coatings or printing ink are influenced, and various defects such as shrinkage cavities, falling and the like are generated in the coating. Therefore, the development of the silica gel protective film with low silicon transfer must become the subsequent development direction in the industry.
The main silicone rubber of the organic silicon pressure-sensitive adhesive is mainly prepared by synthesizing a chain extender and a small amount of end socket agent by using micromolecular DMC (dimethyl cyclosiloxane mixture), because 100% of micromolecular monomers can not participate in the reaction in the synthesis process, a small amount of micromolecular silicone oil always remains in the system, generally within 2%, and in addition, a small molecule auxiliary agent is also used in the protective film formula process, so that the existence of the micromolecular silicone oil in the whole protective film system can not be avoided, and the micromolecular silicone oil can slowly migrate to the surface under a certain high-temperature high-humidity environment and finally remains on the surface of an object to be stuck to form an extremely thin silicone oil layer, namely the so-called silicon pollution. Because the surface energy of the siloxane is very low, the siloxane has poor compatibility with glue or ink of other systems, and great hidden danger is caused to the subsequent processing procedure and coating of the surface.
Therefore, it is necessary to provide a silica gel protective film with high stability and low small molecule migration.
Disclosure of Invention
The invention aims to provide a silica gel protective film with high stability and low small molecule migration so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a silica gel protective film with high stability and low micromolecule migration consists of the following components:
by weight, 100 parts of macromolecular siloxane, 0-100 parts of vinyl silicone oil, 0-100 parts of tackifying resin, 0.5-3 parts of cross-linking agent A, 0.1-2 parts of cross-linking agent B, 0.4-4 parts of coupling agent, 0.06-2 parts of inhibitor, 1-5 parts of platinum catalyst and 300-700 parts of solvent.
Furthermore, the macromolecular siloxane is high-functional group long-chain siloxane with a vinyl-terminated side group and a vinyl group, and the molecular weight of the macromolecular siloxane is 300000-800000.
Further, the general structural formula is ViMe 2 SiO(SiMe 2 O)n(SiMeViO)mSiMe 2 Vi, wherein m and n are positive integers; the vinyl content is 0.0037 to 0.185mol/100 g.
Further, the vinyl silicone oil is vinyl-terminated polymethylsiloxane with a side group containing vinyl, and the molecular weight of the vinyl silicone oil is 10000-100000; the vinyl content is 0.005-0.15 mol/100 g; the volatile component is less than 0.5 percent.
Furthermore, the tackifying resin is MQ resin containing vinyl, the molar mass of which is 3000-8000 and the M/Q chain link ratio of which is 0.7-0.85.
Further, the cross-linking agent A is hydrogen-containing silicone oil with high hydrogen content and low volatile content and containing Si-H in a side group, the molar mass of the hydrogen-containing silicone oil is 400-1000, and the structural general formula of the hydrogen-containing silicone oil is Me 3 SiO(SiMe 2 O)n(SiMeHO)mSiMe 3 Wherein m and n are positive integers; the content of the volatile micromolecules is 0.1-1.5%.
Further, the content of Si-H bonds in the hydrogen-containing silicone oil is 1.5-1.6 mol/100 g.
Further, the cross-linking agent B is hydrogen-containing MQ silicon resin containing Si-H bonds, and the molar mass of the hydrogen-containing MQ silicon resin is 1000-8000.
Further, the content of Si-H bonds of the hydrogen-containing MQ silicon resin is 0.01-1 mol/100 g; the M/Q chain link ratio of the hydrogen-containing MQ silicon resin is 0.75-0.85.
Further, the coupling agent is a silane coupling agent with one end containing an epoxy group or a vinyl group and the other end containing an alkoxy group; comprises one or more of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma- (2, 3-epoxypropoxy) propyl triethoxy silane, vinyl trimethoxy silane and vinyl triethoxy silane.
Further, the inhibitor refers to a monomer containing unsaturated bonds such as triple bonds or double bonds, and comprises one or more of 2-butyn-1-ol, 1-methyl-butyn-3-ol, 1-alkynylcyclohexanol, maleic anhydride, tetramethyltetravinylcyclotetrasiloxane, tetramethyldivinyldisiloxane, phenylacetylene and 5-dimethyl-1-hexyn-3-ol. Among them, the disclosed classes of inhibitors include, but are not limited to.
