CN110951443B - Single-component organic silica gel for bonding multiple materials and preparation method thereof - Google Patents
Single-component organic silica gel for bonding multiple materials and preparation method thereof Download PDFInfo
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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
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a single-component organic silica gel for bonding multiple materials and a preparation method thereof, wherein the silica gel is a single-component gel, and methyl vinyl MQ resin, methyl silicone oil, hydrogen-containing silicone oil, a silane coupling agent 1, a silane coupling agent 2, a silane coupling agent 3, a base gel, a Pt catalyst and an inhibitor are mixed according to the weight ratio of 20-35: 40-50: 3-7: 1-5: 1-5: 1-5: 7-24: 0.02-0.1: 0.02-0.1 by weight. The filler treatment process adopted by the invention can greatly improve the compatibility of the inorganic filler and the organic silicon resin, and the compound use of a plurality of coupling agents improves the application range of the silica gel adhesive material. The synthesis of the high molecular weight coupling agent effectively reduces the volatile component of the glue, and the preparation method is simple and easy for industrial production.
Description
Technical Field
The invention relates to a single-component organic silica gel for bonding multiple materials and a preparation method thereof, belonging to the field of organic silicon resin modification.
Technical Field
The sealant is an adhesive used for filling the gap to play a role of sealing. Has the functions of leakage prevention, water prevention, vibration prevention, sound insulation, heat insulation and the like. With the development of technology, more and more connecting assemblies are fixed by sealant instead of traditional sealing rings and screws, so that the sealant is widely applied to the fields of buildings, transportation, electronic instruments and meters and the like.
Most of the common organosilicon sealants in the market can be bonded by single materials, and different sealants are required to be selected when different materials are bonded, so that the frequent glue replacement is required in the using process, and the improper selection is easy to occur.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and discloses a single-component organic silica gel for bonding multiple materials and a preparation method thereof. The synthesis of the high molecular weight coupling agent effectively reduces the volatile component of the glue. The preparation method is simple and easy for industrial production.
The invention relates to a single-component organic silica gel for bonding multiple materials, which is a single-component gel, wherein the ratio of methyl vinyl MQ resin, methyl silicone oil, hydrogen-containing silicone oil, silane coupling agent 1, silane coupling agent 2, silane coupling agent 3, base gel, Pt catalyst and inhibitor is (20-35: 40-50): 3-7: 1-5: 1-5: 1-5: 7-24: 0.02-0.1: 0.02-0.1 weight ratio.
The silane coupling agents 1, 2 and 3 are characterized in that the preparation method of the silane coupling agent is as follows: adding hydrogen-containing silicone oil 2 and gamma-methacryloxypropyltrimethoxysilane (or methyl methacrylate and styrene ethyltrimethoxysilane) into a three-neck flask according to the molar ratio of 1-2: 1-2, adding toluene with the same mass as a reaction system, stirring for 5-10 min, then adding 10-20 ppm of Pt catalyst into the reaction system, stirring for 2-4 h at 80-100 ℃, and finally keeping the vacuum condition of the vacuum degree of less than 0.085Mpa to remove low-molecular substances. Silane coupling agents 1, 2 and 3 are obtained, and the reaction formula is as follows:
the technical scheme adopted by the invention is as follows:
(1) the hydrogen-containing silicone oil is hydrogen-containing terminated polymethylsiloxane with the molecular formula of (HMe)2SiO0.5)2(Me2SiO0.5)nN is 2-8, the active hydrogen content is 0.30-1%, and the viscosity is 18-50 mPa.S;
(2) the methyl vinyl MQ resin has the M/Q of 1.0-1.2, the vinyl content of 0.5-2%, the viscosity of 7500-20000 mPa.S at 25 ℃;
