CN115418182B - High-temperature-resistant high-conductivity pressure-sensitive adhesive and preparation method thereof - Google Patents
High-temperature-resistant high-conductivity pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- CN115418182B CN115418182B CN202211140052.XA CN202211140052A CN115418182B CN 115418182 B CN115418182 B CN 115418182B CN 202211140052 A CN202211140052 A CN 202211140052A CN 115418182 B CN115418182 B CN 115418182B
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 38
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 38
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000003607 modifier Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 64
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 54
- 238000002156 mixing Methods 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 32
- 239000007795 chemical reaction product Substances 0.000 claims description 32
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 28
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 22
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 22
- 239000002244 precipitate Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 19
- 238000010992 reflux Methods 0.000 claims description 16
- 238000010025 steaming Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- YXYJVFYWCLAXHO-UHFFFAOYSA-N 2-methoxyethyl 2-methylprop-2-enoate Chemical compound COCCOC(=O)C(C)=C YXYJVFYWCLAXHO-UHFFFAOYSA-N 0.000 claims description 14
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 14
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 14
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 13
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 11
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 11
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 11
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 11
- 239000003999 initiator Substances 0.000 claims description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical group CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- QNWOFLWXQGHSRH-UHFFFAOYSA-N trimethyl-[methyl(trimethylsilyloxy)silyl]oxysilane Chemical compound C[Si](C)(C)O[SiH](C)O[Si](C)(C)C QNWOFLWXQGHSRH-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000010355 oscillation Effects 0.000 claims description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 2
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 2
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 2
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 2
- HQVFKSDWNYVAQD-UHFFFAOYSA-N n-hydroxyprop-2-enamide Chemical compound ONC(=O)C=C HQVFKSDWNYVAQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000006258 conductive agent Substances 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 230000033444 hydroxylation Effects 0.000 description 4
- 238000005805 hydroxylation reaction Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- 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
- C09J143/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Adhesives based on derivatives of such polymers
- C09J143/04—Homopolymers or copolymers of monomers containing silicon
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a high-temperature-resistant high-conductivity pressure-sensitive adhesive and a preparation method thereof; the conductive pressure-sensitive adhesive prepared by the invention firstly uses organic silicon as a modifier, and improves the high temperature resistance by means of higher bond energy; meanwhile, the nano silver and the modified carbon nano tube are also doped as the conductive agent, so that good conductivity can be achieved, and the branched acrylic polymer is grafted on the surface of the modified carbon nano tube prepared by the method, so that the bonding capability of the carbon nano tube and an acrylic pressure-sensitive adhesive system is enhanced, the effect of effectively improving the cohesive force of the acrylic pressure-sensitive adhesive can be achieved in a high-temperature environment, and the high-temperature resistance of the pressure-sensitive adhesive is enhanced. The high-temperature-resistant conductive pressure-sensitive adhesive prepared by the invention has strong conductive capability, good high-temperature resistance and stable property, can be suitable for most high-temperature conductive operations, and has wide application prospects in the related fields.
Description
Technical Field
The invention relates to the technical field of pressure-sensitive adhesives, in particular to a high-temperature-resistant high-conductivity pressure-sensitive adhesive and a preparation method thereof.
Background
The acrylic conductive pressure-sensitive adhesive has the characteristics of good adhesive property, low cost, stable performance and good cohesive strength, and can be used in most application environments in production and life, but with technological development, people have higher requirements on the performance of the pressure-sensitive adhesive so as to face the development of fields such as automobiles, electronics and the like, especially in the electronics field, as the electronic element can generate heat in the use process, the temperature is increased, the conventional acrylic conductive pressure-sensitive adhesive tends to have the phenomena of lower adhesive strength, adhesive residue and the like at high temperature, and the use requirements cannot be met, so that the conventional acrylic conductive pressure-sensitive adhesive is needed to be suitable for the high-temperature environment.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant high-conductivity pressure-sensitive adhesive and a preparation method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a high temperature resistant and high conductivity pressure sensitive adhesive, which has the following characteristics: the high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following components in parts by weight: 25-45 parts of acrylic soft monomer, 6-12 parts of acrylic hard monomer, 2-6 parts of functional monomer, 5-12 parts of organosilicon modifier, 4-8 parts of conductive particles, 6-8 parts of modified carbon nano tubes, 0.05-0.2 part of cross-linking agent, 0.1-0.3 part of initiator and 15-20 parts of solvent.
Further, the acrylic soft body is any one or more of methyl methacrylate, ethyl methacrylate, butyl methacrylate, isooctyl acrylate and lauryl acrylate;
the acrylic hard monomer is any one or more of dimethylaminoethyl methacrylate, methoxyethyl methacrylate, hydroxyethyl acrylate and hydroxypropyl acrylate;
the functional monomer is any one or more of acrylamide or hydroxy acrylamide.