Further, the platinum catalyst is a vinyl complex in which Pt is coordinated to an unsaturated bond; the solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate and alkane. Among them, the solvent disclosed includes, but is not limited to.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, macromolecular siloxane is selected as a main body of the pressure-sensitive adhesive, so that the overall molecular weight distribution of the pressure-sensitive adhesive is improved, and the risk of small molecules is reduced; matching with micromolecular vinyl silicone oil as a diluent to flexibly adjust a coating process and control the residual quantity of the DMC (dimethyl cyclosiloxane mixture) micromolecules; the vinyl content and the molecular weight of the two substances are accurately controlled, so that the problem that the inhibition capacity of siloxane with too low molecular weight on small molecules is not enough and the pressure-sensitive performance of colloid is not good due to the siloxane with too high molecular weight is solved; the viscosity is adjusted by adjusting the molecular weight of the vinyl silicone oil, so that the large molecules and the small molecules are easily combined. The purpose of controlling the content of the vinyl group is to achieve the performance of preventing the small molecules in the pressure-sensitive adhesive from flowing. The influence of the small molecule residue on the performance of the silica gel protective film in the using process is simultaneously inhibited from the aspects of molecular weight distribution and molecular flow performance.
The invention finely divides the vinyl content of macromolecular siloxane and the Si-H bond content of a cross-linking agent A and a cross-linking agent B in order to better generate hydrosilylation cross-linking reaction between Si-H bonds and Si-Vi bonds on organic silicon. When the content of Si-H bonds is too large or the content of Si-Vi bonds is too small, the hydrogen-containing silicone oil is easy to self-polymerize under the action of a platinum catalyst to generate hydrogen and form bubbles, and the hydrogen-containing silicone oil belongs to a small molecular substance and is easy to cause too strong dilution effect when being used too much, so that the reticular crosslinking density of the pressure-sensitive adhesive is reduced, and the performance of the silica gel protective film is influenced; when the content of Si-Vi bonds is too large or the content of Si-H bonds is too small, the pressure-sensitive adhesive is insufficient in crosslinking, cohesive failure occurs due to insufficient cohesive strength, and the performance of the silica gel protective film is affected.
The invention selects the substances with low volatile components as the preparation raw materials, thereby effectively reducing the generation of bubbles in the reaction process; meanwhile, the control of the vinyl content and the M/Q chain link ratio plays a proper role in reinforcing the pressure-sensitive adhesive. When the M/Q value is smaller, more inorganic components exist in the MQ silicon resin, the MQ silicon resin is ionic, the dispersion effect is uneven, and the compatibility is poorer; when the M/Q value is large, the organic component is substantially large and can be uniformly dispersed in the alternation, but the reinforcing effect is deteriorated due to the decrease of the rigid inorganic core. The increase of the vinyl content can generate a centralized crosslinking effect, and when the external force action is, the force can be uniformly dispersed on the molecular chain through the crosslinking point, so that the colloid strength is enhanced. When the vinyl content is too high, the network density becomes too high, and the strength is lowered due to uneven stress caused by uneven distribution of the crosslinking points.
