CN116285867A - Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof - Google Patents
Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof Download PDFInfo
- Publication number
- CN116285867A CN116285867A CN202310298365.6A CN202310298365A CN116285867A CN 116285867 A CN116285867 A CN 116285867A CN 202310298365 A CN202310298365 A CN 202310298365A CN 116285867 A CN116285867 A CN 116285867A
- Authority
- CN
- China
- Prior art keywords
- sensitive adhesive
- silica gel
- graphene oxide
- resin
- gel pressure
- 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.)
- Withdrawn
Links
- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 55
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 35
- 239000000741 silica gel Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910017059 organic montmorillonite Inorganic materials 0.000 claims abstract description 48
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 46
- 229920005989 resin Polymers 0.000 claims abstract description 44
- 239000011347 resin Substances 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 239000002105 nanoparticle Substances 0.000 claims abstract description 42
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 38
- 239000004945 silicone rubber Substances 0.000 claims abstract description 38
- 229910052709 silver Inorganic materials 0.000 claims abstract description 37
- 239000004332 silver Substances 0.000 claims abstract description 37
- 239000002114 nanocomposite Substances 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 28
- 125000005375 organosiloxane group Chemical group 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000004971 Cross linker Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 239000003431 cross linking reagent Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 12
- 239000012265 solid product Substances 0.000 claims description 12
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 8
- -1 octadecyl quaternary ammonium salt Chemical class 0.000 claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical group [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- TVJPBVNWVPUZBM-UHFFFAOYSA-N [diacetyloxy(methyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(OC(C)=O)OC(C)=O TVJPBVNWVPUZBM-UHFFFAOYSA-N 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052710 silicon Inorganic materials 0.000 abstract description 9
- 239000010703 silicon Substances 0.000 abstract description 9
- 150000002500 ions Chemical class 0.000 abstract description 6
- 230000003014 reinforcing effect Effects 0.000 abstract description 6
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002411 thermogravimetry 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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- 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
-
- 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)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-temperature-resistant conductive silica gel pressure-sensitive adhesive and a preparation method thereof, wherein the silica gel pressure-sensitive adhesive comprises the following raw material components: silicone rubber, MQ resin, modified nanoparticle mixture, organosiloxane crosslinker, and catalyst; the modified nanoparticle mixture is obtained by mixing a graphene oxide-silver nanocomposite and organic montmorillonite OMMT according to a mass ratio of 1:2-4:1. The invention utilizes the advantages of graphene-silver nano ions in the aspect of conductivity and the excellent thermal performance and flame retardance reinforcing effect of the organized montmorillonite OMMT, and the graphene-silver nano ions are compounded and applied to the modification of the organic silicon pressure-sensitive adhesive, and the combination can achieve the synergistic reinforcing effect, thereby effectively improving the conductivity and the heat resistance of the silica gel pressure-sensitive adhesive, and the volume resistivity of the obtained silica gel pressure-sensitive adhesive can reach 1 multiplied by 10 ‑1 The heat-resistant temperature can reach 350 ℃.
Description
Technical Field
The invention relates to the field of pressure-sensitive adhesive materials, in particular to a silica gel pressure-sensitive adhesive with high-temperature resistance and conductivity and a preparation method thereof.
Background
The organic silicon pressure-sensitive adhesive has special properties: low chemical activity, low smell, no irritation, good adhesion performance to both low surface energy and high surface energy; the organic silicon pressure-sensitive adhesive also has the advantages of solvent resistance, high and low temperature resistance, aging resistance and the like. Although silicone pressure-sensitive adhesives have many advantages, the electronic field has higher and higher requirements for performance due to technological advancement: higher heat resistance and better conductivity, and new materials are required to be developed or the properties of the original materials are required to be improved.
The conventional silica gel protective film has good temperature resistance at 250-300 ℃ and no residual glue, but has special application scenes that the actual working temperature can reach 350 ℃ or above, and meanwhile, better conductivity is required, so that the conventional silica gel pressure-sensitive adhesive is difficult to meet the use under such severe conditions.
