CN114940877B - Silica gel protection film of high stability low micromolecule migration - Google Patents
Silica gel protection film of high stability low micromolecule migration Download PDFInfo
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- CN114940877B CN114940877B CN202210638924.9A CN202210638924A CN114940877B CN 114940877 B CN114940877 B CN 114940877B CN 202210638924 A CN202210638924 A CN 202210638924A CN 114940877 B CN114940877 B CN 114940877B
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- Prior art keywords
- vinyl
- parts
- silica gel
- protective film
- gel protective
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000000741 silica gel Substances 0.000 title claims abstract description 40
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 40
- 230000005012 migration Effects 0.000 title claims abstract description 22
- 238000013508 migration Methods 0.000 title claims abstract description 22
- 230000001681 protective effect Effects 0.000 claims abstract description 60
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 44
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 39
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 35
- 229920002545 silicone oil Polymers 0.000 claims abstract description 33
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000003384 small molecules Chemical class 0.000 claims abstract description 19
- 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 26
- 239000011347 resin Substances 0.000 claims description 26
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon 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
- -1 polymethylsiloxane Polymers 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 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
- 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
- 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
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 claims description 2
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 239000003292 glue Substances 0.000 abstract description 33
- 230000008859 change Effects 0.000 abstract description 22
- 239000004820 Pressure-sensitive adhesive Substances 0.000 abstract description 19
- 238000000576 coating method Methods 0.000 abstract description 18
- 238000004132 cross linking Methods 0.000 abstract description 16
- 239000000853 adhesive Substances 0.000 abstract description 8
- 230000001070 adhesive effect Effects 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 30
- 239000000463 material Substances 0.000 description 30
- 238000012360 testing method Methods 0.000 description 26
- 238000003756 stirring Methods 0.000 description 25
- 239000011248 coating agent Substances 0.000 description 16
- 239000002390 adhesive tape Substances 0.000 description 13
- 239000000499 gel Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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 10
- 239000000758 substrate Substances 0.000 description 10
- 230000002431 foraging effect Effects 0.000 description 9
- 238000010008 shearing Methods 0.000 description 9
- 238000003825 pressing Methods 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 229920002050 silicone resin Polymers 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000012752 auxiliary agent 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
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 229920005573 silicon-containing polymer Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- 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 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000703 anti-shock Effects 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 238000013016 damping Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 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
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 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
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000003973 paint Substances 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
- 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
- 239000002994 raw material Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- 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
Abstract
The invention discloses a silica gel protective film with high stability and low small molecule migration; according to the invention, macromolecular siloxane is adopted, so that the overall molecular weight distribution of the pressure-sensitive adhesive can be improved, the risk of micromolecules is reduced, the vinyl silicone oil with low volatile component and high vinyl content is used as a diluent, and the coating process can be flexibly adjusted through reasonable change of 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 groups can ensure that the crosslinking degree of main glue is compact enough, and the flowing property of the micromolecules in the pressure-sensitive adhesive can be prevented as much as possible. The compound cross-linking agent is utilized to further improve the reticular cross-linking density of the laminated adhesive, and the self reticular structure characteristic of the laminated adhesive greatly improves the three-dimensional reticular density of the adhesive.
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 small molecule migration.
Background
The organosilicon 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 adhesive mainly consists of polydimethylsiloxane silica gel (polymer) and silicone resin (tackifying resin). Excellent adhesion and initial adhesion, high viscosity, moisture resistance, aging resistance, ultraviolet light resistance, oil resistance, acid and alkali resistance and the like, has good electrical performance, can be adhered to materials with low surface tension, and can be used for coating textile materials. The glass transition temperature of the siloxane is-120 ℃, and the excellent low temperature resistance is determined, and the organic silicon polymer material has excellent temperature resistance and weather resistance because the bond energy (450 kJ/mol) of the Si-O bond is much higher than that of the C-C bond (350 kJ/mol) and the C-O bond (360 kJ/mol). The organic silicon pressure-sensitive adhesive has better high and low temperature resistance, chemical resistance and low dielectric property, and can be used for bonding low-surface-energy surfaces. This has led to the widespread use of silicone pressure-sensitive adhesive tapes in industrial production in the form of splicing tapes, electrical tapes, plasma-sprayed tapes, machining tapes, etc. Silicone pressure sensitive adhesives and tapes thereof are commonly used in Printed Circuit Board (PCB) production and assembly processes. The silicone pressure-sensitive adhesive generally refers to a pressure-sensitive adhesive using a silicone polymer as a main body, or an acrylic and silicone modified rubber type pressure-sensitive adhesive modified with a silicone polymer. Compared with the traditional acrylic pressure-sensitive adhesive and rubber pressure-sensitive adhesive, the 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 be bonded, such as polyolefin (BOPP, PET, PE and the like) fluoroplastic, polyimide, polycarbonate and the like which are not subjected to surface treatment.