Further, the organosilicon modifier is (3-acryloyloxy) methyl bis (trimethylsiloxy) silane; the conductive particles are any one or more of carbon black, nickel powder and nano silver.
Preferably, the conductive particles are nano silver.
Further, the cross-linking agent is glycidyl methacrylate; the initiator is any one of benzoyl peroxide and azodiisobutyronitrile.
Further, the solvent is any one or more of ethyl acetate, toluene and acetone.
A preparation method of a high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following steps:
s1, modifying a carbon nano tube;
s11, adding the carbon nano tube into a nitric acid solution, performing ultrasonic dispersion for 3-6 hours, heating to 70-90 ℃, reacting for 6-8 hours, filtering, collecting precipitate, treating with a sodium hydroxide solution, heating to 90-100 ℃, performing ultrasonic dispersion and reacting for 12-18 hours, filtering, and performing vacuum drying to obtain the carbon nano tube with the surface hydroxylated;
s12, adding the surface hydroxylated carbon nano tube into pure water, dropwise adding dilute hydrochloric acid, regulating the pH value to 5-6.5, performing ultrasonic dispersion for 1-1.5h, adding gamma-methacryloxypropyl trimethoxy silane, heating to 80-95 ℃, performing reflux reaction for 12-18h, performing suction filtration, collecting precipitate, and performing vacuum drying to obtain activated carbon nano tube;
s13, dissolving diethylenetriamine in DMF, slowly adding phthalic anhydride, heating to 50-70 ℃ in a water bath, stirring for reaction for 8-12h, heating to 140-160 ℃, refluxing for reaction for 18-24h, steaming the reaction product, removing excessive solvent, dissolving the reaction product in DMF again, adding butyl acrylate, heating to 60-75 ℃, reacting for 24-36h, steaming the reaction product, removing excessive solvent, washing the reaction product for 4-8 times by using methanol, and drying in vacuum to obtain branched acrylic acid polymer;
s14, dissolving a branched acrylic polymer in DMF (dimethyl formamide) according to parts by weight, adding the activated carbon nanotube prepared in the step S2, slowly dropwise adding potassium persulfate after ultrasonic oscillation treatment for 30-45min, heating to 45-60 ℃ for 8-12h, filtering, and vacuum drying to obtain a modified carbon nanotube;
s2, mixing 3/5 of acrylic soft monomer and 3/5 of acrylic hard monomer with all functional monomers, organosilicon modifier, nano silver and modified carbon nano tube, heating to 80-90 ℃, mixing for 1-1.5h, adding one half of initiator, and continuing mixing reaction for 2-3h;
s3, adding the rest acrylic acid soft monomer and the acrylic acid hard monomer, mixing for 0.5h, adding the rest initiator, all the crosslinking agent and the solvent, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
In order to improve the high temperature resistance of the conductive pressure-sensitive adhesive, the invention firstly uses an organosilicon modified pressure-sensitive adhesive system, and the organosilicon contains Si-O bonds with high bond energy, so that the system stability of the pressure-sensitive adhesive can be effectively improved, the heat resistance of the pressure-sensitive adhesive is enhanced, and the chemical resistance and stability of the pressure-sensitive adhesive system are improved. However, the organic silicon component has low surface energy, and the dispersibility and the binding capacity of the conductive agent component in the pressure-sensitive adhesive can be reduced after the organic silicon is added, so that the addition amount of the nano silver conductive agent is reduced on the basis, and the modified carbon nano tube is additionally prepared;
the invention firstly uses the conventional carbon nano tube as a raw material, uses concentrated nitric acid to corrode the surface of the carbon nano tube to increase the surface area of the carbon nano tube, further uses sodium hydroxide solution to remove nitric acid residues, grafts hydroxyl on the surface of the carbon nano tube, then mixes the carbon nano tube with gamma-methacryloxypropyl trimethoxy silane, hydrolyzes the carbon nano tube to generate active double bonds on the surface of the carbon nano tube, increases the chemical activity of the carbon nano tube, and is convenient for grafting branched acrylic acid polymer.
The preparation method comprises the steps of firstly preparing a polyamide material with a branched structure by using diethylenetriamine and phthalic anhydride, then grafting the polyamide material with butyl acrylate to form an acrylic polymer with a branched structure, then mixing the acrylic polymer with activated carbon nano tubes, grafting an acrylic polymer with an end group of acrylic acid on the surface of the carbon nano tubes under the participation of potassium persulfate, and finally mixing the acrylic polymer with substances such as acrylic soft monomers, hard monomers and the like, forming a crosslinked network under the action of an initiator, and preparing the high-temperature-resistant conductive pressure-sensitive adhesive.