Therefore, there is a need in the art for improvements that provide a more reliable solution.
Disclosure of Invention
The invention aims to solve the technical problem of providing a silica gel pressure-sensitive adhesive with high-temperature resistance and conductivity and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme: the silica gel pressure-sensitive adhesive with high-temperature resistance conductivity comprises the following raw material components: silicone rubber, MQ resin, modified nanoparticle mixture, organosiloxane crosslinker, and catalyst;
the modified nanoparticle mixture is obtained by mixing graphene oxide-silver nanocomposite and organic montmorillonite OMMT according to a mass ratio of 1:2-4:1.
Preferably, the graphene oxide-silver nanocomposite is prepared by the following method:
adding 0.01-1g of graphite oxide into 50-5000mL of deionized water, and uniformly dispersing after ultrasonic treatment for 1-4 hours to obtain graphene oxide dispersion liquid;
and adding 0.01-0.1 g of silver nitrate crystal into the graphene oxide dispersion liquid, uniformly stirring, filtering, washing the obtained solid product with deionized water, and drying to obtain the graphene oxide-silver nanocomposite.
Preferably, the graphene oxide-silver nanocomposite is prepared by the following method:
adding 0.1g of graphite oxide into 500mL of deionized water, and uniformly dispersing after ultrasonic treatment for 2 hours to obtain graphene oxide dispersion liquid;
and adding 0.05g of silver nitrate crystal into the graphene oxide dispersion liquid, uniformly stirring, filtering, washing the obtained solid product with deionized water for 3 times, and drying to obtain the graphene oxide-silver nanocomposite.
Preferably, the organized montmorillonite OMMT is prepared by the following method:
adding 0.1-10 g of montmorillonite into 50-500mL of distilled water, heating and stirring until the montmorillonite is dissolved, then adding 0.01-0.1 g of octadecyl quaternary ammonium salt, stirring for 1-6h, carrying out suction filtration, washing a solid product with distilled water, drying and grinding to obtain the organic montmorillonite OMMT.
Preferably, the organized montmorillonite OMMT is prepared by the following method:
adding 0.2g of montmorillonite into 200mL of distilled water, stirring at 80 ℃ for 20min, dissolving montmorillonite, adding 0.05g of octadecyl quaternary ammonium salt, stirring for 3h, suction filtering, washing solid product with distilled water, drying, and grinding to below 200 meshes to obtain the organic montmorillonite OMMT.
Preferably, the octadecyl quaternary ammonium salt is: octadecyl trimethyl ammonium chloride.
Preferably, the weight ratio of the MQ resin to the silicone rubber is 10:90-40:60;
the addition amount of the modified nanoparticle mixture is 1-5% of the total weight of the MQ resin and the silicone rubber;
the addition amount of the organosiloxane cross-linking agent is 1-5% of the total weight of the MQ resin and the silicone rubber;
the addition amount of the catalyst is 0.1-1% of the total weight of the MQ resin and the silicone rubber.
Preferably, the MQ resin is formed by hydrolytic condensation of hexamethyldisiloxane serving as an M group and tetraethoxysilane or water glass serving as a Q group, wherein the molar ratio of the M group to the Q group is 0.8:1-1.0:1, and the number average molecular weight Mn of the MQ resin is 4000-8000.
Preferably, the organic siloxane crosslinking agent is one or more of vinyl triethoxy silane, aminopropyl triethoxy silane, methyl tributyl ketoxime silane and methyl triacetoxy silane;
the catalyst is a platinum system catalyst.