Currently, for some electronic products, the surface of the product is more easily scratched by contact pollution of some chemical substances or abrasion marks such as nails in the process of manufacture, shipment or use; in order to reduce or avoid the damage or pollution to the surface of the electronic product during the use or the manufacturing process, a protective film is usually attached to the surface of the electronic product for protection, and a silica gel protective film is commonly used in the manufacturing process and the shipment of the type of product.
The organosilicon protective film is prepared by coating low-viscosity organosilicon silica gel glue on the surface of a substrate, 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 matched 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. The method is suitable for protecting various screens, protecting computer keyboards of production process workers and the like, and protecting the appearance with low electrostatic requirements. LCD, LCM screen appearance protection and anti-shock protection effect, use electronic screen, automobile appearance, shell etc., air conditioner appearance and various household appliances appearance protection, too tight belting plate, optical sheet, optical resin plate etc.
Although the silica gel protective film has various advantages not possessed by other types of protective films and can fully satisfy most of scene applications, silica gel has its own defect, namely silicon transfer, in part of extremely high-demand process standards. In the use process of the common silica gel protective film, a layer of small molecular silicone oil is remained on the surface of an object to be adhered through a certain temperature and humidity process, so that the common application is not influenced, and various quality problems can be caused by more small molecular silicone oil residues for products requiring a higher process or requiring subsequent surface processing, because the surface energy of siloxane is very low, the surface tension of the dimethyl silicone oil is about 21 dynes, and compared with the 38 dynes value of an acrylic acid system, the surface tension of the dimethyl silicone oil is very much lower, the re-processing and coating of other paint or ink are influenced, and various defects such as shrinkage cavity, falling and the like can be caused in the coating. Therefore, the development of the silica gel protective film with low silicon transfer is certainly the subsequent development direction in the industry.
The organic silicon pressure-sensitive adhesive main body silicone rubber is mainly prepared by synthesizing small molecular DMC (dimethyl cyclosiloxane mixture) serving as a chain extender and a small amount of end enclosure agent, and because the small molecular monomer cannot participate in the reaction by 100% in the synthesis process, a small amount of small molecular silicone oil always remains in the system, generally within 2%, and a small molecular auxiliary agent is also used in the formula process of the protective film, so that the existence of the small molecular silicone oil in the whole protective film system is unavoidable, the small molecular silicone oil can slowly migrate to the surface in a certain high-temperature and high-humidity environment and finally remains on the surface of an object to be adhered to form an extremely thin silicone oil layer, namely the silicon pollution. Because of its low surface energy of siloxanes, it has poor compatibility with other systems of glues or inks, which can cause significant potential hazards to subsequent processing and coating of the surface.
Therefore, it is necessary to provide a silica gel protective film with high stability and low migration of small molecules.
Disclosure of Invention
The invention aims to provide a silica gel protective film with high stability and low small molecular 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 small molecular migration consists of the following components:
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.
Further, the macromolecular siloxane is a high functional long chain siloxane having vinyl terminated side groups and also containing vinyl groups, and has a molecular weight of 300000 ～ 800000.
Further, the structural general formula is ViMe 2 SiO(SiMe 2 O)n(SiMeViO)mSiMe 2 Vi, wherein m and n are positive integers; the vinyl content is 0.0037-0.185 mol/100g.