(3) the methyl silicone oil is straight-chain polydimethylsiloxane with the molecular formula of (Me)3SiO0.5)2(Me2SiO0.5)nN is 20 to 35, and the viscosity is 30 to 100 mPa.S;
(4) the hydrogen-containing silicone oil 2 is dimethyl-terminated polymethylhydrosiloxane and has a molecular formula of (Me)3SiO0.5)2(HMe2SiO0.5)n(Me2SiO0.5)mN is 4-8, m is 4-8, the active hydrogen content is 0.20% -1%, the viscosity is 10-60 mPa.S at 25 ℃;
(5) the micro silicon powder is powder with the fineness of 850-1250 meshes;
(6) the catalyst is vinyl siloxane complex of chloroplatinic acid, and the platinum content is 2000-6000 ppm;
(7) the white carbon black has a specific surface area of 160-200m2Hydrophobic white carbon black in a per gram ratio;
(8) the inhibitor is one of 1-acetylene and-1-cyclohexanol, 2-methyl-3-butynyl-2-alcohol and 3, 5-dimethyl-1-hexynyl-3-alcohol;
the preparation method of the silane coupling agents 1, 2 and 3 comprises the following steps:
adding hydrogen-containing silicone oil 2 and gamma-methacryloxypropyltrimethoxysilane (or methyl methacrylate and styrene ethyltrimethoxysilane) into a three-neck flask according to the molar ratio of 1-2: 1-2, adding toluene with the same mass as a reaction system, stirring for 5-10 min, then adding 10-20 ppm of Pt catalyst into the reaction system, stirring for 2-4 h at 80-100 ℃, and finally keeping the vacuum condition of the vacuum degree of less than 0.085Mpa to remove low-molecular substances.
In the step, mechanical stirring is adopted for stirring, and the rotating speed is 120-180 revolutions per minute.
The preparation method of the base material comprises the following steps: adding methyl silicone oil, white carbon black, silicon micropowder and a coupling agent 3 into a kneading machine according to the mass ratio of 1:1:1.5:0.1, kneading for 10-15 min, adding an acetic acid aqueous solution with the concentration of 0.05-0.1 and the molar mass of the coupling agent 3 being 4-8 times, kneading for 2-3 hours at 80-100 ℃, heating to 130-150 ℃, and finally kneading for 1-2 hours under the condition that the vacuum degree is less than 0.085Mpa to obtain the base rubber. In the step, mechanical stirring is adopted for stirring, and the rotating speed is 30-50 revolutions per minute.
The filler treatment process adopted by the invention can greatly improve the compatibility of the inorganic filler and the organic silicon resin, and the application range of the silica gel adhesive material is widened due to the compound use of a plurality of coupling agents. The synthesis of the high molecular weight coupling agent effectively reduces the volatile component of the glue, and the preparation method is simple and easy for industrial production.
Detailed Description
Adding hydrogen-containing silicone oil 2(n is 4, m is 4 viscosity is 18 mPa.s) and gamma-methacryloxypropyltrimethoxysilane (or methyl methacrylate and styrene ethyl trimethoxysilane) into a three-neck flask according to a molar ratio of 1:4, adding toluene with the same mass as a reaction system, stirring for 10min, then adding 15ppm of Pt catalyst into the reaction system, then stirring for 3 hours at 100 ℃, and finally keeping vacuum degree to be less than 0.085Mpa to remove low molecular substances.
Preparing base glue: adding 200g of methyl silicone oil, 200g of white carbon black, 300g of silicon micropowder and 20g of coupling agent into a kneader, kneading for 15min, adding 3.7g of 0.06% acetic acid aqueous solution, kneading for 2.5 hours at 80 ℃, heating to 150 ℃, and finally kneading for 1.5 hours under the condition that the vacuum degree is less than 0.085Mpa to obtain the base rubber.
Example 1
15g of methyl vinyl MQ resin (with the vinyl content of 0.8 percent and the viscosity of 1000 mPas), 40g of methyl silicone oil (with the viscosity of 85 mPas), 1.24g of hydrogen-containing silicone oil (with the viscosity of 20 mPas), 13.6 g of silane coupling agent, 14g of base rubber, 0.02g of catalyst with the platinum content of 2500ppm and 0.02g of 2-methyl-3-butynyl-2-ol are stirred in vacuum and defoamed in sequence, and then cured for 2h at 150 ℃.