Preferably, the preparation method of the silica gel pressure-sensitive adhesive with high-temperature resistance and conductivity comprises the following steps:
s1, preparing a modified nanoparticle mixture solution: mixing the graphene oxide-silver nanocomposite with the organized montmorillonite OMMT to obtain a modified nanoparticle mixture, adding the modified nanoparticle mixture into toluene, and uniformly stirring to obtain a modified nanoparticle mixture solution;
s2, mixing MQ resin and silicone rubber, adding the modified nanoparticle mixture solution, stirring for 0.5-3h, adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
The beneficial effects of the invention are as follows:
the invention adopts the graphene-silver nanocomposite and the organic montmorillonite OMMT to compound to modify the organic silicon pressure-sensitive adhesive, can effectively improve the conductivity and the high temperature resistance of the organic silicon pressure-sensitive adhesive, and has the volume resistivity of 1 multiplied by 10 -1 The heat-resistant temperature can reach 350 ℃;
according to the graphene-silver nanocomposite material prepared by the method, the dispersibility of Ag is improved by modifying the nano silver with graphene, so that the agglomeration phenomenon of nano Ag can be effectively prevented, meanwhile, ag is inserted between graphene sheets, the intermolecular acting force between the graphene sheets can be reduced, and the aggregation of the graphene sheets can be effectively avoided; according to the invention, montmorillonite is subjected to organic treatment and then combined with the polymer, so that the heat resistance and the dispersibility can be improved, the apparent decomposition temperature of the organic silicon pressure-sensitive adhesive is increased, and the mechanical property and the thermal property of the organic silicon pressure-sensitive adhesive can be improved;
the invention utilizes the advantages of graphene-silver nano ions in the aspect of conductivity and the excellent thermal performance and flame retardance reinforcing effect of the organized montmorillonite OMMT, and the graphene-silver nano ions are compounded and applied to the modification of the organic silicon pressure-sensitive adhesive, and the combination can achieve the synergistic reinforcing effect, so that the conductivity and the heat resistance of the silica gel pressure-sensitive adhesive can be effectively improved.
Detailed Description
The present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
The test methods used in the following examples are conventional methods unless otherwise specified. The material reagents and the like used in the following examples are commercially available unless otherwise specified. The following examples were conducted under conventional conditions or conditions recommended by the manufacturer, without specifying the specific conditions. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The invention provides a high-temperature-resistant conductive silica gel pressure-sensitive adhesive, which comprises the following raw material components: silicone rubber, MQ resin, modified nanoparticle mixture, organosiloxane crosslinker, and catalyst.
In the invention, the modified nanoparticle mixture is obtained by mixing graphene oxide-silver nanocomposite and organic montmorillonite OMMT according to the mass ratio of 1:2-4:1.
In the invention, the preparation method of the silica gel pressure-sensitive adhesive comprises the following steps:
s1, preparing a modified nanoparticle mixture solution: mixing the graphene oxide-silver nanocomposite with the organized montmorillonite OMMT to obtain a modified nanoparticle mixture, adding the modified nanoparticle mixture into deionized water, and uniformly stirring to obtain a modified nanoparticle mixture solution;
s2, mixing MQ resin and silicone rubber, adding the modified nanoparticle mixture solution, stirring for 0.5-3h, adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
In the invention, the graphene oxide-silver nanocomposite is prepared by the following method:
adding 0.01-1g of graphite oxide into 50-5000mL of deionized water, and uniformly dispersing after ultrasonic treatment for 1-4 hours to obtain graphene oxide dispersion liquid; adding 0.01-0.1 g of silver nitrate crystal into graphene oxide dispersion liquid, stirring uniformly, filtering, washing the obtained solid product with deionized water, and adding excessive Ag + And (5) washing and drying to obtain the graphene oxide-silver nanocomposite.