In the invention, the modified carbon nano tube and the nano silver simultaneously play a role of a conductive agent, the modified carbon nano tube has extremely high length-diameter ratio, and can be crosslinked and entangled in an acrylic acid system to form a conductive network, so that the conductive efficiency can be greatly improved.
Further, in step S11, the concentration of the nitric acid solution is 60-65wt% and the concentration of the sodium hydroxide solution is 30-40%.
Further, in the step S12, the mass ratio of the surface hydroxylated carbon nanotube to the γ -methacryloxypropyl trimethoxysilane is (1-1.8): (3.5-7.2).
Further, in the step S13, the molar ratio of diethylenetriamine, phthalic anhydride and butyl acrylate is (3-4.5): (2.5-4): (0.5-1.5).
Further, in the step S14, the mass ratio of the branched acrylic polymer, the activated carbon nanotube and the potassium persulfate is (0.5-2.5): (5-10): (0.01-0.03).
Compared with the prior art, the invention has the following beneficial effects: the conductive pressure-sensitive adhesive prepared by the invention firstly uses organic silicon as a modifier, and improves the high temperature resistance by means of higher bond energy; meanwhile, the nano silver and the modified carbon nano tube are also doped as the conductive agent, so that good conductivity can be achieved, and the branched acrylic polymer is grafted on the surface of the modified carbon nano tube prepared by the method, so that the bonding capability of the carbon nano tube and an acrylic pressure-sensitive adhesive system is enhanced, the effect of effectively improving the cohesive force of the acrylic pressure-sensitive adhesive can be achieved in a high-temperature environment, and the high-temperature resistance of the pressure-sensitive adhesive is enhanced. The high-temperature-resistant conductive pressure-sensitive adhesive prepared by the invention has strong conductive capability, good high-temperature resistance and stable property, can be suitable for most high-temperature conductive operations, and has wide application prospects in the related fields.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1.
A preparation method of a high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following steps:
s1, modifying a carbon nano tube;
s11, adding the carbon nano tube into a nitric acid solution with the concentration of 60wt percent and completely immersing, using ultrasonic dispersion with the frequency of 30KHz for 3 hours, heating to 70 ℃, reacting for 6 hours, filtering, collecting the precipitate, immersing the precipitate in a sodium hydroxide solution with the concentration of 30wt percent, heating to 90 ℃, carrying out ultrasonic dispersion and reaction for 12 hours, filtering, and drying at the vacuum temperature of 60 ℃ for 8 hours to obtain the carbon nano tube with the surface hydroxylated;
s12, adding 1 part of carbon nano tube with surface hydroxylation into 50 parts of pure water according to parts by weight, dropwise adding dilute hydrochloric acid, regulating the pH value to 5, performing ultrasonic dispersion for 1h, adding 3.5 parts of gamma-methacryloxypropyl trimethoxy silane, heating to 80 ℃, performing reflux reaction for 12h, performing suction filtration, collecting precipitate, and performing vacuum drying at 60 ℃ for 12h to obtain activated carbon nano tube;
s13, dissolving 3 parts of diethylenetriamine in 5 parts of DMF (dimethyl formamide), slowly adding 2.5 parts of phthalic anhydride, heating to 50 ℃ in a water bath, stirring for reaction for 8 hours, heating to 140 ℃, refluxing for 18 hours, steaming the reaction product, removing excessive solvent, dissolving the reaction product in 10 parts of DMF again, adding 0.5 part of butyl acrylate, heating to 60 ℃, reacting for 24 hours, steaming the reaction product, removing excessive solvent, washing the reaction product for 4 times by using methanol, and drying at 60 ℃ in vacuum for 24 hours to obtain a branched acrylic polymer;
s14, according to parts by weight, dissolving 0.5 part of branched acrylic polymer in 30 parts of DMF, adding 5 parts of activated carbon nanotube prepared in the step S2, slowly dropwise adding 0.03 part of potassium persulfate after ultrasonic oscillation treatment for 30min, wherein the dropwise adding time is 1.5h, heating to 45 ℃, reacting for 8h, filtering, and drying at 60 ℃ in vacuum for 12h to obtain modified carbon nanotube;
s2, mixing 15 parts of butyl methacrylate, 3.6 parts of methoxyethyl methacrylate, 2 parts of acrylamide, 5 parts of (3-acryloyloxy) methyl bis (trimethylsiloxy) silane, 4 parts of nano silver and 4 parts of modified carbon nano tube according to parts by weight, heating to 80 ℃, mixing for 1h, adding 0.05 part of benzoyl peroxide, and continuing to carry out a mixing reaction for 2h;
s3, adding 10 parts of butyl methacrylate and 2.4 parts of methoxyethyl methacrylate, mixing for 0.5h, adding 0.05 part of benzoyl peroxide, 0.05 part of glycidyl methacrylate and 15 parts of ethyl acetate, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
Example 2.