The existence of a large amount of vinyl in the invention can ensure that the crosslinking degree of the main body glue is sufficiently compact, the compound crosslinking agent formed by combining the crosslinking agent A and the crosslinking agent B further improves the net crosslinking density of the pressure-sensitive adhesive, and the three-dimensional net density of the adhesive is greatly improved by the characteristics of the network structure of the adhesive.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
Example 1
Adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 200 parts of toluene, 20 parts of tackifying resin and 50 parts of vinyl silicone oil, adding the next material after adding one material and stirring for 1 hour, sequentially adding 3 parts of cross-linking agent A, 2 parts of cross-linking agent B, 1 part of coupling agent and 1 part of inhibitor after stirring uniformly, stirring for 15 minutes at intervals for each material, finally adding 5 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
Example 2
Adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 180 parts of toluene, 75 parts of tackifying resin and 30 parts of vinyl silicone oil, adding the next material after adding one material and stirring for 1 hour, uniformly stirring, sequentially adding 2.8 parts of cross-linking agent A, 1.1 parts of cross-linking agent B, 0.66 part of coupling agent and 1.45 parts of inhibitor, stirring for 15 minutes at intervals for each material, finally adding 3.0 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
Example 3
Adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear type dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 250 parts of toluene, 50 parts of tackifying resin and 50 parts of vinyl silicone oil, adding the next material after adding one material and stirring for 1 hour, uniformly stirring, sequentially adding 1.5 parts of cross-linking agent A, 0.8 part of cross-linking agent B, 0.65 part of coupling agent and 0.9 part of inhibitor, stirring for 15 minutes at intervals, finally adding 3.5 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
Example 4
Adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear type dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 100 parts of toluene, 10 parts of tackifying resin and 28 parts of vinyl silicone oil, adding the next material after each material is added and stirring for 1 hour, uniformly stirring, sequentially adding 2.1 parts of cross-linking agent A, 0.3 part of cross-linking agent B, 2.5 parts of coupling agent and 0.55 part of inhibitor, stirring for 15 minutes at intervals for each material, finally adding 2.8 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
Example 5:
adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 100 parts of toluene, 10 parts of tackifying resin and 100 parts of vinyl silicone oil, adding the next material after each material is added and stirring for 1 hour, uniformly stirring, sequentially adding 3.1 parts of cross-linking agent A, 0.3 part of cross-linking agent B, 2.5 parts of coupling agent and 0.62 part of inhibitor, stirring for 15 minutes at intervals for each material, finally adding 3.3 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
Example 6:
adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear type dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 100 parts of toluene and 10 parts of tackifying resin, adding the next material after adding one material and stirring for 1 hour, sequentially adding 0.5 part of cross-linking agent A, 0.1 part of cross-linking agent B, 1.5 parts of coupling agent and 0.35 part of inhibitor after stirring uniformly, stirring for 15 minutes at intervals for each material, finally adding 1.6 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
Comparative example 1
Adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 100 parts of toluene, 10 parts of tackifying resin and 100 parts of vinyl silicone oil with the volatile content of 2%, stirring for 1 hour after adding one material, then adding the next material, stirring for 1 hour again, stirring uniformly, sequentially adding 3.1 parts of cross-linking agent A, 0.3 part of cross-linking agent B, 2.5 parts of coupling agent and 0.62 part of inhibitor, stirring for 15 minutes at intervals for each material, finally adding 3.3 parts of platinum catalyst, and continuing stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
Comparative example 2
The content of the crosslinking agent ASi-H bond is 0.8mol/100 g;
adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 250 parts of toluene, 50 parts of tackifying resin and 50 parts of vinyl silicone oil, adding the next material after each material is added and stirring for 1 hour, uniformly stirring, sequentially adding 1.5 parts of cross-linking agent (Si-H content is 0.8mol/100g), 0.8 part of cross-linking agent B, 0.65 part of coupling agent and 0.9 part of inhibitor, stirring for 15 minutes at intervals for each material, finally adding 3.5 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50uPET (polyethylene terephthalate) substrate, curing at 150 ℃ for 60s at the thickness of 10u dry glue to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the diffusion sheet to a standard adhesive tape.
Comparative example 3
Adding 233.3 parts of toluene into 100 parts of macromolecular siloxane, dispersing for 4 hours by using a shear type dispersion machine, dissolving into 30% crude rubber solution, sequentially adding 180 parts of toluene, 75 parts of tackifying resin and 30 parts of vinyl silicone oil, adding the next material after adding one material and stirring for 1 hour, uniformly stirring, sequentially adding 3.5 parts of cross-linking agent A, 0.66 part of coupling agent and 1.45 parts of inhibitor, stirring for 15 minutes at intervals for each material, finally adding 3.0 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50u PET substrate, curing at 150 ℃ for 60s with the thickness of dry glue of 10u to obtain a silica gel protective film with low micromolecule migration, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing the diffusion sheet in a constant temperature and humidity box 6090 for aging for 3d, and testing the water drop angle change before and after attaching the surface of the diffusion sheet and the viscosity change of the standard adhesive tape.