The graphene oxide is a two-dimensional carbon nanomaterial consisting of a single layer of densely arranged carbon atoms, and the two-dimensional planar structure provides multiple platforms for hybridization of different materials. Silver nanoparticles have unique properties, and have more active sites on their surface, which can promote electron transfer. The preparation process is simple and the cost efficiency is high. Silver nano particles have good electrocatalytic activity, but are poorly dispersed and easily aggregated in solution. In order to avoid the occurrence of the situation, when the graphene is used as a carrier to introduce the silver nano particles, the accumulation of the graphene is reduced, so that a higher surface area is provided, and the graphene is used as a growth carrier to fully exert the catalytic performance of the silver nano particles. According to the preparation method, the graphene oxide and the nano silver are compounded to prepare the graphene oxide-silver nanocomposite, and the catalytic activity and stability of the nano silver are enhanced through the direct strong synergistic effect of the graphene oxide and the nano silver.
In the invention, the organic montmorillonite OMMT is prepared by the following method:
adding 0.01-1g of montmorillonite into 50-500mL of distilled water, heating and stirring until the montmorillonite is dissolved, then adding 0.01-0.1 g of octadecyl quaternary ammonium salt, stirring for 1-6h, carrying out suction filtration, washing a solid product with distilled water, drying, and grinding to obtain the organic montmorillonite OMMT. Wherein the octadecyl quaternary ammonium salt is octadecyl trimethyl ammonium chloride.
Montmorillonite (MMT) is a layered silicate, belongs to monoclinic crystals, and has a basic structural unit of a layered structure formed by sandwiching an aluminum oxide octahedron between two layers of silicon oxide tetrahedrons and sharing oxygen atoms, and the MMT is subjected to organic treatment and then is combined with a polymer, so that the composite material has excellent mechanical property, thermal property, flame retardant property and high barrier property.
According to the invention, the advantages of graphene-silver nano ions in terms of conductivity and excellent thermal performance and flame retardance reinforcing effect of the organic montmorillonite OMMT are utilized, and the graphene-silver nano ions are compounded and applied to the modification of the organic silicon pressure-sensitive adhesive, so that the synergistic reinforcing effect can be achieved by the combination, and the conductivity and the heat resistance of the silica gel pressure-sensitive adhesive can be effectively improved.
In a preferred embodiment, the weight ratio of the MQ resin to the silicone rubber is 10:90-40:60; the addition amount of the modified nanoparticle mixture is 1-5% of the total weight of the MQ resin and the silicone rubber; the addition amount of the organosiloxane cross-linking agent is 1-5% of the total weight of the MQ resin and the silicone rubber; the addition amount of the catalyst is 0.1-1% of the total weight of the MQ resin and the silicone rubber.
In a preferred embodiment, the MQ resin is formed by hydrolytic condensation of hexamethyldisiloxane as an M group and ethyl orthosilicate or water glass as a Q group, the molar ratio of the M group to the Q group is 0.8:1-1.0:1, and the number average molecular weight Mn of the MQ resin is 4000-8000.
In a preferred embodiment, the organosiloxane cross-linking agent is one or more of vinyltriethoxysilane, aminopropyltriethoxysilane, methyltributylketonoxime silane, methyltriacetoxy silane;
in a preferred embodiment, the catalyst is a platinum system catalyst.
The foregoing is a general inventive concept and the following detailed examples and comparative examples are provided on the basis thereof to further illustrate the invention.
The preparation methods of the graphene-silver nanocomposite and the organized montmorillonite OMMT in the following examples and comparative examples are the same, and specifically as follows.
The graphene-silver nanocomposite is prepared by the following method:
adding 0.1g of graphite oxide into 500mL of deionized water, and uniformly dispersing after ultrasonic treatment for 2 hours to obtain graphene oxide dispersion liquid;
and adding 0.05g of silver nitrate crystal into the graphene oxide dispersion liquid, uniformly stirring, filtering, washing the obtained solid product with deionized water for 3 times, and drying to obtain the graphene oxide-silver nanocomposite.
The organized montmorillonite OMMT is prepared by the following method:
adding 0.2g of montmorillonite into 200mL of distilled water, stirring at 80 ℃ for 20min, dissolving montmorillonite, then adding 0.05g of octadecyl trimethyl ammonium chloride, stirring for 3h, carrying out suction filtration, washing a solid product with distilled water, drying, and grinding to below 200 meshes to obtain the organic montmorillonite OMMT.
