CN116285877A - Acid-base-resistant organic silicon pressure-sensitive adhesive, preparation method thereof and protective film material - Google Patents
Acid-base-resistant organic silicon pressure-sensitive adhesive, preparation method thereof and protective film material Download PDFInfo
- Publication number
- CN116285877A CN116285877A CN202310387729.8A CN202310387729A CN116285877A CN 116285877 A CN116285877 A CN 116285877A CN 202310387729 A CN202310387729 A CN 202310387729A CN 116285877 A CN116285877 A CN 116285877A
- Authority
- CN
- China
- Prior art keywords
- acid
- sensitive adhesive
- parts
- pressure sensitive
- alkali resistant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 42
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 39
- 239000010703 silicon Substances 0.000 title claims abstract description 39
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 25
- 230000001681 protective effect Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 30
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 30
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 29
- -1 polysiloxane Polymers 0.000 claims abstract description 28
- 239000003513 alkali Substances 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 22
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 22
- 239000002683 reaction inhibitor Substances 0.000 claims abstract description 20
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 239000011347 resin Substances 0.000 claims abstract description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 66
- 229910052697 platinum Inorganic materials 0.000 claims description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 15
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000006555 catalytic reaction Methods 0.000 claims description 14
- 238000007865 diluting Methods 0.000 claims description 12
- BPSIOYPQMFLKFR-VIFPVBQESA-N trimethoxy-[3-[[(2r)-oxiran-2-yl]methoxy]propyl]silane Chemical group CO[Si](OC)(OC)CCCOC[C@H]1CO1 BPSIOYPQMFLKFR-VIFPVBQESA-N 0.000 claims description 12
- 239000012790 adhesive layer Substances 0.000 claims description 8
- 239000010410 layer Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 18
- 230000001070 adhesive effect Effects 0.000 abstract description 18
- 239000003792 electrolyte Substances 0.000 abstract description 11
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000003085 diluting agent Substances 0.000 abstract description 2
- 239000002585 base Substances 0.000 description 15
- 239000003292 glue Substances 0.000 description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 9
- 229920000139 polyethylene terephthalate Polymers 0.000 description 9
- 229920002050 silicone resin Polymers 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 229920002799 BoPET Polymers 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- UEXCJVNBTNXOEH-UHFFFAOYSA-N Ethynylbenzene Chemical group C#CC1=CC=CC=C1 UEXCJVNBTNXOEH-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 1
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 1
- 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
- 102100027446 Acetylserotonin O-methyltransferase Human genes 0.000 description 1
- 101000936718 Homo sapiens Acetylserotonin O-methyltransferase Proteins 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000004804 winding Methods 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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides an acid and alkali resistant organic silicon pressure sensitive adhesive, which comprises the following components: 50-150 parts of polysiloxane containing vinyl; 20-80 parts of methyl MQ resin; 0.8-1.5 parts of cross-linking agent; 0.5-1.0 part of Pt catalyst; 0.05-0.2 part of reaction inhibitor; 0.5-1.5 parts of silane coupling agent; 150-250 parts of diluent solvent. The invention also relates to a preparation method and a protective film material thereof. According to the invention, the synthesis operation flow of the formed adhesive is simple according to the optimized raw materials and the preparation proportion, and the adhesive is convenient to produce and use; and has good storage property at normal temperature. The electrolyte-resistant organic silicon protective film prepared by the adhesive has the characteristics of high curing speed, high strength, high temperature and humidity resistance, stable stripping force and acid and alkali electrolyte resistance when the 180-degree stripping force is tested according to GB/2792-1998.
Description
Technical Field
The invention relates to the field of adhesives, in particular to an acid and alkali resistant organic silicon pressure-sensitive adhesive, a preparation method thereof and a protective film material.
Background
The organic silicon pressure-sensitive adhesive is a novel adhesive, has wide development prospect, and is a high-quality and high-grade variety in the pressure-sensitive adhesive. The adhesive has the characteristics of good adhesive strength and initial adhesion of pressure-sensitive adhesive, has good adhesion to high-energy and low-energy surface materials, can keep the adhesive strength and flexibility between 50 ℃ below zero and 200 ℃ and can be used for a long time. The excellent chemical inertness and electrical property of the organic silicon pressure-sensitive adhesive can lead the organic silicon pressure-sensitive adhesive to have irreplaceable advantages in the electronic industry and the medical industry. The method is widely applied to the aspects of electronics, medicine, optics, electroplating protection, new energy and material processing and the like.