In this example, the addition amount of γ -methacryloxypropyl trimethoxysilane in step S12 was increased as compared with example 1;
a preparation method of a high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following steps:
s1, modifying a carbon nano tube;
s11, adding the carbon nano tube into a nitric acid solution with the concentration of 60wt percent and completely immersing, using ultrasonic dispersion with the frequency of 30KHz for 3 hours, heating to 70 ℃, reacting for 6 hours, filtering, collecting the precipitate, immersing the precipitate in a sodium hydroxide solution with the concentration of 30wt percent, heating to 90 ℃, carrying out ultrasonic dispersion and reaction for 12 hours, filtering, and drying at the vacuum temperature of 60 ℃ for 8 hours to obtain the carbon nano tube with the surface hydroxylated;
s12, adding 1 part of carbon nano tube with surface hydroxylation into 50 parts of pure water according to parts by weight, dropwise adding dilute hydrochloric acid, regulating the pH value to 5, performing ultrasonic dispersion for 1h, adding 7.2 parts of gamma-methacryloxypropyl trimethoxy silane, heating to 80 ℃, performing reflux reaction for 12h, performing suction filtration, collecting precipitate, and performing vacuum drying at 60 ℃ for 12h to obtain activated carbon nano tube;
s13, dissolving 3 parts of diethylenetriamine in 5 parts of DMF (dimethyl formamide), slowly adding 2.5 parts of phthalic anhydride, heating to 50 ℃ in a water bath, stirring for reaction for 8 hours, heating to 140 ℃, refluxing for 18 hours, steaming the reaction product, removing excessive solvent, dissolving the reaction product in 10 parts of DMF again, adding 0.5 part of butyl acrylate, heating to 60 ℃, reacting for 24 hours, steaming the reaction product, removing excessive solvent, washing the reaction product for 4 times by using methanol, and drying at 60 ℃ in vacuum for 24 hours to obtain a branched acrylic polymer;
s14, according to parts by weight, dissolving 0.5 part of branched acrylic polymer in 30 parts of DMF, adding 5 parts of activated carbon nanotube prepared in the step S2, slowly dropwise adding 0.03 part of potassium persulfate after ultrasonic oscillation treatment for 30min, wherein the dropwise adding time is 1.5h, heating to 45 ℃, reacting for 8h, filtering, and drying at 60 ℃ in vacuum for 12h to obtain modified carbon nanotube;
s2, mixing 15 parts of butyl methacrylate, 3.6 parts of methoxyethyl methacrylate, 2 parts of acrylamide, 5 parts of (3-acryloyloxy) methyl bis (trimethylsiloxy) silane, 4 parts of nano silver and 4 parts of modified carbon nano tube according to parts by weight, heating to 80 ℃, mixing for 1h, adding 0.05 part of benzoyl peroxide, and continuing to carry out a mixing reaction for 2h;
s3, adding 10 parts of butyl methacrylate and 2.4 parts of methoxyethyl methacrylate, mixing for 0.5h, adding 0.05 part of benzoyl peroxide, 0.05 part of glycidyl methacrylate and 15 parts of ethyl acetate, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
Example 3.