In the following examples and comparative examples, the organosiloxane crosslinker is vinyltriethoxysilane; the catalyst is a platinum system catalyst: ceramic catalyst 4000 。
Example 1
The silica gel pressure-sensitive adhesive with high-temperature resistance conductivity comprises the following raw material components: silicone rubber, MQ resin, modified nanoparticle mixture, organosiloxane crosslinker, and catalyst.
Wherein the weight ratio of the MQ resin to the silicone rubber is 20:80; the addition amount of the modified nanoparticle mixture is 1% of the total weight of the MQ resin and the silicone rubber; the addition amount of the organosiloxane cross-linking agent is 2% of the total weight of the MQ resin and the silicone rubber; the addition amount of the catalyst is 0.5 percent of the total weight of the MQ resin and the silicone rubber.
The preparation method of the silica gel pressure-sensitive adhesive comprises the following steps:
s1, preparing a modified nanoparticle mixture solution: oxidized graphene-silver nanocomposite material according to mass ratio: mixing the organic montmorillonite OMMT at a ratio of 3:1 to obtain a modified nanoparticle mixture, adding the modified nanoparticle mixture into toluene, and uniformly stirring to obtain a modified nanoparticle mixture solution with a mass concentration of 45%;
s2, mixing MQ resin and silicone rubber, adding the modified nanoparticle mixture solution, stirring for 1h, adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
Example 2
The silica gel pressure-sensitive adhesive with high-temperature resistance conductivity comprises the following raw material components: silicone rubber, MQ resin, modified nanoparticle mixture, organosiloxane crosslinker, and catalyst.
Wherein the weight ratio of the MQ resin to the silicone rubber is 20:80; the addition amount of the modified nanoparticle mixture is 1% of the total weight of the MQ resin and the silicone rubber; the addition amount of the organosiloxane cross-linking agent is 2% of the total weight of the MQ resin and the silicone rubber; the addition amount of the catalyst is 0.5 percent of the total weight of the MQ resin and the silicone rubber.
The preparation method of the silica gel pressure-sensitive adhesive comprises the following steps:
s1, preparing a modified nanoparticle mixture solution: oxidized graphene-silver nanocomposite material according to mass ratio: mixing the organic montmorillonite OMMT at a ratio of 2:1 to obtain a modified nanoparticle mixture, adding the modified nanoparticle mixture into toluene, and uniformly stirring to obtain a modified nanoparticle mixture solution with a mass concentration of 45%;
s2, mixing MQ resin and silicone rubber, adding the modified nanoparticle mixture solution, stirring for 1h, adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
Comparative example 1
The silica gel pressure-sensitive adhesive comprises the following raw material components: silicone rubber, MQ resin, organosiloxane cross-linking agent, and catalyst.
Wherein the weight ratio of the MQ resin to the silicone rubber is 20:80; the addition amount of the organosiloxane cross-linking agent is 2% of the total weight of the MQ resin and the silicone rubber; the addition amount of the catalyst is 0.5 percent of the total weight of the MQ resin and the silicone rubber.