With the development requirements of new technology and the continuous extension of the application of the organic silicon pressure-sensitive adhesive, the viscosity range of the protective film is required to be expanded to two directions of high viscosity and low viscosity, and meanwhile, the application environment of the protective film is also required to a certain extent. In particular, in the metal etching industry, it is required that the silica gel protective film be more biased towards tolerance to different acid-base electrolytes.
Thus, the existing pressure-sensitive adhesive components are required to be improved, and the acid and alkali resistant organic silicon pressure-sensitive adhesive is designed.
Disclosure of Invention
In order to overcome the defects in the prior art, the first aim of the invention is to provide an acid and alkali resistant organic silicon pressure-sensitive adhesive, which comprises the following raw materials in parts by weight:
preferably, the polysiloxane has the structural general formula:
R(CH 3 ) 2 SiO[Si(CH 3 ) 2 O] n [Si(CH 3 )(CH＝CH 2 )O] m Si(CH 3 ) 2 r, wherein R is vinyl; the polysiloxane has a viscosity of 100000mpa.s at 25 ℃; the vinyl content is 0.04% -0.16%.
Preferably, the ratio of M units to Q units in the methyl MQ resin is: m is Q > 1.
Preferably, the cross-linking agent is silicone oil containing a silicon hydrogen (SiH) group, and the molecular structure is as follows: me (Me) 3 SiO(Me 2 SiO) m (Me (2-a) H a SiO) n SiMe 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein m/n is a positive integer, a is an integer of 1 to 2, and the mass percentage of hydrogen (H) is 1.0 to 1.6 percent; more preferably 1.2 to 1.6%, still more preferably 1.4 to 1.6%; the viscosity at 25 ℃ is 30-100 mpa.s;
preferably, the Pt catalyst has a platinum content of 3000ppm to 5000ppm.
Preferably, the Pt catalyst is a catalyst prepared by carrying out coordination exchange on a Karster catalyst by using siloxane oligomer containing long-chain alkyl and vinyl, and preparing a platinum-a, w-di (n-octyl) polymethyl vinyl siloxane complex.
Preferably, the reaction inhibitor is an alkynol catalytic reaction inhibitor.
Preferably, the silane coupling agent is r-glycidoxypropyl trimethoxysilane and/or r-methacryloxypropyl trimethoxysilane.
The second object of the invention is to provide a preparation method of an acid and alkali resistant organic silicon pressure-sensitive adhesive, which comprises the following steps:
s1, adding the vinyl polysiloxane, the methyl MQ silicon resin and a diluting solvent into a reaction kettle, and stirring for 0.5h at normal temperature to obtain a dispersion liquid A;
s2, adding the cross-linking agent, the reaction inhibitor, the silane coupling agent and the Pt catalyst into the dispersion liquid A in sequence while stirring, and fully and uniformly mixing to obtain the finished organosilicon pressure-sensitive adhesive.
A third object of the present invention is to provide a protective film material comprising an adhesive layer composed of the acid and alkali resistant silicone pressure sensitive adhesive of claim 1 and a base material layer.
Compared with the prior art, the invention has the beneficial effects that: the invention provides an acid and alkali resistant organic silicon pressure sensitive adhesive, which comprises the following components: 50-150 parts of polysiloxane containing vinyl; 20-80 parts of methyl MQ resin; 0.8-1.5 parts of cross-linking agent; 0.5-1.0 part of Pt catalyst; 0.05-0.2 part of reaction inhibitor; 0.5-1.5 parts of silane coupling agent; 150-250 parts of diluent solvent. The invention also relates to a preparation method and a protective film material thereof. According to the invention, the synthesis operation flow of the formed adhesive is simple according to the optimized raw materials and the preparation proportion, and the adhesive is convenient to produce and use; and has good storage property at normal temperature. The electrolyte-resistant organic silicon protective film prepared by the adhesive has the characteristics of high curing speed, high strength, high temperature and humidity resistance, stable stripping force and acid and alkali electrolyte resistance when the 180-degree stripping force is tested according to GB/2792-1998.