The related test method comprises the following steps:
1. gel content test (reference national standard: GB/T37498-2019)
2. Surface water contact angle change test of diffusion sheet of attached object
1) And (3) attaching the protective film to the surface of the specified diffusion sheet, pressing the surface of the specified diffusion sheet by using a 2kg roller for 3 times at a pressing speed of 600mm/min, and placing the diffusion sheet in a constant-temperature and constant-humidity box for damp-heat aging under the aging condition of 60903d after attachment.
2) Taking out the sample, standing for 2 hours in a standard environment, uncovering the protective film, and testing a water contact angle theta 1; (ii) a
3) Testing the water contact angle theta 2 of the surface of the original diffusion sheet;
4) water contact angle change delta theta 1-theta 2
3. Viscous decay Rate test
1) And (3) attaching the protective film to the surface of the specified diffusion sheet, pressing the surface of the specified diffusion sheet by using a 2kg roller for 3 times at a pressing speed of 600mm/min, and placing the diffusion sheet in a constant-temperature and constant-humidity box for damp-heat aging under the aging condition of 60903d after attachment.
2) Taking out the sample and standing for 2 hours in a standard environment;
3) the stripping force of the aged diffusion sheet is tested by taking a Nidong 31B adhesive tape as a standard adhesive tape, and the specific method is as follows:
uncovering the protective film on the aged diffusion sheet, attaching a standard adhesive tape on the uncovered area of the diffusion sheet, pressing the diffusion sheet for 3 times by using a 2kg roller, wherein the pressing speed is 600mm/min, standing the diffusion sheet for 20min in a standard environment, and testing the relative peeling force F1;
4) testing the peeling force F2 of the standard adhesive tape to the original diffusion sheet;
5) viscous attenuation rate calculation method: the attenuation rate was (1-F1/F2) × 100%.
And (3) testing the gel content:
| gel content (%) | |
| Example 1 | 98.88 |
| Example 2 | 98.42 |
| Example 3 | 99.05 |
| Example 4 | 98.75 |
| Example 5 | 98.98 |
| Example 6 | 99.02 |
| Comparative example 1 | 97.12 |
| Comparative example 2 | 96.89 |
| Comparative example 3 | 96.77 |
Change of water contact angle on the surface of the diffusion sheet:
viscosity decay rate:
| F1 | F2 | (1-F1/F2)*100％ | |
| example 1 | 481 | 541 | 11.1％ |
| Example 2 | 469 | 541 | 13.3％ |
| Example 3 | 475 | 541 | 12.2％ |
| Example 4 | 470 | 541 | 13.12％ |
| Example 5 | 466 | 541 | 13.86％ |
| Example 6 | 480 | 541 | 11.28％ |
| Comparative example 1 | 413 | 541 | 23.65％ |
| Comparative example 2 | 411 | 541 | 24.03％ |
| Comparative example 3 | 402 | 541 | 25.69％ |
And (4) conclusion:
in examples 1-6, the macromolecular siloxane is a linear structure with a structural formula of-Si-O-Si-, a side group contains-Me and-Vi groups, and the macromolecular siloxane has the characteristics of low content of micromolecules, long-chain flexibility, low surface energy and good wettability. The relative content of small molecules is reduced from the whole formula system; the existence of a large amount of vinyl increases the cross-linking points of the silica gel system, so that the cross-linked network structure is more compact, and the migration fluidity of small molecules in the silica gel system is favorably reduced; the compound cross-linking agent consisting of the cross-linking agent A and the cross-linking agent B is utilized to further improve the net cross-linking density of the dough pressing glue, the net structure characteristics of the hydrogen-containing MQ silicon resin greatly improve the three-dimensional net density of the glue, and the gel content can be more than 98 percent; the low-volatile vinyl silicone oil can flexibly adjust the relation between the solid content and the viscosity of the glue, and can meet the coating requirements of different thicknesses and different solid contents in the process.
In comparative example 1, the conventional vinyl silicone oil with a higher volatile content was used as a diluent, and the small analytical transfer amount of the protective film bonding interface was higher due to the higher small molecule content.
In comparative example 2, the Si-H content of the crosslinking agent A was changed to 0.8mol/100g, and the Si-H density was reduced, so that the degree of crosslinking was not dense enough to inhibit the flow of small molecules in the gel layer, thereby increasing the amount of silicon transferred.