The preparation method of the silica gel pressure-sensitive adhesive comprises the following steps: mixing MQ resin and silicone rubber, adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
Comparative example 2
This example is substantially the same as example 2, except that the modified nanoparticle mixture of example 2, i.e., the preparation method of the silica gel pressure-sensitive adhesive in this example, is replaced with a graphene-silver nanocomposite material in this example, which comprises the following steps:
s1, adding a graphene oxide-silver nanocomposite material into toluene, and uniformly stirring to obtain a graphene oxide-silver nanocomposite material solution with the mass concentration of 45%;
s2, mixing MQ resin and silicone rubber, then adding graphene oxide-silver nanocomposite solution, stirring for 1h, then adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
Comparative example 3
This example is substantially the same as example 2, except that in this example an organized montmorillonite OMMT is used instead of the modified nanoparticle mixture of example 2, i.e. the method for preparing a silicone pressure sensitive adhesive in this example comprises the following steps:
s1, adding an organic montmorillonite OMMT into toluene, and uniformly stirring to obtain an organic montmorillonite OMMT solution with the mass concentration of 45%;
s2, mixing MQ resin and silicone rubber, then adding graphene oxide-silver nanocomposite solution, stirring for 1h, then adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
The silicone pressure-sensitive adhesives prepared in examples 1-2 and comparative examples 1-3 were subjected to the following performance tests:
(1) The heat-resistant temperature test method comprises the following steps: thermogravimetric analysis (TGA)
(2) Detecting the volume resistivity at 25 ℃; normal temperature
The test results are shown in table 1 below:
TABLE 1
| Heat resistant temperature/°c | Volume resistivity/Ω cm | |
| Example 1 | 340 | 1×10 -1 |
| Example 2 | 350 | 1×10 -1 |
| Comparative example 1 | 260 | 1×10 3 |
| Comparative example 2 | 275 | 1.9×10 2 |
| Comparative example 3 | 318 | 7.7×10 2 |
As can be seen from the results of table 1, the silica gel pressure-sensitive adhesives of examples 1-2 have excellent high temperature resistance and good electrical conductivity; the results of comparative examples 1-3 show that the compound addition of the graphene oxide-silver nanocomposite and the organic montmorillonite OMMT has synergistic enhancement effect on the improvement of the high temperature resistance and the conductivity of the silica gel pressure-sensitive adhesive.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (10)
1. The silica gel pressure-sensitive adhesive with high-temperature resistance and conductivity is characterized by comprising the following raw material components: silicone rubber, MQ resin, modified nanoparticle mixture, organosiloxane crosslinker, and catalyst;
the modified nanoparticle mixture is obtained by mixing graphene oxide-silver nanocomposite and organic montmorillonite OMMT according to a mass ratio of 1:2-4:1.
2. The silica gel pressure-sensitive adhesive with high-temperature resistance and conductivity according to claim 1, wherein the graphene oxide-silver nanocomposite is prepared by the following method:
adding 0.01-1g of graphite oxide into 50-5000mL of deionized water, and uniformly dispersing after ultrasonic treatment for 1-4 hours to obtain graphene oxide dispersion liquid;
and adding 0.01-0.1 g of silver nitrate crystal into the graphene oxide dispersion liquid, uniformly stirring, filtering, washing the obtained solid product with deionized water, and drying to obtain the graphene oxide-silver nanocomposite.
3. The silica gel pressure-sensitive adhesive with high-temperature resistance and conductivity according to claim 2, wherein the graphene oxide-silver nanocomposite is prepared by the following method:
adding 0.1g of graphite oxide into 500mL of deionized water, and uniformly dispersing after ultrasonic treatment for 2 hours to obtain graphene oxide dispersion liquid;
and adding 0.05g of silver nitrate crystal into the graphene oxide dispersion liquid, uniformly stirring, filtering, washing the obtained solid product with deionized water for 3 times, and drying to obtain the graphene oxide-silver nanocomposite.
4. The silica gel pressure-sensitive adhesive with high temperature resistance and conductivity according to claim 1, wherein the organized montmorillonite OMMT is prepared by the following method:
adding 0.1-10 g of montmorillonite into 50-500mL of distilled water, heating and stirring until the montmorillonite is dissolved, then adding 0.01-0.1 g of octadecyl quaternary ammonium salt, stirring for 1-6h, carrying out suction filtration, washing a solid product with distilled water, drying and grinding to obtain the organic montmorillonite OMMT.