Further, the vinyl silicone oil refers to vinyl-terminated polymethylsiloxane with vinyl groups on side groups, and the molecular weight of the vinyl silicone oil is 10000-100000; vinyl content is 0.005-0.15 mol/100g; volatile less than 0.5%.
Further, the tackifying resin is a vinyl-containing MQ resin having a molar mass of 3000-8000 and an M/Q mer ratio of 0.7-0.85.
Further, the cross-linking agent A is hydrogen-containing silicone oil with high hydrogen content and low volatile component and Si-H-containing side group with molar mass of 400-1000 and has the structural general formula of Me 3 SiO(SiMe 2 O)n(SiMeHO)mSiMe 3 Wherein m and n are positive integers; the content of the volatilizable micromolecules is 0.1 to 1.5 percent.
Further, the Si-H bond content of the hydrogen-containing silicone oil is 1.5-1.6 mol/100g.
Further, the crosslinking agent B refers to hydrogen-containing MQ silicone resin containing Si-H bonds, wherein the molar mass of the hydrogen-containing MQ silicone resin is 1000-8000.
Further, the Si-H bond content of the hydrogen-containing MQ silicon resin is 0.01-1 mol/100g; 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 epoxy group or vinyl group and the other end containing alkoxy group; comprises one or more of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, gamma- (2, 3-glycidoxy) propyl triethoxy silane, vinyl trimethoxy silane and vinyl triethoxy silane.
Further, the inhibitor is a monomer containing triple bonds or double bonds and other unsaturated bonds, and comprises one or more of 2-butyn-1-ol, 1-methyl-butyn-3-ol, 1-alkynyl cyclohexanol, maleic anhydride, tetramethyl tetravinyl cyclotetrasiloxane, tetramethyl divinyl disiloxane, phenylacetylene and 5-dimethyl-1-hexynyl-3-ol. Among these, the types of inhibitor disclosures include, but are not limited to.
Further, the platinum catalyst is a vinyl complex formed by coordination of Pt and unsaturated bonds; the solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate and alkanes. Among them, the solvent disclosure category includes, but is not limited to.
Compared with the prior art, the invention has the following beneficial effects: the invention selects macromolecular siloxane as the main body of the pressure-sensitive adhesive to improve the overall molecular weight distribution of the pressure-sensitive adhesive and reduce the risk of micromolecules; the coating process is flexibly adjusted by matching with small molecular vinyl silicone oil as a diluent, and the residual quantity of DMC (dimethyl cyclosiloxane mixture) small molecules is controlled; the vinyl content and the molecular weight of the two substances are accurately controlled, so that the aim is to prevent the insufficient small molecule inhibition capability of siloxane with too low molecular weight, which can cause poor pressure-sensitive performance of colloid; the viscosity is regulated by regulating the molecular weight of vinyl silicone oil, so that the combination of large and small molecules is easy. The vinyl content is controlled to achieve the effect of preventing the flow of small molecules inside the pressure sensitive adhesive. The influence of the residual small molecules on the performance of the silica gel protective film in the use process is simultaneously inhibited from the two 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 the cross-linking agent A and the cross-linking agent B, so that Si-H bond and Si-Vi bond on organosilicon can better generate hydrosilylation cross-linking reaction. When the content of Si-H bonds is too large or the content of Si-Vi bonds is too small, hydrogen-containing silicone oil is easy to self-polymerize under the action of a platinum catalyst to generate hydrogen so as to form bubbles, and the hydrogen-containing silicone oil belongs to small molecular substances, so that too much hydrogen-containing silicone oil is easy to dilute, the net-shaped crosslinking density of the pressure-sensitive adhesive is reduced, and the performance of the silica gel protective film is affected; when the Si-Vi bond content is too large or the Si-H bond content is too small, insufficient crosslinking of the pressure-sensitive adhesive can be caused, cohesive failure occurs due to insufficient cohesive strength, and the performance of the silica gel protective film is affected.