The foregoing description is only an overview of the present invention, and is intended to provide a better understanding of the present invention, as it is hereinafter described in more detail with reference to the preferred embodiments of the present invention. Specific embodiments of the present invention are given in detail by the following examples.
Detailed Description
The present invention will be further described with reference to the following specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
The invention relates to an acid and alkali resistant organic silicon pressure sensitive adhesive, which comprises the following raw materials in parts by weight:
the solid content of the adhesive obtained by the components is 30% -50%; and the full curing can be realized within 1-2min at the curing temperature of 160 ℃, so that the aim of directly winding and rapidly curing after the substrate is coated and rubberized can be fulfilled. According to the invention, the synthesis operation flow of the formed adhesive is simple according to the optimized raw materials and the preparation proportion, and the adhesive is convenient to produce and use; and has good storage property at normal temperature. The electrolyte-resistant organic silicon protective film (the adhesive is the main component of an organic silicon protective film adhesive layer) can be manufactured through the adhesive, so that the purposes of meeting the process protection requirement and ensuring the performance stability of a product are achieved. In addition, the 180-degree stripping force of the electrolyte-resistant organic silicon protective film prepared by the invention is tested according to GB/2792-1998, and the electrolyte-resistant organic silicon protective film has the characteristics of high curing speed, high strength, high temperature and humidity resistance, stable stripping force and acid and alkali electrolyte resistance.
In some embodiments, the cross-linking agent is a hydrogen-containing silicone oil.
In some embodiments, the polysiloxane has the general structural formula:
R(CH 3 ) 2 SiO[Si(CH 3 ) 2 O] n [Si(CH 3 )(CH＝CH 2 )O] m Si(CH 3 ) 2 r, wherein m/n is a positive integer, R is vinyl; the polysiloxane has a viscosity of 100000mpa.s at 25 ℃; vinyl content is 0.04% -0.16%; more preferably 0.09% -0.11%.
In some embodiments, the ratio of M units to Q units in the methyl MQ resin is: m is Q > 1. The structure can ensure that the network structure of intermolecular combination is more compact, thereby improving the acid and alkali resistance.
The cross-linking agent is silicone oil containing a silicon hydrogen (SiH) group, and the molecular structure is as follows: me (Me) 3 SiO(Me 2 SiO) m (Me (2-a) H a SiO) n SiMe 3 The method comprises the steps of carrying out a first treatment on the surface of the Wherein m/n is a positive integer, a is an integer of 1 to 2, and the mass percentage of hydrogen (H) is 1.0 to 1.6 percent; more preferably 1.2 to 1.6%, still more preferably 1.4 to 1.6%; the viscosity at 25 ℃ is 30-100 mpa.s;
in some embodiments, the Pt catalyst has a platinum content of 3000ppm to 5000ppm, more preferably 3500ppm to 4000ppm; in the proportion range, the platinum catalysis can achieve the complete catalysis effect, and the product is completely solidified. The platinum catalyst is a platinum catalyst coordinated with methyl vinyl siloxane, and can effectively catalyze addition reaction at the temperature of more than 80 ℃.
In some embodiments, the solvent is a mixture of one or more of toluene, xylene, ethyl acetate. Preferably, the solvent is toluene, xylene, ethyl acetate; more preferably toluene, ethyl acetate. Thus, the uniformity of mixing and dispersing of the glue of the product and the stability of the coating appearance of the product can be ensured.
In some embodiments, the reaction inhibitor is an alkynol catalytic reaction inhibitor. Optionally, the inhibitor is one or any combination of phenylacetylene, 1-ethynyl-1-cyclohexanol, tetramethyl tetra-vinyl cyclotetrasiloxane, 2-methyl-3-butynyl-2-ol, 3-methyl-1-ethynyl-3-ol, 3, 5-dimethyl-1-hexynyl-3-ol and 3-methyl-1-dodecynyl-3-ol.
In some embodiments, the silane coupling agent is r-glycidoxypropyl trimethoxysilane and/or r-methacryloxypropyl trimethoxysilane. Preferably, the silane coupling agent is r-glycidoxypropyl trimethoxysilane.