5. The silica gel pressure-sensitive adhesive with high temperature resistance and conductivity according to claim 4, wherein the organized montmorillonite OMMT is prepared by the following method:
adding 0.2g of montmorillonite into 200mL of distilled water, stirring at 80 ℃ for 20min, dissolving montmorillonite, adding 0.05g of octadecyl quaternary ammonium salt, stirring for 3h, suction filtering, washing solid product with distilled water, drying, and grinding to below 200 meshes to obtain the organic montmorillonite OMMT.
6. The silica gel pressure-sensitive adhesive with high temperature resistance according to claim 4 or 5, wherein the octadecyl quaternary ammonium salt is octadecyl trimethyl ammonium chloride.
7. The silica gel pressure-sensitive adhesive with high temperature resistance and conductivity according to claim 1, wherein the weight ratio of the MQ resin to the silicone rubber is 10:90-40:60;
the addition amount of the modified nanoparticle mixture is 1-5% of the total weight of the MQ resin and the silicone rubber;
the addition amount of the organosiloxane cross-linking agent is 1-5% of the total weight of the MQ resin and the silicone rubber;
the addition amount of the catalyst is 0.1-1% of the total weight of the MQ resin and the silicone rubber.
8. The silica gel pressure-sensitive adhesive with high-temperature conductivity according to claim 7, wherein the MQ resin is formed by hydrolytic condensation of hexamethyldisiloxane as an M group and tetraethoxysilane or water glass as a Q group, the molar ratio of the M group to the Q group is 0.8:1 to 1.0:1, and the number average molecular weight Mn of the MQ resin is 4000 to 8000.
9. The silica gel pressure-sensitive adhesive with high-temperature conductivity according to claim 7, wherein said organosiloxane cross-linking agent is one or more of vinyl triethoxysilane, aminopropyl triethoxysilane, methyltributylketon oximido silane, methyltriacetoxy silane;
the catalyst is a platinum system catalyst.
10. The silica gel pressure-sensitive adhesive with high temperature resistance and conductivity according to any one of claims 1 to 9, wherein the preparation method comprises the following steps:
s1, preparing a modified nanoparticle mixture solution: mixing the graphene oxide-silver nanocomposite with the organized montmorillonite OMMT to obtain a modified nanoparticle mixture, adding the modified nanoparticle mixture into toluene, and uniformly stirring to obtain a modified nanoparticle mixture solution;
s2, mixing MQ resin and silicone rubber, adding the modified nanoparticle mixture solution, stirring for 0.5-3h, adding an organosiloxane cross-linking agent and a catalyst, stirring uniformly, standing, and defoaming to obtain the high-temperature-resistant conductive silicone pressure-sensitive adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310298365.6A CN116285867A (en) | 2023-03-24 | 2023-03-24 | Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310298365.6A CN116285867A (en) | 2023-03-24 | 2023-03-24 | Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116285867A true CN116285867A (en) | 2023-06-23 |
Family
ID=86837656
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310298365.6A Withdrawn CN116285867A (en) | 2023-03-24 | 2023-03-24 | Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116285867A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730560A (en) * | 2005-08-16 | 2006-02-08 | 上海工程技术大学 | Add-on type liquid silicon rubber/organic montmorillonite nanometer composite material and its preparation method |
| CN107629467A (en) * | 2017-10-31 | 2018-01-26 | 定远县保尔工贸有限公司 | A kind of charger baby Silicone Case of good heat dissipation effect |
| CN109400960A (en) * | 2018-08-28 | 2019-03-01 | 江苏理工学院 | A kind of graphene/nano silver polymer composites and preparation method thereof |
| CN111548765A (en) * | 2020-05-09 | 2020-08-18 | 浙江祥隆科技有限公司 | Organosilicon system conductive adhesive and preparation method thereof |
| CN112029284A (en) * | 2020-09-10 | 2020-12-04 | 安徽大学 | Graphene oxide dispersion-assisted montmorillonite modified polysulfide rubber and preparation method thereof |