In comparative example 3, only one crosslinking agent is used, the crosslinking degree is not compact enough, which is not beneficial to inhibiting the precipitation of small molecules, and the situation that the crosslinking density is not compact enough, which leads to the unsatisfactory small analysis control can also occur.
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, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (12)
1. A silica gel protection film of low small molecule migration of high stability which characterized in that: the composition consists of the following components:
by weight, 100 parts of macromolecular siloxane, 0-100 parts of vinyl silicone oil, 0-100 parts of tackifying resin, 0.5-3 parts of cross-linking agent A, 0.1-2 parts of cross-linking agent B, 0.4-4 parts of coupling agent, 0.06-2 parts of inhibitor, 1-5 parts of platinum catalyst and 300-700 parts of solvent.
2. The protective film of high-stability low-small-molecule-migration silica gel according to claim 1, wherein: the macromolecular siloxane is vinyl-terminated high-functional group long-chain siloxane with a side group containing vinyl, and the molecular weight of the macromolecular siloxane is 300000-800000.
3. The protective film of silica gel with high stability and low small molecule migration according to claim 2, wherein: the general formula of the structure is ViMe 2 SiO(SiMe 2 O)n(SiMeViO)mSiMe 2 Vi, wherein m and n are positive integers; the vinyl content is 0.0037 to 0.185mol/100 g.
4. The protective film of silica gel with high stability and low small molecule migration according to claim 1, wherein: the vinyl silicone oil is vinyl-terminated polymethylsiloxane with a side group containing vinyl, and the molecular weight of the vinyl silicone oil is 10000-100000; the vinyl content is 0.005-0.15 mol/100 g; the volatile component is less than 0.5 percent.
5. The protective film of silica gel with high stability and low small molecule migration according to claim 1, wherein: the tackifying resin is MQ resin containing vinyl, the molar mass of which is 3000-8000 and the M/Q chain link ratio of which is 0.7-0.85.
6. The protective film of silica gel with high stability and low small molecule migration according to claim 1, wherein: the cross-linking agent A is hydrogen-containing silicone oil with high hydrogen content and low volatile content and a structural general formula of Me, wherein the molar mass of the cross-linking agent A is 400-1000, and a side group contains Si-H 3 SiO(SiMe 2 O)n(SiMeHO)mSiMe 3 Wherein m and n are positive integers; the content of the volatile micromolecules is 0.1-1.5%.
7. The protective film of claim 6, wherein the protective film comprises: the Si-H bond content of the hydrogen-containing silicone oil is 1.5-1.6 mol/100 g.
8. The protective film of silica gel with high stability and low small molecule migration according to claim 1, wherein: the cross-linking agent B is hydrogen-containing MQ silicon resin containing Si-H bonds with the molar mass of 1000-8000.
9. The protective film of claim 8, wherein the protective film comprises: the Si-H bond content of the hydrogen-containing MQ silicon resin is 0.01-1 mol/100 g; the M/Q chain link ratio of the hydrogen-containing MQ silicon resin is 0.75-0.85.
10. The protective film of silica gel with high stability and low small molecule migration according to claim 1, wherein: the coupling agent is a silane coupling agent with one end containing epoxy group or vinyl and the other end containing alkoxy; comprises one or more of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, gamma- (2, 3-epoxypropoxy) propyl triethoxy silane, vinyl trimethoxy silane and vinyl triethoxy silane.
11. The protective film of silica gel with high stability and low small molecule migration according to claim 1, wherein: the inhibitor is a monomer containing unsaturated bonds such as triple bonds or double bonds, and comprises one or more of 2-butyn-1-ol, 1-methyl-butyn-3-ol, 1-alkynyl cyclohexanol, maleic anhydride, tetramethyl tetravinylcyclotetrasiloxane, tetramethyl divinyl disiloxane, phenylacetylene and 5-dimethyl-1-hexynyl-3-ol.
12. The protective film of silica gel with high stability and low small molecule migration according to claim 1, wherein: the platinum catalyst is a vinyl complex formed by coordination of Pt and an unsaturated bond; the solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate and alkane.
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