Compared with example 1, this example increases the addition amount of the branched acrylic polymer in step S14;
a preparation method of a high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following steps:
s1, modifying a carbon nano tube;
s11, adding the carbon nano tube into a nitric acid solution with the concentration of 60wt percent and completely immersing, using ultrasonic dispersion with the frequency of 30KHz for 3 hours, heating to 70 ℃, reacting for 6 hours, filtering, collecting the precipitate, immersing the precipitate in a sodium hydroxide solution with the concentration of 30wt percent, heating to 90 ℃, carrying out ultrasonic dispersion and reaction for 12 hours, filtering, and drying at the vacuum temperature of 60 ℃ for 8 hours to obtain the carbon nano tube with the surface hydroxylated;
s12, adding 1 part of carbon nano tube with surface hydroxylation into 50 parts of pure water according to parts by weight, dropwise adding dilute hydrochloric acid, regulating the pH value to 5, performing ultrasonic dispersion for 1h, adding 3.5 parts of gamma-methacryloxypropyl trimethoxy silane, heating to 80 ℃, performing reflux reaction for 12h, performing suction filtration, collecting precipitate, and performing vacuum drying at 60 ℃ for 12h to obtain activated carbon nano tube;
s13, dissolving 3 parts of diethylenetriamine in 5 parts of DMF (dimethyl formamide), slowly adding 2.5 parts of phthalic anhydride, heating to 50 ℃ in a water bath, stirring for reaction for 8 hours, heating to 140 ℃, refluxing for 18 hours, steaming the reaction product, removing excessive solvent, dissolving the reaction product in 10 parts of DMF again, adding 0.5 part of butyl acrylate, heating to 60 ℃, reacting for 24 hours, steaming the reaction product, removing excessive solvent, washing the reaction product for 4 times by using methanol, and drying at 60 ℃ in vacuum for 24 hours to obtain a branched acrylic polymer;
s14, dissolving 2.5 parts of branched acrylic polymer in 30 parts of DMF (dimethyl formamide), adding 5 parts of activated carbon nanotubes prepared in the step S2, slowly dropwise adding 0.03 part of potassium persulfate after ultrasonic oscillation treatment for 30min, wherein the dropwise adding time is 1.5h, heating to 45 ℃, reacting for 8h, filtering, and drying at the vacuum temperature of 60 ℃ for 12h to obtain modified carbon nanotubes;
s2, mixing 15 parts of butyl methacrylate, 3.6 parts of methoxyethyl methacrylate, 2 parts of acrylamide, 5 parts of (3-acryloyloxy) methyl bis (trimethylsiloxy) silane, 4 parts of nano silver and 4 parts of modified carbon nano tube according to parts by weight, heating to 80 ℃, mixing for 1h, adding 0.05 part of benzoyl peroxide, and continuing to carry out a mixing reaction for 2h;
s3, adding 10 parts of butyl methacrylate and 2.4 parts of methoxyethyl methacrylate, mixing for 0.5h, adding 0.05 part of benzoyl peroxide, 0.05 part of glycidyl methacrylate and 15 parts of ethyl acetate, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
Example 4.
Compared with example 1, this example increases the addition amount of the modified carbon nanotubes in step S2;
a preparation method of a high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following steps:
s1, modifying a carbon nano tube;
s11, adding the carbon nano tube into a nitric acid solution with the concentration of 60wt percent and completely immersing, using ultrasonic dispersion with the frequency of 30KHz for 3 hours, heating to 70 ℃, reacting for 6 hours, filtering, collecting the precipitate, immersing the precipitate in a sodium hydroxide solution with the concentration of 30wt percent, heating to 90 ℃, carrying out ultrasonic dispersion and reaction for 12 hours, filtering, and drying at the vacuum temperature of 60 ℃ for 8 hours to obtain the carbon nano tube with the surface hydroxylated;
s12, adding 1 part of carbon nano tube with surface hydroxylation into 50 parts of pure water according to parts by weight, dropwise adding dilute hydrochloric acid, regulating the pH value to 5, performing ultrasonic dispersion for 1h, adding 3.5 parts of gamma-methacryloxypropyl trimethoxy silane, heating to 80 ℃, performing reflux reaction for 12h, performing suction filtration, collecting precipitate, and performing vacuum drying at 60 ℃ for 12h to obtain activated carbon nano tube;
s13, dissolving 3 parts of diethylenetriamine in 5 parts of DMF (dimethyl formamide), slowly adding 2.5 parts of phthalic anhydride, heating to 50 ℃ in a water bath, stirring for reaction for 8 hours, heating to 140 ℃, refluxing for 18 hours, steaming the reaction product, removing excessive solvent, dissolving the reaction product in 10 parts of DMF again, adding 0.5 part of butyl acrylate, heating to 60 ℃, reacting for 24 hours, steaming the reaction product, removing excessive solvent, washing the reaction product for 4 times by using methanol, and drying at 60 ℃ in vacuum for 24 hours to obtain a branched acrylic polymer;
s14, according to parts by weight, dissolving 0.5 part of branched acrylic polymer in 30 parts of DMF, adding 5 parts of activated carbon nanotube prepared in the step S2, slowly dropwise adding 0.03 part of potassium persulfate after ultrasonic oscillation treatment for 30min, wherein the dropwise adding time is 1.5h, heating to 45 ℃, reacting for 8h, filtering, and drying at 60 ℃ in vacuum for 12h to obtain modified carbon nanotube;
s2, mixing 15 parts of butyl methacrylate, 3.6 parts of methoxyethyl methacrylate, 2 parts of acrylamide, 5 parts of (3-acryloyloxy) methyl bis (trimethylsiloxy) silane, 4 parts of nano silver and 8 parts of modified carbon nano tube according to parts by weight, heating to 80 ℃, mixing for 1h, adding 0.05 part of benzoyl peroxide, and continuing to carry out a mixing reaction for 2h;
s3, adding 10 parts of butyl methacrylate and 2.4 parts of methoxyethyl methacrylate, mixing for 0.5h, adding 0.05 part of benzoyl peroxide, 0.05 part of glycidyl methacrylate and 15 parts of ethyl acetate, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
Example 5.