The invention selects low volatile matters as the preparation raw materials, thereby effectively reducing the generation of bubbles in the reaction process; simultaneously, the vinyl content and the M/Q chain link ratio are controlled to play a proper role in reinforcing the pressure-sensitive adhesive. When the M/Q value is smaller, inorganic components in the MQ silicon resin are more, the MQ silicon resin is in an ionic state, the dispersion effect is uneven, and the compatibility is poor; when the M/Q value is large, the organic component is true and can be uniformly dispersed in the alternation, but the reinforcing effect is deteriorated due to the decrease of the rigid inorganic core. The vinyl content is increased to generate a concentrated crosslinking effect, and when an external force acts, the force can be uniformly dispersed on a molecular chain through a crosslinking point, so that the colloid strength is enhanced. When the vinyl content is too high, the network density is too high, and uneven stress is caused by uneven distribution of crosslinking points, so that the strength is reduced.
The presence of a large amount of vinyl groups in the invention can ensure that the crosslinking degree of the main glue is compact enough, and the compound crosslinking agent formed by combining the crosslinking agent A and the crosslinking agent B further improves the reticular crosslinking density of the pressure-sensitive adhesive, and the self network structure characteristics of the compound crosslinking agent greatly improve the three-dimensional reticular compactness of the colloid.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
100 parts of macromolecular siloxane, adding 233.3 parts of toluene, dispersing for 4 hours by using a shearing type dispersing machine, dissolving into a raw rubber solution of 30%, sequentially adding 200 parts of toluene, 20 parts of tackifying resin and 50 parts of vinyl silicone oil, stirring for 1 hour after adding one material, adding the next material, stirring for 1 hour again, stirring uniformly, 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, stirring each material at intervals for 15 minutes, finally adding 5 parts of platinum catalyst, and continuously stirring for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Example 2
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% raw rubber solution is dissolved, 180 parts of toluene, 75 parts of tackifying resin and 30 parts of vinyl silicone oil are sequentially added, each of the materials is stirred for 1 hour, the next material is added, stirring is carried out for 1 hour, 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 are sequentially added after uniform stirring, each material is stirred for 15 minutes at intervals, and finally 3.0 parts of platinum catalyst is added, and stirring is continued for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Example 3
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% raw rubber solution is dissolved, 250 parts of toluene, 50 parts of tackifying resin and 50 parts of vinyl silicone oil are sequentially added, each of the materials is stirred for 1 hour, the next material is added, stirring is carried out for 1 hour, 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 are sequentially added after uniform stirring, each material is stirred for 15 minutes at intervals, and finally 3.5 parts of platinum catalyst is added, and stirring is continued for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Example 4
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% raw rubber solution is dissolved, 100 parts of toluene, 10 parts of tackifying resin and 28 parts of vinyl silicone oil are sequentially added, each of the materials is stirred for 1 hour, the next material is added, stirring is carried out for 1 hour, 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 are sequentially added after uniform stirring, each material is stirred for 15 minutes at intervals, and finally 2.8 parts of platinum catalyst are added, and stirring is continued for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Example 5:
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% raw rubber solution is dissolved, 100 parts of toluene, 10 parts of tackifying resin and 100 parts of vinyl silicone oil are sequentially added, each of the materials is stirred for 1 hour, the next material is added, stirring is carried out for 1 hour, 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 are sequentially added after uniform stirring, each material is stirred for 15 minutes at intervals, and finally 3.3 parts of platinum catalyst is added, and stirring is continued for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Example 6:
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% of raw rubber solution is dissolved, 100 parts of toluene and 10 parts of tackifying resin are sequentially added, each material is added and stirred for 1 hour, the next material is added and stirred for 1 hour, after uniform stirring, 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 are sequentially added, each material is stirred for 15 minutes at intervals, and finally 1.6 parts of platinum catalyst is added and stirred for 30 minutes continuously. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Comparative example 1
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% raw rubber solution is dissolved, 100 parts of toluene, 10 parts of tackifying resin and 100 parts of vinyl silicone oil with 2% volatile are sequentially added, each material is added and stirred for 1 hour, the next material is added and stirred for 1 hour, 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 are sequentially added after uniform stirring, each material is stirred for 15 minutes at intervals, and finally 3.3 parts of platinum catalyst is added and stirring is continued for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Comparative example 2
The crosslinking agent ASi-H bond content is 0.8mol/100g;
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% raw rubber solution is dissolved, 250 parts of toluene, 50 parts of tackifying resin and 50 parts of vinyl silicone oil are sequentially added, each of the materials is stirred for 1 hour, the next material is added, stirring is carried out for 1 hour, 1.5 parts of cross-linking agent (Si-H content is 0.8mol/100 g) is sequentially added after uniform stirring, 0.8 part of cross-linking agent B, 0.65 part of coupling agent and 0.9 part of inhibitor are sequentially added, each material is stirred for 15 minutes at intervals, and finally 3.5 parts of platinum catalyst is added, and stirring is continued for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a standard adhesive tape.
