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 PDF

Info

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Withdrawn
Application number
CN202310298365.6A
Other languages
Chinese (zh)
Inventor
金闯
裴家发
包静炎
张熠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Taicang Sidike New Material Science and Technology Co Ltd
Jiangsu Sidike New Materials Science and Technology Co Ltd
Original Assignee
Taicang Sidike New Material Science and Technology Co Ltd
Jiangsu Sidike New Materials Science and Technology Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Taicang Sidike New Material Science and Technology Co Ltd, Jiangsu Sidike New Materials Science and Technology Co Ltd filed Critical Taicang Sidike New Material Science and Technology Co Ltd
Priority to CN202310298365.6A priority Critical patent/CN116285867A/en
Publication of CN116285867A publication Critical patent/CN116285867A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02Electrically-conducting adhesives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy 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

Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof
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.
CN202310298365.6A 2023-03-24 2023-03-24 Silica gel pressure-sensitive adhesive with high-temperature resistance conductivity and preparation method thereof Withdrawn CN116285867A (en)

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)

* Cited by examiner, † Cited by third party
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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