A preparation method of a high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following steps:
s1, modifying a carbon nano tube;
s11, adding the carbon nano tube into a 65wt% nitric acid solution, immersing completely, dispersing for 6 hours by using 30KHz ultrasonic wave, heating to 90 ℃, reacting for 8 hours, filtering, collecting precipitate, immersing the precipitate in a 40wt% sodium hydroxide solution, heating to 100 ℃, dispersing and reacting for 18 hours by ultrasonic wave, filtering, and drying at 60 ℃ in vacuum for 8 hours to obtain the carbon nano tube with the hydroxylated surface;
s12, adding 1.8 parts of surface hydroxylated carbon nano tube into 50 parts of pure water according to parts by weight, dropwise adding dilute hydrochloric acid, regulating the pH value to 5, performing ultrasonic dispersion for 1h, adding 6 parts of gamma-methacryloxypropyl trimethoxy silane, heating to 95 ℃, performing reflux reaction for 18h, performing suction filtration, collecting precipitate, and drying at 60 ℃ in vacuum for 12h to obtain activated carbon nano tube;
s13, dissolving 4.5 parts of diethylenetriamine in 10 parts of DMF (dimethyl formamide), slowly adding 4 parts of phthalic anhydride, heating to 70 ℃ in a water bath, stirring for reaction for 12 hours, heating to 160 ℃, refluxing for reaction for 24 hours, steaming the reaction product, removing excessive solvent, dissolving the reaction product in 10 parts of DMF again, adding 1.5 parts of butyl acrylate, heating to 75 ℃, reacting for 36 hours, steaming the reaction product, removing excessive solvent, washing the reaction product 8 times by using methanol, and drying at 60 ℃ in vacuum for 24 hours to obtain a branched acrylic polymer;
s14, dissolving 0.8 part of branched acrylic polymer in 30 parts of DMF (dimethyl formamide), adding 10 parts of activated carbon nanotubes prepared in the step S2, slowly dropwise adding 0.03 part of potassium persulfate after ultrasonic vibration treatment for 30min, wherein the dropwise adding time is 3h, heating to 60 ℃, reacting for 12h, filtering, and drying at 60 ℃ in vacuum for 12h to obtain modified carbon nanotubes;
s2, mixing 27 parts of butyl methacrylate, 7.2 parts of methoxyethyl methacrylate, 6 parts of acrylamide, 12 parts of (3-acryloyloxy) methyl bis (trimethylsiloxy) silane, 8 parts of nano silver and 8 parts of modified carbon nano tube according to parts by weight, heating to 80 ℃, mixing for 1h, adding 0.1 part of benzoyl peroxide, and continuing to carry out a mixing reaction for 2h;
s3, adding 18 parts of butyl methacrylate and 4.8 parts of methoxyethyl methacrylate, mixing for 0.5h, adding 0.1 part of benzoyl peroxide, 0.2 part of glycidyl methacrylate and 20 parts of ethyl acetate, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
Comparative example 1.