| CN112812739A (en) * | 2020-12-31 | 2021-05-18 | 河北诚和龙盛电力工程有限公司 | Silicone rubber self-adhesive tape and preparation method thereof |
-
2023
- 2023-03-24 CN CN202310298365.6A patent/CN116285867A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730560A (en) * | 2005-08-16 | 2006-02-08 | 上海工程技术大学 | Add-on type liquid silicon rubber/organic montmorillonite nanometer composite material and its preparation method |
| CN107629467A (en) * | 2017-10-31 | 2018-01-26 | 定远县保尔工贸有限公司 | A kind of charger baby Silicone Case of good heat dissipation effect |
| CN109400960A (en) * | 2018-08-28 | 2019-03-01 | 江苏理工学院 | A kind of graphene/nano silver polymer composites and preparation method thereof |
| CN111548765A (en) * | 2020-05-09 | 2020-08-18 | 浙江祥隆科技有限公司 | Organosilicon system conductive adhesive and preparation method thereof |
| CN112029284A (en) * | 2020-09-10 | 2020-12-04 | 安徽大学 | Graphene oxide dispersion-assisted montmorillonite modified polysulfide rubber and preparation method thereof |
| CN112812739A (en) * | 2020-12-31 | 2021-05-18 | 河北诚和龙盛电力工程有限公司 | Silicone rubber self-adhesive tape and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘建;田庆丰;李小红;张治军;: "纳米材料增强液体硅橡胶的研究进展", 合成橡胶工业, no. 06 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109778335B (en) | Modified polypropylene fiber and preparation method thereof | |
| EP1832553B1 (en) | Clay film product | |
| JP5761111B2 (en) | Insulating heat dissipation sheet and method for granulating boron nitride | |
| WO2011144010A1 (en) | Graphene based conductive material and preparation method thereof | |
| CN108102579A (en) | A kind of preparation method and application of high heat-conductivity conducting glue | |
| CN104861910A (en) | Graphene-coated inorganic filler and epoxy resin composite adhesive and preparation method thereof | |
| Meer et al. | Attributes of polymer and silica nanoparticle composites: A review | |
| CN107418204B (en) | Preparation method of graphene @ calcium copper titanate-polybenzoxazole three-phase composite film | |
| JP7311415B2 (en) | Epoxy paste composition containing core-shell structured silver-coated copper nanowires and conductive film containing the same | |
| CN112188660B (en) | Preparation method of water-based graphene-based electrothermal film | |
| CN103183889A (en) | High-thermal-conductivity and insulating polymer composite material and preparation method thereof | |
| CN106674599B (en) | The preparation method and application of silicon rubber functionalization graphene | |
| CN111732743A (en) | Preparation method of carbon nanotube/graphene flexible film | |
| CN108299830B (en) | Silicone rubber-based flexible graphene heating film, preparation method thereof, heating device and application | |
| CN113493619A (en) | Graphene surface-coated silicon dioxide composite material and preparation method and application thereof | |
| US20110152553A1 (en) | Carbon nanotube composite and preparation method of the same | |
| CN112608689B (en) | Antistatic organic silicon pressure-sensitive adhesive containing electron transport material and preparation method thereof | |
| CN110713816A (en) | Organosilicon electromagnetic shielding pressure-sensitive adhesive and preparation method thereof | |
| CN116285867A (en) | Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof | |
| CN106467670B (en) | A kind of preparation method of silver nanoparticle mixed fillers modified silicon rubber conducing composite material | |
| CN112480684B (en) | Silanized graphene/silicone rubber composite material and preparation method and application thereof | |
| JP6019761B2 (en) | Planar heating element and manufacturing method thereof | |
| JP2004091251A (en) | Method for reducing thin-film particle having framework comprising carbon | |
| CN109651622B (en) | synthetic method of organic silicon modified carbon nano-tube suitable for pressure-sensitive adhesive system | |
| CN110343419B (en) | High-thermal-conductivity insulating polyimide ink 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 | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20230623 |
|
| WW01 | Invention patent application withdrawn after publication |