Comparative example 3
100 parts of macromolecular siloxane, 233.3 parts of toluene are added, a shearing type dispersing machine is used for dispersing for 4 hours, 30% of raw rubber solution is dissolved, 180 parts of toluene, 75 parts of tackifying resin and 30 parts of vinyl silicone oil are sequentially added, each material is added and stirred for 1 hour, the next material is added and stirred for 1 hour, 3.5 parts of cross-linking agent A, 0.66 part of coupling agent and 1.45 parts of inhibitor are sequentially added after uniform stirring, each material is stirred for 15 minutes at intervals, and finally 3.0 parts of platinum catalyst is added and stirring is continued for 30 minutes. Coating the prepared glue solution on a 50uPET substrate, curing the glue solution at the dry glue thickness of 10u and the temperature of 150 ℃ for 60s to obtain a low-molecular migration silica gel protective film, testing the gel content of the protective film, attaching the protective film to the surface of a specified diffusion sheet, placing 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 to a 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 for diffusion sheet of stuck object
1) And sticking the protective film on the surface of the appointed diffusion sheet, and pressing the diffusion sheet by using a 2kg roller for 3 times at the pressing speed of 600mm/min, and placing a constant temperature and humidity box for humid heat aging after the lamination, wherein the aging condition is 60903d.
2) Taking out the sample, standing for 2 hours in a standard environment, uncovering the protective film, and testing the water contact angle theta 1; the method comprises the steps of carrying out a first treatment on the surface of the
3) Testing the water contact angle theta 2 of the surface of the diffusion sheet original sheet;
4) Water contact angle change Δ= θ1- θ2
3. Tack decay Rate test
1) And sticking the protective film on the surface of the appointed diffusion sheet, and pressing the diffusion sheet by using a 2kg roller for 3 times at the pressing speed of 600mm/min, and placing a constant temperature and humidity box for humid heat aging after the lamination, wherein the aging condition is 60903d.
2) Taking out the sample, and standing for 2 hours in a standard environment;
3) The peel force of the Nidong 31B adhesive tape serving as a standard adhesive tape to the aged diffusion sheet is tested, and the specific method is as follows:
removing the protective film on the aged diffusion sheet, attaching a standard adhesive tape on the removed area of the diffusion sheet, pressing the diffusion sheet by a 2kg roller for 3 times, standing for 20min under a standard environment at a pressing speed of 600mm/min, and testing the relative stripping force F1;
4) Testing the stripping force F2 of the standard adhesive tape to the diffusion sheet original sheet;
5) The viscous damping rate calculation method comprises the following steps: attenuation ratio= (1-F1/F2) 100%.
Gel content test:
| 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 |
Diffusion sheet surface water contact angle change:
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％ |
Conclusion:
examples 1 to 6 show that macromolecular siloxanes are linear structures with the structural formula of-Si-O-Si-, and the side groups contain-Me and-Vi groups, so that the macromolecular siloxanes have the characteristics of low content of small molecules, and also have the characteristics of flexibility of long chains of the siloxanes, low surface energy and good wettability. The relative content of small molecules is reduced from the whole formula system; the existence of a large number of vinyl groups increases the crosslinking points of the silica gel system, so that the crosslinked reticular structure is more compact, and the migration mobility of internal small molecules is reduced; the compound cross-linking agent formed by the cross-linking agent A and the cross-linking agent B improves the reticular cross-linking density of the laminated adhesive in a further step, the reticular structure characteristic of the hydrogen-containing MQ silicon resin greatly improves the three-dimensional reticular density of the adhesive, 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 thickness and solid content in the process.