The invention also relates to a preparation method of the acid and alkali resistant organic silicon pressure-sensitive adhesive, which comprises the following steps:
s1, adding the vinyl polysiloxane, the methyl MQ silicon resin and a diluting solvent into a reaction kettle, and stirring for 0.5h at normal temperature to obtain a dispersion liquid A;
s2, adding the cross-linking agent, the reaction inhibitor, the silane coupling agent and the Pt catalyst into the dispersion liquid A in sequence while stirring, and fully and uniformly mixing to obtain the finished organosilicon pressure-sensitive adhesive. The preparation method can achieve the purposes of simplifying the production process, ensuring the performance stability of the product and enabling the protective film to resist the etching of electrolyte.
The invention also relates to a protective film material, which comprises an adhesive layer and a substrate layer, wherein the substrate layer is a polyester PET film, and the thickness of the substrate can be adjusted in a large range; in some embodiments, it is a 50um thick polyester PET film; the adhesive layer consists of the acid and alkali resistant organic silicon pressure sensitive adhesive; the adhesive layer is coated on one surface or two surfaces of the substrate layer; the protective film material is obtained by coating the adhesive layer on the surface of the substrate layer and then curing at 160 ℃ for 1-2 min. Specifically, a 50um polyester PET film is used as a base material, an organic silicon pressure-sensitive adhesive is coated on the surface of the base material through a tape coater, after the coating is completed, the base material is cured for 1-2min at 160 ℃ through an oven, and then a separation film is attached to obtain the double-layer organic silicon protection film. The protective film material has good electrolyte resistance.
Example 1
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.2 parts of cross-linking agent, 1 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.6%.
Wherein, the silane coupling agent is: r-glycidoxypropyl trimethoxysilane.
Example two
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 0.8 part of cross-linking agent, 1 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.6%.
Wherein, the silane coupling agent is: r-glycidoxypropyl trimethoxysilane.
Example III
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.5 parts of cross-linking agent, 1 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.6%.
Wherein, the silane coupling agent is: r-glycidoxypropyl trimethoxysilane.
Example IV
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.2 parts of cross-linking agent, 0.5 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.6%.
Wherein, the silane coupling agent is: r-glycidoxypropyl trimethoxysilane.
Example five
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.2 parts of cross-linking agent, 1.5 parts of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.6%.
Wherein, the silane coupling agent is: r-glycidoxypropyl trimethoxysilane.
Comparative example one
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.2 parts of cross-linking agent, 1 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.6%.
Wherein, the silane coupling agent is: r-methacryloxypropyl trimethoxysilane.
Comparative example two
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.2 parts of cross-linking agent, 1 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.6%.
Wherein, the silane coupling agent is: the r-methacryloxypropyl trimethoxysilane and the r-glycidoxypropyl trimethoxysilane are mixed according to a ratio of 1:1.
Comparative example three
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.2 parts of cross-linking agent, 1 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.0%.
Wherein, the silane coupling agent is: r-glycidoxypropyl trimethoxysilane.
Comparative example four
The acid-base resistant organic silicon pressure-sensitive adhesive provided by the embodiment comprises the following raw materials in parts by weight, wherein the raw materials comprise 100 parts of polysiloxane containing 0.1% of vinyl, 50 parts of methyl MQ silicone resin and 200 parts of diluting solvent, and the materials are stirred and mixed to obtain dispersion liquid; after complete dissolution, adding 0.1 part of alkynol catalytic reaction inhibitor, 1.2 parts of cross-linking agent, 1 part of silane coupling agent and 0.8 part of platinum catalyst with 4000ppm of platinum content in the Pt catalyst, and uniformly stirring; glue was applied to a 50 micron thick PET substrate, 10um thick, and baked at 160℃for 2min.
Wherein, the cross-linking agent contains hydrogen (H) in mass percent: 1.2%.
Wherein, the silane coupling agent is: r-glycidoxypropyl trimethoxysilane.
The products prepared in examples one to five, comparative examples one to fourth were tested for their respective properties. The specific test results are shown in table 1 below.
Peel force test: ASMT D3330— tensile machine;
alkali resistance test: pH 12 alkali liquor 70 ℃/2H
Acid resistance test: PH value of 3 acid liquor 70 ℃/2H
Table 1 test results table of different examples
As can be seen from the example one/example two/example three comparison: the difference in the amount of the crosslinking agent added leads to a difference in the crosslinking density, thereby affecting the acid resistance. The amount of the crosslinking agent added is already a lower limit of 0.8%.