Example 2
15g of methyl vinyl MQ resin (with the vinyl content of 0.8 percent and the viscosity of 1000 mPas), 40g of methyl silicone oil (with the viscosity of 85 mPas), 1.24g of hydrogen-containing silicone oil (with the viscosity of 20 mPas), 23.6 g of silane coupling agent, 14g of base rubber, 0.02g of catalyst with the platinum content of 2500ppm and 0.02g of 2-methyl-3-butynyl-2-ol are stirred in vacuum and defoamed in sequence, and then cured for 2h at 150 ℃.
Example 3
15g of methyl vinyl MQ resin (with the vinyl content of 0.8 percent and the viscosity of 1000 mPas), 40g of methyl silicone oil (with the viscosity of 85 mPas), 1.24g of hydrogen-containing silicone oil (with the viscosity of 20 mPas), 33.6 g of silane coupling agent, 14g of base rubber, 0.02g of catalyst with the platinum content of 2500ppm and 0.02g of 2-methyl-3-butynyl-2-ol are stirred in vacuum and defoamed in sequence, and then cured for 2h at 150 ℃.
Example 4:
15g of methyl vinyl MQ resin (with the vinyl content of 0.8 percent and the viscosity of 1000 mPas), 40g of methyl silicone oil (with the viscosity of 85 mPas), 1.24g of hydrogen-containing silicone oil (with the viscosity of 20 mPas), 11.2 g of silane coupling agent, 21.2 g of silane coupling agent, 31.2 g of silane coupling agent, 14g of base rubber, 0.02g of catalyst with the platinum content of 2500ppm and 0.02g of 2-methyl-3-butynyl-2-alcohol are stirred and defoamed in vacuum, and then cured for 2h at 150 ℃.
Comparative example 1
15g of methyl vinyl MQ resin (with the vinyl content of 0.8 percent and the viscosity of 1000 mPas), 40g of methyl silicone oil (with the viscosity of 85 mPas), 1.24g of hydrogen-containing silicone oil (with the viscosity of 20 mPas), 3.9g of silica micropowder, 3.9g of white carbon black, 0.02g of catalyst with the platinum content of 2500ppm and 0.02g of 2-methyl-3-butynyl-2-ol are stirred in vacuum and defoamed in sequence, and then cured for 2h at 150 ℃.
Table 1: results of Performance testing
| Performance of | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 |
| hardness/Shore A | 42 | 43 | 43 | 44 | 44 |
| Bonding to aluminum | ● | Δ | ● | ● | Δ |
| Bonding to copper | ● | Δ | ● | ● | Δ |
| Bonding to steel | ● | ● | ● | ● | Δ |
| Bonding to glass | ● | Δ | Δ | ● | Δ |
| To PCT bonding | Δ | ● | ● | ● | Δ |
| To PBT | Δ | ● | Δ | ● | Δ |
| Bonding to PPA | Δ | Δ | ● | ● | Δ |
| Bubble condition after curing | Bubble-free | Bubble-free | Bubble-free | Bubble-free | With air bubbles |
Remarking: ● bulk separation delta interfacial separation.