In comparative example 1, the conventional vinyl silicone oil with higher volatile component is used as the diluent, and the small analysis transfer amount of the attaching interface of the protective film is higher due to the higher content of small molecules.
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 lowered, so that the crosslinking degree was not dense enough, and the flow of small molecules in the adhesive layer was inhibited disadvantageously, thereby increasing the silicon transfer amount.
In comparative example 3, only one crosslinking agent was used, and the degree of crosslinking was not dense enough, which was not conducive to suppressing precipitation of small molecules, and the case where the degree of crosslinking was not dense enough, which resulted in insufficient control of small analysis, was also observed.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A silica gel protection film that high stability low micromolecule migrated, its characterized in that: the composition comprises the following components:
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;
the macromolecular siloxane is a high functional long chain siloxane with vinyl terminated side groups also containing vinyl groups and has a molecular weight of 300000 ～ 800000;
vinyl silicone oil refers to vinyl-terminated polymethylsiloxane with vinyl groups on side groups, and the molecular weight of the vinyl-terminated polymethylsiloxane is 10000-100000; vinyl content is 0.005-0.15 mol/100g; volatile component less than 0.5%;
the cross-linking agent A is hydrogen-containing silicone oil with high hydrogen content and low volatile component and Si-H-containing side group with molar mass of 400-1000 and structural general formula Me 3 SiO(SiMe 2 O)n(SiMeHO)mSiMe 3 Wherein m and n are positive integers; the content of the volatilizable micromolecules is 0.1 to 1.5 percent; the Si-H bond content of the hydrogen-containing silicone oil is 1.5-1.6 mol/100g;
the cross-linking agent B is hydrogen-containing MQ silicon resin with the molar mass of 1000-8000 and containing Si-H bonds; the Si-H bond content of the hydrogen-containing MQ silicon resin is 0.01-1 mol/100g;
the inhibitor is monomer containing triple bond or double bond, including one or more of 2-butyn-1-ol, 1-methyl-butyn-3-ol, 1-alkynyl cyclohexanol, maleic anhydride, tetramethyl tetravinyl cyclosiloxane, tetramethyl divinyl disiloxane, phenylacetylene, and 5-dimethyl-1-hexynyl-3-ol.
2. The silica gel protective film with high stability and low migration of small molecules according to claim 1, wherein the silica gel protective film is characterized in that: the macromolecular siloxane has a structural general formula of ViMe 2 SiO(SiMe 2 O)n(SiMeViO)mSiMe 2 Vi, wherein m and n are positive integers; the vinyl content is 0.0037-0.185 mol/100g.
3. The silica gel protective film with high stability and low migration of small molecules according to claim 1, wherein the silica gel protective film is characterized in that: the tackifying resin is a vinyl-containing MQ resin having a molar mass of 3000-8000 and an M/Q mer ratio of 0.7-0.85.
4. The silica gel protective film with high stability and low migration of small molecules according to claim 1, wherein the silica gel protective film is characterized in that: the M/Q chain link ratio of the hydrogen-containing MQ silicon resin is 0.75-0.85.
5. The silica gel protective film with high stability and low migration of small molecules according to claim 1, wherein the silica gel protective film is characterized in that: the coupling agent is a silane coupling agent with one end containing epoxy group or vinyl group and the other end containing alkoxy group; comprises one or more of gamma- (2, 3-glycidoxy) propyl trimethoxy silane, gamma- (2, 3-glycidoxy) propyl triethoxy silane, vinyl trimethoxy silane and vinyl triethoxy silane.
6. The silica gel protective film with high stability and low migration of small molecules according to claim 1, wherein the silica gel protective film is characterized in that: the platinum catalyst is a vinyl complex formed by coordination of Pt and unsaturated bonds; the solvent is one or more of toluene, xylene, ethyl acetate, butyl acetate and alkanes.
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