As can be seen from the example one/example four/example five comparison: the different addition amounts of the silane coupling agents can influence the adhesiveness of the adhesive surface and the film surface, thereby influencing the acid resistance. The addition amount of the silane coupling agent of 0.5% has been the lower limit.
As can be seen from the example one/comparative example two). The different types of the silane coupling agents can influence the adhesiveness of the adhesive surface and the film surface, thereby influencing the acid resistance. The r-glycidol ether oxypropyl trimethoxy silane has better use effect.
As can be seen from the example one/comparative example three/comparative example four comparison: the difference in mass percentages of the hydrogen (H) contained in the crosslinking agent affects the structure of intermolecular crosslinking reaction, thereby affecting acid resistance. The mass percentage of hydrogen (H) is already 1% as the lower limit.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use, and further modifications may be readily made by those skilled in the art without departing from the general concepts defined by the claims and the equivalents thereof, and therefore the invention is not limited to the specific details and examples shown herein.
Claims (10)
1. The acid and alkali resistant organic silicon pressure sensitive adhesive is characterized by comprising the following raw materials in parts by weight:
2. the acid and alkali resistant silicone pressure sensitive adhesive of claim 1, wherein the polysiloxane has the general structural formula:
R(CH 3 ) 2 SiO[Si(CH 3 ) 2 O] n [Si(CH 3 )(CH＝CH 2 )O] m Si(CH 3 ) 2 r, wherein R is vinyl; the polysiloxane has a viscosity of 100000mpa.s at 25 ℃; the vinyl content is 0.04% -0.16%.
3. The acid and alkali resistant silicone pressure sensitive adhesive of claim 1 wherein the ratio of M units to Q units in the methyl MQ resin is: m is Q > 1.
4. The acid and alkali resistant silicone pressure sensitive adhesive of claim 1, wherein the cross-linking agent is silicone oil containing a silicon hydrogen (SiH) group, and the molecular structure is:
Me 3 SiO(Me 2 SiO) m (Me (2-a) H a SiO) n SiMe 3 the method comprises the steps of carrying out a first treatment on the surface of the Wherein m/n is a positive integer, a is an integer of 1 to 2, and the mass percentage of hydrogen (H) is 1.0 to 1.6 percent.
5. The acid and alkali resistant silicone pressure sensitive adhesive of claim 1, wherein the Pt catalyst has a platinum content of 3000ppm to 5000ppm.
6. The acid and alkali resistant silicone pressure sensitive adhesive of claim 5, wherein the Pt catalyst is a catalyst that coordinates exchange of a carlst catalyst with a siloxane oligomer containing long chain alkyl groups and vinyl groups to prepare a platinum-a, w-di (n-octyl) polymethylvinylsiloxane complex.
7. The acid and alkali resistant silicone pressure sensitive adhesive of claim 1 wherein the reaction inhibitor is an alkynol catalytic reaction inhibitor.
8. The acid and alkali resistant silicone pressure sensitive adhesive of claim 1, wherein the silane coupling agent is r-glycidoxypropyl trimethoxysilane and/or r-methacryloxypropyl trimethoxysilane.
9. The method for preparing the acid and alkali resistant organosilicon pressure sensitive adhesive according to claim 1, comprising the following steps:
s1, adding the vinyl polysiloxane, the methyl MQ silicon resin and a diluting solvent into a reaction kettle, and stirring for 0.5h at normal temperature to obtain a dispersion liquid A;
s2, adding the cross-linking agent, the reaction inhibitor, the silane coupling agent and the Pt catalyst into the dispersion liquid A in sequence while stirring, and fully and uniformly mixing to obtain the finished organosilicon pressure-sensitive adhesive.