The separation of the body is considered to be a good bond to the material. As can be seen from the experimental results, it is difficult to achieve adhesion to a variety of materials using a single coupling agent. The problem is solved by compounding a plurality of coupling agents. Meanwhile, the pretreatment of the coupling agent 3 on the filler improves the compatibility of the organic material and the inorganic material and avoids the generation of bubbles in the heating and curing process. The formulation of example 4 therefore works best.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, which is intended to cover all modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (1)
1. A single-component organic silica gel for bonding multiple materials is characterized in that methyl vinyl MQ resin, methyl silicone oil, hydrogen-containing silicone oil, a silane coupling agent 1, a silane coupling agent 2, a silane coupling agent 3, a base adhesive, a Pt catalyst and an inhibitor are mixed according to the weight ratio of 20-35: 40-50: 3-7: 1-5: 7-24: 0.02-0.1;
the silane coupling agent 1 has the structure
the silane coupling agent 2 has the structure
the silane coupling agent 3 has the structure
the preparation method of the silane coupling agent 1 comprises the following steps: adding hydrogen-containing silicone oil 2 and gamma-methacryloxypropyltrimethoxysilane into a three-neck flask according to the molar ratio of 1-2: 1-2, adding toluene with the same mass as that of a reaction system, stirring for 5-10 min, then adding a Pt catalyst with 10-20 ppm of the reaction system, stirring for 2-4 h at 80-100 ℃, and finally removing low molecular substances under the vacuum condition that the vacuum degree is less than 0.085Mpa to obtain a silane coupling agent 1;
the preparation method of the silane coupling agent 3 comprises the following steps: adding hydrogen-containing silicone oil 2 and styrene ethyl trimethoxy silane into a three-neck flask according to a molar ratio of 1-2: 1-2, adding toluene with the same mass as that of a reaction system, stirring for 5-10 min, then adding a Pt catalyst with 10-20 ppm as the reaction system, stirring for 2-4 h at 80-100 ℃, and finally removing low molecular substances under a vacuum condition with the vacuum degree of less than 0.085Mpa to obtain a silane coupling agent 3;
the hydrogen-containing silicone oil 2 is dimethyl-terminated polymethylhydrosiloxane and has a molecular formula of (Me)3SiO0.5)2(HMe2SiO)n(Me2SiO)mN is 4-8, m is 4-8, the active hydrogen content is 0.20-1%, and the viscosity at 25 ℃ is 10-60 mPa & S;
the preparation method of the base material comprises the following steps: adding methyl silicone oil, white carbon black, silicon micropowder and a coupling agent 3 into a kneading machine according to the mass ratio of 1:1:1.5:0.1, kneading for 10-15 min, adding an acetic acid aqueous solution with the concentration of 0.05-0.1 and the molar mass of 4-8 times that of the silane coupling agent 3, kneading for 2-3 hours at 80-100 ℃, heating to 130-150 ℃, and finally kneading for 1-2 hours under the condition that the vacuum degree is less than 0.085Mpa to obtain a base rubber;
the molecular formula of the hydrogen-containing silicone oil is (HMe)2SiO0.5)2(Me2SiO)nN is 2-8, the active hydrogen content is 0.30-1%, and the viscosity is 18-50 mPa.S; the methyl vinyl MQ resin has the M/Q of 1.0-1.2, the vinyl content of 0.5-2% and the viscosity of 7500-20000 mPa.S at 25 ℃; the methyl silicone oil is straight-chain polydimethylsiloxane with the molecular formula of (Me)3SiO0.5)2(Me2SiO)nN is 20 to 35, and the viscosity is 30 to 100mPa · S;
the catalyst is vinyl siloxane complex of chloroplatinic acid, and the platinum content is 2000-6000 ppm; the inhibitor is one of 1-ethynyl-1-cyclohexanol, 2-methyl-3-butynyl-2-alcohol and 3, 5-dimethyl-1-hexynyl-3-alcohol;
the micro silicon powder is powder with the fineness of 850-1250 meshes; the white carbon black has a specific surface area of 160-200m2The hydrophobic white carbon black is/g.
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| CN111875970B (en) * | 2020-08-14 | 2022-08-19 | 烟台德邦科技股份有限公司 | Oil-resistant, high-temperature-resistant and low-volatile organic silica gel |
| CN114656792A (en) * | 2022-02-21 | 2022-06-24 | 青岛卓尤新材料有限公司 | Single-component heat-conducting silica gel capable of being transported at normal temperature and reworked and preparation method thereof |
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| JP2003128924A (en) * | 2001-10-26 | 2003-05-08 | Ge Toshiba Silicones Co Ltd | Room temperature curable polyorganosiloxane composition |
| CN103788916A (en) * | 2014-02-11 | 2014-05-14 | 绵阳惠利电子材料有限公司 | Organic silicon sealant with fast-curing property and high heat and humidity resistance and preparation method thereof |
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| CN105754543A (en) * | 2016-04-06 | 2016-07-13 | 深圳市欧普特工业材料有限公司 | Organic silicon pouring sealant containing functional group MQ resin for LED and preparation method of organic silicon pouring sealant |
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2019
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| JPH10168419A (en) * | 1996-12-13 | 1998-06-23 | Asahi Glass Co Ltd | Adhesive composition |
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