Compared with example 1, the modified carbon nanotubes were not prepared and replaced with an equivalent amount of nano silver;
a preparation method of a high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following steps:
s1, mixing 15 parts of butyl methacrylate, 3.6 parts of methoxyethyl methacrylate, 2 parts of acrylamide, 5 parts of (3-acryloyloxy) methyl bis (trimethylsiloxy) silane and 8 parts of nano silver according to parts by weight, heating to 80 ℃, mixing for 1h, adding 0.05 part of benzoyl peroxide, and continuing to perform a mixing reaction for 2h;
s2, adding 10 parts of butyl methacrylate and 2.4 parts of methoxyethyl methacrylate, mixing for 0.5h, adding 0.05 part of benzoyl peroxide, 0.05 part of glycidyl methacrylate and 15 parts of ethyl acetate, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
And (3) detection: the pressure-sensitive adhesive prepared in examples 1 to 5 and comparative example 1 was coated on a 25 μm copper foil and dried at 120℃for 3 minutes to form a pressure-sensitive adhesive tape sample having a dry adhesive thickness of 25. Mu.m;
detecting the holding power according to GB/T4851-2014;
and (3) high temperature resistance detection: the pressure-sensitive adhesive tape is stuck on a stainless steel plate, 2kg of press rolls are rolled for 2 rounds, the pressure-sensitive adhesive tape is respectively placed in an oven with the temperature gradient of 120-280 ℃, the oven is taken out after being placed for 1 hour, the pressure-sensitive adhesive tape is torn off after being cooled for 30 minutes, the phenomenon of residual glue is detected, and the highest temperature of no residual glue is used as the high temperature resistant temperature of the pressure-sensitive adhesive tape;
and (3) conductive performance detection: cutting the pressure-sensitive adhesive tape into a sample sheet with a side length of more than 1 square inch, and using a digital micro-resistance instrument to measure a surface resistance (XY direction) and a vertical resistance (Z direction) of 1 inch;
the detection results are shown in the following table:
finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a high temperature resistant high conductive pressure sensitive adhesive which characterized in that: the high-temperature-resistant high-conductivity pressure-sensitive adhesive comprises the following components in parts by weight: 25-45 parts of acrylic soft monomer, 6-12 parts of acrylic hard monomer, 2-6 parts of functional monomer, 5-12 parts of organosilicon modifier, 4-8 parts of conductive particles, 6-8 parts of modified carbon nano tubes, 0.05-0.2 part of cross-linking agent, 0.1-0.3 part of initiator and 15-20 parts of solvent;
the preparation method of the modified carbon nano tube comprises the following steps:
s11, adding the carbon nano tube into a nitric acid solution, performing ultrasonic dispersion for 3-6 hours, heating to 70-90 ℃, reacting for 6-8 hours, filtering, collecting precipitate, treating with a sodium hydroxide solution, heating to 90-100 ℃, performing ultrasonic dispersion and reacting for 12-18 hours, filtering, and performing vacuum drying to obtain the carbon nano tube with the surface hydroxylated;
s12, adding the surface hydroxylated carbon nano tube into pure water, dropwise adding dilute hydrochloric acid, regulating the pH value to 5-6.5, performing ultrasonic dispersion for 1-1.5h, adding gamma-methacryloxypropyl trimethoxy silane, heating to 80-95 ℃, performing reflux reaction for 12-18h, performing suction filtration, collecting precipitate, and performing vacuum drying to obtain activated carbon nano tube;
s13, dissolving diethylenetriamine in DMF, slowly adding phthalic anhydride, heating to 50-70 ℃ in a water bath, stirring for reaction for 8-12h, heating to 140-160 ℃, refluxing for reaction for 18-24h, steaming the reaction product, removing excessive solvent, dissolving the reaction product in DMF again, adding butyl acrylate, heating to 60-75 ℃, reacting for 24-36h, steaming the reaction product, removing excessive solvent, washing the reaction product for 4-8 times by using methanol, and drying in vacuum to obtain branched acrylic acid polymer;
s14, according to the weight portion, dissolving the branched acrylic polymer in DMF, adding the activated carbon nanotube prepared in the step S2, slowly dropwise adding potassium persulfate after ultrasonic oscillation treatment for 30-45min, heating to 45-60 ℃, reacting for 8-12h, filtering, and vacuum drying to obtain the modified carbon nanotube.
2. The high temperature resistant and high conductivity pressure sensitive adhesive according to claim 1, wherein: the acrylic soft body is any one or more of methyl methacrylate, ethyl methacrylate, butyl methacrylate, isooctyl acrylate and lauryl acrylate;
the acrylic hard monomer is any one or more of dimethylaminoethyl methacrylate, methoxyethyl methacrylate, hydroxyethyl acrylate and hydroxypropyl acrylate;
the functional monomer is any one or more of acrylamide or hydroxy acrylamide.
3. The high temperature resistant and high conductivity pressure sensitive adhesive according to claim 1, wherein: the organosilicon modifier is (3-acryloyloxy) methyl bis (trimethylsiloxy) silane;
the conductive particles are any one or more of carbon black, nickel powder and nano silver.
4. The high temperature resistant and high conductivity pressure sensitive adhesive according to claim 1, wherein: the cross-linking agent is glycidyl methacrylate; the initiator is any one of benzoyl peroxide and azodiisobutyronitrile.
5. The high temperature resistant and high conductivity pressure sensitive adhesive according to claim 1, wherein: the solvent is one or more of ethyl acetate, toluene and acetone.
6. A method for preparing the high-temperature-resistant high-conductivity pressure-sensitive adhesive according to any one of claims 1 to 5, comprising the steps of:
s1, modifying a carbon nano tube;
s11, adding the carbon nano tube into a nitric acid solution, performing ultrasonic dispersion for 3-6 hours, heating to 70-90 ℃, reacting for 6-8 hours, filtering, collecting precipitate, treating with a sodium hydroxide solution, heating to 90-100 ℃, performing ultrasonic dispersion and reacting for 12-18 hours, filtering, and performing vacuum drying to obtain the carbon nano tube with the surface hydroxylated;
s12, adding the surface hydroxylated carbon nano tube into pure water, dropwise adding dilute hydrochloric acid, regulating the pH value to 5-6.5, performing ultrasonic dispersion for 1-1.5h, adding gamma-methacryloxypropyl trimethoxy silane, heating to 80-95 ℃, performing reflux reaction for 12-18h, performing suction filtration, collecting precipitate, and performing vacuum drying to obtain activated carbon nano tube;
s13, dissolving diethylenetriamine in DMF, slowly adding phthalic anhydride, heating to 50-70 ℃ in a water bath, stirring for reaction for 8-12h, heating to 140-160 ℃, refluxing for reaction for 18-24h, steaming the reaction product, removing excessive solvent, dissolving the reaction product in DMF again, adding butyl acrylate, heating to 60-75 ℃, reacting for 24-36h, steaming the reaction product, removing excessive solvent, washing the reaction product for 4-8 times by using methanol, and drying in vacuum to obtain branched acrylic acid polymer;
s14, dissolving a branched acrylic polymer in DMF (dimethyl formamide) according to parts by weight, adding the activated carbon nanotube prepared in the step S2, slowly dropwise adding potassium persulfate after ultrasonic oscillation treatment for 30-45min, heating to 45-60 ℃ for 8-12h, filtering, and vacuum drying to obtain a modified carbon nanotube;
s2, mixing 3/5 of acrylic soft monomer and 3/5 of acrylic hard monomer with all functional monomers, organosilicon modifier, nano silver and modified carbon nano tube, heating to 80-90 ℃, mixing for 1-1.5h, adding one half of initiator, and continuing mixing reaction for 2-3h;
s3, adding the rest acrylic acid soft monomer and the acrylic acid hard monomer, mixing for 0.5h, adding the rest initiator, all the cross-linking agent and the solvent, continuously reacting for 120min, and cooling to room temperature to obtain the high-temperature-resistant conductive pressure-sensitive adhesive.
7. The method for preparing the high-temperature-resistant high-conductivity pressure-sensitive adhesive according to claim 6, wherein the method comprises the following steps: in the step S11, the concentration of the nitric acid solution is 60-65wt% and the concentration of the sodium hydroxide solution is 30-40%.
8. The method for preparing the high-temperature-resistant high-conductivity pressure-sensitive adhesive according to claim 6, wherein the method comprises the following steps: in the step S12, the mass ratio of the surface hydroxylated carbon nano tube to the gamma-methacryloxypropyl trimethoxy silane is (1-1.8): (3.5-7.2).
9. The method for preparing the high-temperature-resistant high-conductivity pressure-sensitive adhesive according to claim 6, wherein the method comprises the following steps: in the step S13, the mol ratio of diethylenetriamine, phthalic anhydride and butyl acrylate is (3-4.5): (2.5-4): (0.5-1.5).
10. The method for preparing the high-temperature-resistant high-conductivity pressure-sensitive adhesive according to claim 6, wherein the method comprises the following steps: in the step S14, the mass ratio of the branched acrylic polymer to the activated carbon nano tube to the potassium persulfate is (0.5-2.5): (5-10): (0.01-0.03).
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| KR20130103014A (en) * | 2012-03-09 | 2013-09-23 | 인하대학교 산학협력단 | Surface modification of carbon nanotubes using ultrasound |
| CN108192138A (en) * | 2016-12-08 | 2018-06-22 | 中国石油天然气股份有限公司 | Modification method of carbon nano tube used as rubber filler |
| CN114921202A (en) * | 2022-04-28 | 2022-08-19 | 深圳市通泰盈科技股份有限公司 | High-temperature-resistant acrylic pressure-sensitive adhesive, preparation method thereof, pressure-sensitive adhesive tape and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20130103014A (en) * | 2012-03-09 | 2013-09-23 | 인하대학교 산학협력단 | Surface modification of carbon nanotubes using ultrasound |
| CN108192138A (en) * | 2016-12-08 | 2018-06-22 | 中国石油天然气股份有限公司 | Modification method of carbon nano tube used as rubber filler |
| CN114921202A (en) * | 2022-04-28 | 2022-08-19 | 深圳市通泰盈科技股份有限公司 | High-temperature-resistant acrylic pressure-sensitive adhesive, preparation method thereof, pressure-sensitive adhesive tape and preparation method thereof |
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