10. A protective film material comprising an adhesive layer and a substrate layer, wherein the adhesive layer consists of the acid and alkali resistant silicone pressure sensitive adhesive of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310387729.8A CN116285877A (en) | 2023-04-12 | 2023-04-12 | Acid-base-resistant organic silicon pressure-sensitive adhesive, preparation method thereof and protective film material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310387729.8A CN116285877A (en) | 2023-04-12 | 2023-04-12 | Acid-base-resistant organic silicon pressure-sensitive adhesive, preparation method thereof and protective film material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116285877A true CN116285877A (en) | 2023-06-23 |
Family
ID=86830689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310387729.8A Pending CN116285877A (en) | 2023-04-12 | 2023-04-12 | Acid-base-resistant organic silicon pressure-sensitive adhesive, preparation method thereof and protective film material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116285877A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113388362A (en) * | 2021-07-22 | 2021-09-14 | 江苏斯迪克新材料科技股份有限公司 | Low-climbing organic silicon pressure-sensitive adhesive and preparation method and application thereof |
| CN114316896A (en) * | 2022-01-17 | 2022-04-12 | 江苏斯迪克新材料科技股份有限公司 | Silicon gel, preparation method and protective film applying silicon gel |
| CN115612444A (en) * | 2022-09-01 | 2023-01-17 | 江苏斯迪克新材料科技股份有限公司 | Adhesive for silica gel protective film attached to cambered surface glass, preparation method of adhesive and adhesive tape |
-
2023
- 2023-04-12 CN CN202310387729.8A patent/CN116285877A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113388362A (en) * | 2021-07-22 | 2021-09-14 | 江苏斯迪克新材料科技股份有限公司 | Low-climbing organic silicon pressure-sensitive adhesive and preparation method and application thereof |
| CN114316896A (en) * | 2022-01-17 | 2022-04-12 | 江苏斯迪克新材料科技股份有限公司 | Silicon gel, preparation method and protective film applying silicon gel |
| CN115612444A (en) * | 2022-09-01 | 2023-01-17 | 江苏斯迪克新材料科技股份有限公司 | Adhesive for silica gel protective film attached to cambered surface glass, preparation method of adhesive and adhesive tape |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106753195B (en) | Organic silicon pressure-sensitive adhesive and pressure-sensitive adhesive tape or film | |
| EP3275961B1 (en) | Laminate comprising release liner based on release agent composition for silicone adhesive | |
| CN113388362A (en) | Low-climbing organic silicon pressure-sensitive adhesive and preparation method and application thereof | |
| CN111548518A (en) | Ultra-light/ultra-heavy non-silicon release film and preparation method thereof | |
| CN105001422B (en) | A kind of addition-type silicon rubber tackifier and preparation method thereof and addition-type silicon rubber | |
| CN107602863B (en) | Fluoroalkyl hydrogen-containing silicone oil and preparation method thereof | |
| CN114058290B (en) | Solvent-free organosilicon release agent with ultralow release force and preparation method thereof | |
| CN110564347A (en) | One-component epoxy structure adhesive for waterproof sealing and preparation method thereof | |
| CN111423844A (en) | Transferable pressure-sensitive adhesive, pressure-sensitive adhesive tape and application method of pressure-sensitive adhesive tape | |
| CN114574097B (en) | Bi-component normal-temperature curing epoxy modified MQ silicon resin coating | |
| KR20170096881A (en) | Anti-static silicone tight-release coating film | |
| KR102438686B1 (en) | Solvent-type silicone release coating composition for coating of ultralight release film | |
| CN102775792B (en) | Modified hydrogen-containing silicone oil, preparation method and application thereof, and silicon rubber containing modified hydrogen-containing silicone oil | |
| CN106519876A (en) | Hyperbranched polymer modified silicone acrylate containing antiadhesion agent and preparation method thereof | |
| CN111499870A (en) | Boiling-resistant organic silicon pressure-sensitive adhesive tackifier and preparation method thereof | |
| CN109251659A (en) | Compound release liquid and preparation method thereof and function film | |
| CN116285877A (en) | Acid-base-resistant organic silicon pressure-sensitive adhesive, preparation method thereof and protective film material | |
| JPH0718185A (en) | Silicone composition for release agent | |
| CN115612444A (en) | Adhesive for silica gel protective film attached to cambered surface glass, preparation method of adhesive and adhesive tape | |
| CN112250704A (en) | Silicon-titanium copolymerization primer and preparation method thereof | |
| CN109536085B (en) | Preparation method of organic silicon modified polyacrylate pressure-sensitive adhesive and pressure-sensitive adhesive prepared by preparation method | |
| CN113845860A (en) | Silica gel protective film and preparation method thereof | |
| CN113881365A (en) | Acrylic pressure-sensitive adhesive with thin coating and high viscosity solvent and synthesis method thereof | |
| CN113502130A (en) | Double-sided adhesive tape and preparation method thereof | |
| CN113024810A (en) | Single-component self-crosslinkable fluorosilicone release agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |