CN110982074A - Normal-temperature curing tackifier system, preparation method and pouring sealant using same - Google Patents
Normal-temperature curing tackifier system, preparation method and pouring sealant using same Download PDFInfo
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- 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
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- 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
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- 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
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Abstract
The invention relates to the field of silicone rubber bonding sealing materials, in particular to a normal-temperature curing tackifier system, a preparation method and a pouring sealant using the same. A preparation method of a normal-temperature curing tackifier system comprises the following steps: (1) at room temperature, mixing and stirring 6-60 parts of epoxy hydrocarbon silane coupling agent, 6-60 parts of ethyl orthosilicate, 0.2-2 parts of titanate and 6-60 parts of trimethylolpropane diallyl ester uniformly according to the parts by mass of the raw materials; (2) heating to 75-85 ℃ while stirring and mixing, reacting for 2-3 h, and then decompressing and vacuumizing to remove low-boiling-point substances for 0.5-2 h under the conditions that the temperature and the vacuum degree are-0.09 to-0.1 MPa to obtain the light yellow transparent liquid tackifier with the volatile content of less than 2%. The invention aims to provide a normal-temperature curing tackifier system, a preparation method and a pouring sealant using the same.
Description
Technical Field
The invention relates to the field of silicone rubber bonding sealing materials, in particular to a normal-temperature curing tackifier system, a preparation method and a pouring sealant using the same.
Background
The addition type silicone rubber limits the use of a plurality of coupling agents in the addition type silicone rubber because the catalyst is mainly a platinum catalyst, and because the platinum catalyst can generate a poisoning phenomenon in an organic matter containing elements such as N, P, S and the like and an ionic compound containing heavy metals such as Sn, Ph, Hg, Bi and the like to block vulcanization, most of the bonding coupling agents cannot be directly used, and a vulcanization network is realized only by virtue of hydrosilylation of vinyl silicone oil and hydrogen-containing silicone oil under the action of the platinum catalyst, so that the surface acting force of most of silicone rubber products and other base materials is weak, no bonding is caused, and the application of the addition type silicone rubber in more fields is limited. Therefore, the primer is generally required to be used for improving the adhesion performance of the addition type silicone rubber and the surface of the base material, but on one hand, the primer used contains a large amount of organic solvent, has relatively high toxicity and is easy to pollute the environment, and on the other hand, the use of the primer increases the processing procedures and affects the production efficiency.
In addition, most of the existing addition type silicone rubber tackifiers have adhesiveness only under the condition of high temperature or heating, and a small part of tackifiers have a general adhesive effect which can play a role in adhesion at normal temperature, for example, boron-containing tackifiers can only play a role in adhesion of most of metals and a small number of plastics, such as aluminum sheets, copper sheets, stainless steel, PCB (printed circuit board) boards, PBT (polybutylene terephthalate) and the like, and cannot form effective adhesive force on difficult-to-adhere materials, such as PC (polycarbonate), PS (polystyrene), PMMA (polymethyl methacrylate), ABS (acrylonitrile butadiene styrene) and the like. Therefore, there is a need to develop an adhesion promoter system that can be cured at room temperature and an addition-type heat-conducting potting adhesive that can bond well to most substrates.
Disclosure of Invention
Aiming at the problems brought forward by the background technology, the invention aims to provide a normal-temperature curing tackifier system which can be reacted and cured at normal temperature and normal pressure, has strong operability, excellent cohesive force and strong adhesive force, has good cohesive property on most base materials such as metal, plastic and the like, and solves the problems that the existing tackifier has poor cohesive force and can only perform the cohesive action on most metal and a few plastics.
The invention also aims to provide a preparation method of the normal-temperature curing tackifier system, the normal-temperature curing tackifier system prepared by the method has strong wettability to organic materials and compatibility with the surfaces of organic polymers and inorganic materials, forms stable covalent bonds in the using process, and has good cohesiveness to most of base materials such as metal, plastic and the like.
The invention also aims to provide the pouring sealant using the normal-temperature curing tackifier system, which has excellent fluidity and heat conductivity, can be cured at room temperature, is simple to operate, can have excellent adhesion to most of metal and plastic substrates without using a primer, and has a wide application range.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a normal-temperature curing tackifier system comprises the following steps:
(1) at room temperature, mixing and stirring 6-60 parts of epoxy hydrocarbon silane coupling agent, 6-60 parts of ethyl orthosilicate, 0.2-2 parts of titanate and 6-60 parts of trimethylolpropane diallyl ester uniformly according to the parts by mass of the raw materials;
(2) heating to 75-85 ℃ while stirring and mixing, reacting for 2-3 h, and then decompressing and vacuumizing to remove low-boiling-point substances for 0.5-2 h under the conditions that the temperature and the vacuum degree are-0.09 to-0.1 MPa to obtain a light yellow transparent liquid tackifier with the volatile content of less than 2%;
(3) after the light yellow transparent liquid tackifier is cooled to room temperature, the light yellow transparent liquid tackifier, the boron-containing tackifier and the aluminum-acetylacetone are mixed according to the mass ratio of 48.7: 50: 1.3, uniformly mixing and stirring to obtain the normal-temperature curing tackifier system.
Preferably, the titanate is butyl titanate, and the epoxy alkyl silane coupling agent is one of 3-glycidoxypropylalkoxysilane or 2- (3, 4-epoxycyclohexyl) ethylalkoxysilane.
Preferably, the boron-containing tackifier is one of boric acid, a reactant of boric acid and a multifunctional silane, or a reactant of boric acid and a carbon-functional siloxane.
The normal-temperature curing tackifier system is prepared by using the preparation method of the normal-temperature curing tackifier system.
A pouring sealant using the normal-temperature curing tackifier system comprises a component A consisting of vinyl silicone oil, filler, fumed silica, the normal-temperature curing tackifier system and a catalyst, and a component B consisting of the vinyl silicone oil, the filler, the fumed silica, hydrogen-containing silicone oil and an inhibitor;
the formula of the component A comprises the following components in parts by mass:
the formula of the component B comprises the following components in parts by mass:
preferably, the viscosity of the vinyl silicone oil at the temperature of 25 ℃ is 100 to 500mPa · s, and the vinyl content of the vinyl silicone oil is 0.1 to 1.0 percent.
Preferably, the filler is one or two of quartz powder and alumina which are compounded according to any proportion, the particle size of the quartz powder is 3-10 μm, and the particle size of the alumina is 3-10 μm.
Preferably, the hydrogen-containing silicone oil has a hydrogen content of 0.4-0.75% and a viscosity of 50-500 mPas at 25 ℃.
Preferably, the catalyst is one of chloroplatinic acid or a complex thereof, the platinum content of the catalyst is 1000ppm to 5000ppm, and the fumed silica is hydrophilic fumed silica.
Preferably, the inhibitor is a mixture of acetylene cyclohexanol and vinyl silicone oil, the acetylene cyclohexanol accounts for 0.5-1.5% of the inhibitor by mass, and the viscosity of the vinyl silicone oil in the inhibitor at the temperature of 25 ℃ is 150-500 mPa & s.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, an epoxy alkyl silane coupling agent is used as a coupling agent, titanate is used as a catalyst, and reacts with ethyl orthosilicate and trimethylolpropane diallyl ester to prepare a light yellow transparent liquid tackifier, then the adhesion force of a tackifier system in use is improved through the synergistic effect of aluminum-acetylacetone and the light yellow transparent liquid tackifier, and a room temperature curing tackifier system obtained by matching the light yellow transparent liquid tackifier, a boron-containing tackifier and aluminum-acetylacetone can participate in the reaction at normal temperature and normal pressure without activation at specific high temperature, so that the preparation method is convenient to operate, strong in operability and excellent in adhesion force. The adhesion promoter system greatly improves the wettability of the adhesion promoter system on organic materials and the compatibility with the surfaces of organic polymers and inorganic materials through the mutual synergistic effect of reactants, so that stable covalent bonds are formed in the using process, and the obtained normal-temperature cured adhesion promoter system has good adhesion to most base materials such as metal, plastic and the like.
The addition type heat conduction pouring sealant prepared by using the normal temperature curing tackifier system can have excellent adhesion to most metal and plastic substrates without using a primer. The aluminum oxide is added as a heat-conducting filler to improve the heat-conducting property of the pouring sealant, the fluidity of the pouring sealant is ensured by controlling the viscosity of the vinyl silicone oil and the hydrogen-containing silicone oil, the pouring sealant has excellent fluidity and heat-conducting property, and can be used by mixing the component A and the component B and then curing at room temperature.
Detailed Description
A preparation method of a normal-temperature curing tackifier system comprises the following steps:
(1) at room temperature, mixing and stirring 6-60 parts of epoxy hydrocarbon silane coupling agent, 6-60 parts of ethyl orthosilicate, 0.2-2 parts of titanate and 6-60 parts of trimethylolpropane diallyl ester uniformly according to the parts by mass of the raw materials;
(2) heating to 75-85 ℃ while stirring and mixing, reacting for 2-3 h, and then decompressing and vacuumizing to remove low-boiling-point substances for 0.5-2 h under the conditions that the temperature and the vacuum degree are-0.09 to-0.1 MPa to obtain a light yellow transparent liquid tackifier with the volatile content of less than 2%;
(3) after the light yellow transparent liquid tackifier is cooled to room temperature, the light yellow transparent liquid tackifier, the boron-containing tackifier and the aluminum-acetylacetone are mixed according to the mass ratio of 48.7: 50: 1.3, uniformly mixing and stirring to obtain the normal-temperature curing tackifier system.
The normal temperature curing tackifier system of the invention uses epoxy alkyl silane coupling agent as coupling agent, titanate as catalyst, and reacts with ethyl orthosilicate and trimethylolpropane diallyl ester to prepare a light yellow transparent liquid tackifier, then the adhesion force of the tackifier system in use is improved through the synergistic effect of aluminum-acetylacetone and the light yellow transparent liquid tackifier, boron-containing tackifier and aluminum-acetylacetone are matched at the same time, the mass ratio of the light yellow transparent liquid tackifier to the boron-containing tackifier is 48.7: 50: the normal-temperature curing tackifier system obtained by matching the proportion of 1.3 can participate in the reaction at normal temperature and normal pressure, can play a reaction role without being activated at specific high temperature, is convenient and has strong operability and excellent cohesive force. The adhesion promoter system greatly improves the wettability of the adhesion promoter system on organic materials and the compatibility with the surfaces of organic polymers and inorganic materials through the mutual synergistic effect of reactants, so that stable covalent bonds are formed in the using process, and the obtained normal-temperature cured adhesion promoter system has good adhesion to most base materials such as metal, plastic and the like.
Preferably, the titanate is butyl titanate, and the epoxy alkyl silane coupling agent is one of 3-glycidoxypropylalkoxysilane or 2- (3, 4-epoxycyclohexyl) ethylalkoxysilane.
Titanate is added as a catalyst, so that the room temperature curing performance of the tackifier system can be improved, the bonding strength of the tackifier system at room temperature is improved, and the room temperature curing speed is improved; the epoxy hydrocarbon silane coupling agent is used, and the activity of epoxy hydroxyl is utilized, so that the epoxy hydrocarbon silane coupling agent can be complexed with the surfaces of an alloy base material and a plastic base material, the interface action between a tackifier system and the base material is improved, the binding force between the base material and the tackifier system is improved, and the adhesion property and the weather resistance of the tackifier system are improved.
Preferably, the boron-containing tackifier is one of boric acid, a reactant of boric acid and a multifunctional silane, or a reactant of boric acid and a carbon-functional siloxane.
Because the boron-containing tackifier only can bond most of metals and a few of plastics, the invention combines the boron-containing tackifier and the prepared faint yellow transparent liquid tackifier according to the mass proportion, so that the prepared normal-temperature curing tackifier system can form effective covalent bonds for most of materials to form the binding power.
The normal-temperature curing tackifier system is prepared by using the preparation method of the normal-temperature curing tackifier system.
The normal-temperature curing tackifier system prepared by the preparation method of the normal-temperature curing tackifier system has the characteristics of reaction curing at normal temperature and normal pressure, strong operability, excellent adhesive force, strong adhesive force and good adhesive property on most base materials such as metal, plastic and the like.
A pouring sealant using the normal-temperature curing tackifier system comprises a component A consisting of vinyl silicone oil, filler, fumed silica, the normal-temperature curing tackifier system and a catalyst, and a component B consisting of the vinyl silicone oil, the filler, the fumed silica, hydrogen-containing silicone oil and an inhibitor;
the formula of the component A comprises the following components in parts by mass:
the formula of the component B comprises the following components in parts by mass:
the pouring sealant using the normal-temperature curing tackifier system can have excellent adhesion to most of metal and plastic substrates without using a primer. The aluminum oxide is added as a heat-conducting filler to improve the heat-conducting property of the pouring sealant, the fluidity of the pouring sealant is ensured by controlling the viscosity of the vinyl silicone oil and the hydrogen-containing silicone oil, the pouring sealant has excellent fluidity and heat-conducting property, and can be used by mixing the component A and the component B and then curing at room temperature.
Preferably, the viscosity of the vinyl silicone oil at the temperature of 25 ℃ is 100 to 500mPa · s, and the vinyl content of the vinyl silicone oil is 0.1 to 1.0 percent.
The viscosity of the vinyl silicone oil and the vinyl content of the vinyl silicone oil are limited, the prepared pouring sealant has the characteristics of low viscosity, good fluidity and moderate hardness, and in addition, the low-viscosity vinyl silicone oil can effectively improve the filling amount of the filler, so that the filling sealant has high heat conductivity and excellent flow property. If the viscosity of the vinyl silicone oil is too high and the vinyl content of the vinyl silicone oil is too high, the prepared pouring sealant is easy to have poor fluidity and high hardness, and the glue surface is easy to crack during curing and use, so that the service performance of the pouring sealant is seriously influenced.
Preferably, the filler is one or two of quartz powder and alumina which are compounded according to any proportion, the particle size of the quartz powder is 3-10 μm, and the particle size of the alumina is 3-10 μm.
The aluminum oxide can improve the heat-conducting property of the pouring sealant as a heat-conducting filler, the quartz powder can improve the fluidity of the pouring sealant as a filler, the cost is reduced, the aluminum oxide and the particle size range of the quartz powder are limited, the prepared pouring sealant has good fluidity, and has higher heat conductivity coefficient, so that lower specific gravity and reduced cost are achieved, if the aluminum oxide and the particle size of the quartz powder are too small, the effect of improving the heat-conducting property and the fluidity of the pouring sealant cannot be achieved, and if the particle size of the aluminum oxide and the particle size of the quartz powder is too large, the raw material components are easily mixed unevenly, so that the service performance of the pouring sealant is influenced.
Preferably, the hydrogen-containing silicone oil has a hydrogen content of 0.4-0.75% and a viscosity of 50-500 mPas at 25 ℃.
The hydrogen content and the viscosity of the hydrogen-containing silicone oil are limited, so that the cross-linking density of the pouring sealant is moderate during curing, the fluidity of the pouring sealant under the limited viscosity is good, if the hydrogen content is too high, the hardness of the pouring sealant is increased along with the increase of the cross-linking density, and the permeability of the glue solution is poor during use, so that the bonding performance of the glue solution after curing is reduced.
Preferably, the catalyst is one of chloroplatinic acid or a complex thereof, the platinum content of the catalyst is 1000ppm to 5000ppm, and the fumed silica is hydrophilic fumed silica.
The catalyst used in the invention is chloroplatinic acid or a complex thereof, the platinum content is limited to 1000 ppm-5000 ppm, if the platinum content is too low, the catalytic activity is insufficient, the catalytic reaction efficiency is low, and the curing reaction speed is reduced, if the platinum content is too high, the catalytic reaction efficiency is too high, the curing speed is too high, and the glue solution is cured without spreading on the surface of the substrate, so that the bonding effect cannot be achieved.
Preferably, the inhibitor is a mixture of acetylene cyclohexanol and vinyl silicone oil, the acetylene cyclohexanol accounts for 0.5-1.5% of the inhibitor by mass, and the viscosity of the vinyl silicone oil in the inhibitor at the temperature of 25 ℃ is 150-500 mPa & s.
Limiting the mass percentage of the ethyne cyclohexanol in the inhibitor, coordinating the ethynyl and the metal platinum, controlling the reaction activity of the pouring sealant at room temperature, and ensuring that the pouring sealant has enough pot life and operable time when in use; the viscosity of the vinyl silicone oil in the inhibitor is limited to 150-500 mPa & s, the vinyl silicone oil plays a role in diluting in the inhibitor, and the moderate viscosity of the silicone oil can ensure that the pouring sealant has good fluidity. The inhibitor used in the invention can delay the crosslinking curing speed of the pouring sealant, is convenient for construction operation, is diluted by vinyl silicone oil, is convenient for measuring and operation, reduces the volatilization probability of acetylene cyclohexanol, and improves the storage period of the inhibitor.
Preferably, the preparation method of the pouring sealant comprises the following steps:
a. preparation of component A: at normal temperature, 50-500 parts of vinyl silicone oil, 50-300 parts of filler, 2-10 parts of fumed silica, 2-20 parts of tackifier system and 0.5-2 parts of catalyst are taken and placed in a high-speed shearing dispersion machine to be uniformly dispersed for 40-90 min at room temperature, so as to prepare a component A;
b. preparation of the component B: at normal temperature, taking 50-200 parts of vinyl silicone oil, 50-300 parts of filler, 2-10 parts of fumed silica, 10-50 parts of hydrogen-containing silicone oil and 0.01-0.1 part of inhibitor, and placing the mixture in a high-speed shearing dispersion machine to disperse uniformly for 40-90 min at room temperature to prepare a component B;
c. preparing a pouring sealant: at normal temperature, mixing the component A and the component B according to a mass ratio of 1: 1, placing the mixture in a vacuum device, vacuumizing at normal temperature, keeping the vacuum degree at-0.09 MPa for 10-30 min, and removing bubbles to obtain the addition type heat-conducting pouring sealant with good bonding property.
The addition type heat conduction pouring sealant prepared by the invention has excellent fluidity and heat conduction performance, can be cured at room temperature, is simple to operate, can have excellent adhesive property to most metal and plastic substrates without using a primer, has good adhesive property to aluminum materials, copper sheets, glass, stainless steel, PCB boards, PBT, PC, PS, PMMA, ABS and other substrates after curing, and has wide application range.
The technical solution of the present invention is further explained by the following embodiments.
And (3) performance testing:
(1) and (3) viscosity measurement: performing viscosity measurement according to GB/T2794-2013 'Single-cylinder rotational viscometer method for measuring viscosity of adhesives';
(2) and (3) density measurement: density measurement is carried out according to GB/T533-;
(3) and (3) measuring the heat conductivity coefficient: measuring the heat conductivity coefficient according to ASTM D5470-2006 test method for thermal transmission performance standard of heat-conducting electric insulation material;
(4) and (3) measuring the adhesion: selecting a base material with the thickness of 50mm multiplied by 3mm as a bonding sample, and cleaning the surface of the base material by using acetone before coating silicon rubber; coating an additional heat-conducting pouring sealant on the bonding surface of the base material; then the bonding surfaces of the two base materials are folded and lightly pressurized; the molded product was allowed to stand still and cured at room temperature for 24 hours, and the addition type heat conductive potting adhesive layer was peeled off manually from the integrated product, and adhesiveness was evaluated based on cohesive failure.
Preparation of a normal-temperature curing tackifier system:
(1) at room temperature, 60 parts of epoxy hydrocarbon silane coupling agent, 60 parts of ethyl orthosilicate, 1 part of titanate and 60 parts of trimethylolpropane diallyl ester are mixed and stirred uniformly;
(2) heating to 80 ℃ while stirring and mixing, reacting for 3h, and then decompressing and vacuumizing to remove low-boiling-point substances for 1h under the conditions of 80 ℃ and vacuum degree of-0.09 MPa to obtain the light yellow transparent liquid tackifier with the volatile content of less than 2%.
(3) And after the faint yellow transparent liquid tackifier is cooled to room temperature, mixing and stirring uniformly 48.7 parts of faint yellow transparent liquid tackifier, 50 parts of boron-containing tackifier with the model of Jiangxianna new material Z-15 series and 1.3 parts of aluminum-acetylacetone to obtain a normal-temperature curing tackifier system.
Example 1
(1) At normal temperature, 300 parts of vinyl silicone oil with the vinyl content of 0.57 percent and the viscosity of 300 mPas, 100 parts of quartz powder with the particle size of 3-10 mu m, 100 parts of alumina with the particle size of 3-10 mu m, 3 parts of hydrophilic fumed silica with the type of Kabot 150, 0.6 part of chloroplatinic acid and 3 parts of normal-temperature curing tackifier system are taken and placed in a high-speed shearing disperser to be uniformly dispersed for 60min at room temperature, and the component A is prepared.
(2) At normal temperature, 300 parts of vinyl silicone oil with the vinyl content of 0.57 percent and the viscosity of 300 mPas, 100 parts of quartz powder with the particle size of 3 to 10 mu m, 100 parts of alumina with the particle size of 3 to 10 mu m, 16 parts of hydrogen silicone oil with the hydrogen content of 0.5 percent and the viscosity of 50 mPas, 3 parts of hydrophilic fumed silica with the type of Cabot 150 and 0.04 part of inhibitor with the mass percent of ethynl cyclohexanol of 0.5 percent are taken and placed in a high-speed shearing disperser to be uniformly dispersed for 60min at room temperature, thus obtaining the component B.
(3) At normal temperature, 50 parts of the prepared component A and 50 parts of the prepared component B are uniformly mixed and stirred, and then the mixture is placed in a vacuum machine to be vacuumized at normal temperature, the vacuum degree is-0.09 MPa, and the mixture is kept for 30min to be subjected to bubble removal treatment, so that the addition type heat conduction pouring sealant with good bonding is prepared.
Example 2
(1) At normal temperature, 100 parts of vinyl silicone oil with the vinyl content of 0.32 percent and the viscosity of 1000 mPas, 75 parts of quartz powder with the particle size of 5-10 mu m, 4 parts of hydrophilic fumed silica with the type of Kabot 150, 0.5 part of chloroplatinic acid and 5 parts of normal-temperature curing tackifier system are taken and placed in a high-speed shearing dispersion machine to be uniformly dispersed for 60min at room temperature, and the component A is prepared.
(2) At normal temperature, 100 parts of vinyl silicone oil with the vinyl content of 0.43 percent and the viscosity of 500 mPas, 75 parts of quartz powder with the particle size of 3-10 μm, 10 parts of hydrogen-containing silicone oil with the hydrogen content of 0.5 percent and the viscosity of 50 mPas, 4 parts of hydrophilic fumed silica with the model of cabot 150 and 0.02 part of inhibitor with the mass percent of ethyne cyclohexanol of 0.5 percent are taken and placed in a high-speed shearing disperser to be uniformly dispersed for 60min at room temperature, and the component B is prepared.
(3) At normal temperature, 50 parts of the prepared component A and 50 parts of the prepared component B are uniformly mixed and stirred, and then the mixture is placed in a vacuum machine to be vacuumized at normal temperature, the vacuum degree is-0.09 MPa, and the mixture is kept for 30min to be subjected to bubble removal treatment, so that the addition type heat conduction pouring sealant with good bonding is prepared.
Example 3
(1) At normal temperature, 200 parts of vinyl silicone oil with the vinyl content of 0.43 percent and the viscosity of 500 mPas, 75 parts of quartz powder with the particle size of 5-10 mu m, 80 parts of alumina with the particle size of 5-8 mu m, 2 parts of hydrophilic fumed silica with the type of Kabot 150, 0.6 part of chloroplatinic acid and 8 parts of normal-temperature curing tackifier system are taken and placed in a high-speed shearing disperser to be uniformly dispersed for 60min at room temperature, and the component A is prepared.
(2) At normal temperature, 200 parts of vinyl silicone oil with the vinyl content of 0.43 percent and the viscosity of 500 mPas, 75 parts of quartz powder with the particle size of 3 to 8 mu m, 80 parts of alumina with the particle size of 5 to 8 mu m, 15 parts of hydrogen silicone oil with the hydrogen content of 0.5 percent and the viscosity of 50 mPas, 2 parts of hydrophilic fumed silica with the type of Cabot 150 and 0.02 part of inhibitor with the mass percent of ethynl cyclohexanol of 0.5 percent are taken and placed in a high-speed shearing disperser to be uniformly dispersed for 60min at room temperature, thus obtaining the component B.
(3) At normal temperature, 50 parts of the prepared component A and 50 parts of the prepared component B are uniformly mixed and stirred, and then the mixture is placed in a vacuum machine to be vacuumized at normal temperature, the vacuum degree is-0.09 MPa, and the mixture is kept for 30min to be subjected to bubble removal treatment, so that the addition type heat conduction pouring sealant with good bonding is prepared.
Comparative example 1
(1) At normal temperature, 100 parts of vinyl silicone oil with the vinyl content of 0.57 percent and the viscosity of 300 mPas, 25 parts of quartz powder with the particle size of 3-10 mu m, 75 parts of alumina with the particle size of 3-10 mu m, 2 parts of hydrophilic fumed silica with the type of Kabot 150, 0.4 part of chloroplatinic acid and 8 parts of boron-containing tackifier with the type of Jiangxienna new material Z-15 series are placed in a high-speed shearing disperser and are uniformly dispersed for 60min at room temperature to prepare the component A.
(2) At normal temperature, 100 parts of vinyl silicone oil with the vinyl content of 0.57 percent and the viscosity of 300 mPas, 25 parts of quartz powder with the particle size of 3 to 10 mu m, 75 parts of alumina with the particle size of 3 to 10 mu m, 10 parts of hydrogen silicone oil with the hydrogen content of 0.7 percent and the viscosity of 100 mPas, 2 parts of hydrophilic fumed silica with the type of Cabot 150 and 0.02 part of inhibitor with the mass percent of acetylene cyclohexanol of 1 percent are taken and placed in a high-speed shearing disperser to be uniformly dispersed for 60min at room temperature, so as to prepare the component B.
(3) At normal temperature, 50 parts of the prepared component A and 50 parts of the prepared component B are uniformly mixed and stirred, and then the mixture is placed in a vacuum machine to be vacuumized at normal temperature, the vacuum degree is-0.09 MPa, and the mixture is kept for 30min to remove bubbles, so that the boron-containing tackifier addition type heat conduction pouring sealant is prepared.
Comparative example 2
(1) At normal temperature, 100 parts of vinyl silicone oil with the vinyl content of 0.57 percent and the viscosity of 300 mPas, 25 parts of quartz powder with the particle size of 3-10 mu m, 75 parts of alumina with the particle size of 3-10 mu m, 2 parts of hydrophilic fumed silica with the type of Kabot 150 and 0.4 part of chloroplatinic acid are taken and placed in a high-speed shearing dispersion machine to be uniformly dispersed for 60min at room temperature, and the component A is prepared.
(2) At normal temperature, 100 parts of vinyl silicone oil with the vinyl content of 0.57 percent and the viscosity of 300 mPas, 25 parts of quartz powder with the particle size of 3 to 10 mu m, 75 parts of alumina with the particle size of 3 to 10 mu m, 10 parts of hydrogen silicone oil with the hydrogen content of 0.7 percent and the viscosity of 100 mPas, 2 parts of hydrophilic fumed silica with the type of Cabot 150 and 0.02 part of inhibitor with the mass percent of acetylene cyclohexanol of 1 percent are taken and placed in a high-speed shearing disperser to be uniformly dispersed for 60min at room temperature, so as to prepare the component B.
(3) At normal temperature, 50 parts of the prepared component A and 50 parts of the prepared component B are uniformly mixed and stirred, and then the mixture is placed in a vacuum machine to be vacuumized at normal temperature, the vacuum degree is-0.09 MPa, and the mixture is kept for 30min to be subjected to bubble removal treatment, so that the addition type heat conduction pouring sealant is prepared.
TABLE 2 Performance testing of examples and comparative examples
Note that the notation means that ○ represents cohesive failure ≧ 80%, and X represents cohesive failure ═ 0% (peel).
According to the test results, the normal temperature curing tackifier system is used in the component A in the examples 1-3, the prepared addition type heat conduction pouring sealant has good cohesiveness and can realize room temperature curing, wherein the example 3 not only can have good cohesiveness to copper sheets, aluminum sheets, stainless steel, PCB boards, PBT and the like, but also can realize the cohesiveness to difficult-to-adhere materials such as PC, PS, PMMA and ABS plastics, and has excellent cohesiveness, and the viscosity of the prepared pouring sealant is higher than that of the examples 1, 1 and 2 because the vinyl silicone oil used in the raw material in the example 3 has higher viscosity.
The addition type heat-conducting potting adhesive prepared in the embodiment 1 has good adhesion, can realize room temperature curing, can realize adhesion to copper sheets, aluminum sheets, stainless steel, PCB boards and PBT, and adhesion to difficult-to-adhere materials such as PC and PMMA plastics, but cannot realize adhesion to PS and ABS substrates, and the adhesion force is poorer than that of the potting adhesive prepared in the embodiments 2 and 3 because the mass part of the room temperature curing tackifier system added in the component A in the embodiment 1 is smaller than that in the embodiments 2 and 3.
The addition type heat-conducting potting adhesive prepared in the embodiment 2 has good adhesiveness, can realize room temperature curing, but has a low heat conductivity coefficient, and cannot realize the adhesion to a PS substrate, because only quartz powder filler capable of adjusting fluidity is added into the fillers of the component A and the component B in the embodiment 2, no alumina heat-conducting filler is added, and the vinyl silicone oil used in the component A in the embodiment 2 has an excessively high viscosity, the heat-conducting property is poor, the viscosity is high, and because the mass part of the room temperature curing tackifier system added into the component A is smaller than that of the embodiment 3, the adhesion force is poor compared with that of the potting adhesive prepared in the embodiment 3, the adhesion of PC, PMMA and ABS plastics can be realized, and the adhesion to the PS substrate cannot be realized.
As can be seen from examples 1-3 and comparative examples 1-2, in comparative example 2, the tackifier is not added to the component A, so that the prepared addition type heat-conducting pouring sealant has no adhesive force to the base material, and only depends on a vulcanization network realized by hydrosilylation of vinyl silicone oil and hydrogen-containing silicone oil under the action of a platinum catalyst, so that the surface acting force of the addition type heat-conducting pouring sealant prepared in comparative example 2 and most of the base material is weak, and the adhesion is not caused; the component A of the comparative example 1 is added with the boron-containing tackifier, so that the prepared boron-containing tackifier addition type heat conduction pouring sealant has a bonding effect on most metals and a few plastics, such as copper sheets, aluminum sheets, stainless steel, PCB (printed circuit board), PBT (polybutylene terephthalate) and the like, and cannot form effective bonding force on difficult-to-bond materials such as PC (polycarbonate), PS (polystyrene), PMMA (polymethyl methacrylate), ABS (acrylonitrile butadiene styrene) plastics, and the difficult-to-bond materials such as PC, PS (polystyrene), PMMA (polymethyl methacrylate), ABS (acrylonitrile butadiene styrene) and the like are peeled off in a performance test.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. The preparation method of the normal-temperature curing tackifier system is characterized by comprising the following steps of:
(1) at room temperature, mixing and stirring 6-60 parts of epoxy hydrocarbon silane coupling agent, 6-60 parts of ethyl orthosilicate, 0.2-2 parts of titanate and 6-60 parts of trimethylolpropane diallyl ester uniformly according to the parts by mass of the raw materials;
(2) heating to 75-85 ℃ while stirring and mixing, reacting for 2-3 h, and then decompressing and vacuumizing to remove low-boiling-point substances for 0.5-2 h under the conditions that the temperature and the vacuum degree are-0.09 to-0.1 MPa to obtain a light yellow transparent liquid tackifier with the volatile content of less than 2%;
(3) after the light yellow transparent liquid tackifier is cooled to room temperature, the light yellow transparent liquid tackifier, the boron-containing tackifier and the aluminum-acetylacetone are mixed according to the mass ratio of 48.7: 50: 1.3, uniformly mixing and stirring to obtain the normal-temperature curing tackifier system.
2. The method of claim 1, wherein the titanate is butyl titanate, and the alkylene oxide silane coupling agent is one of 3-glycidoxypropylalkoxysilane or 2- (3, 4-epoxycyclohexyl) ethylalkoxysilane.
3. The method of claim 1, wherein the boron-containing adhesion promoter is one of boric acid, a reactant of boric acid and a multifunctional silane, or a reactant of boric acid and a carbon-functional siloxane.
4. An ambient-temperature-curing tackifier system prepared by the method for preparing an ambient-temperature-curing tackifier system according to any one of claims 1 to 3.
5. A pouring sealant using the normal-temperature curing tackifier system of claim 4, characterized by comprising a component A consisting of vinyl silicone oil, filler, fumed silica, a normal-temperature curing tackifier system and a catalyst, and a component B consisting of vinyl silicone oil, filler, fumed silica, hydrogen-containing silicone oil and an inhibitor;
the formula of the component A comprises the following components in parts by mass:
the formula of the component B comprises the following components in parts by mass:
6. the pouring sealant as claimed in claim 5, wherein the vinyl silicone oil has a viscosity of 100 to 500mPa · s at a temperature of 25 ℃, and the vinyl content of the vinyl silicone oil is 0.1 to 1.0%.
7. The pouring sealant according to claim 5, wherein the filler is one or two of quartz powder and alumina, and is compounded according to any proportion, the particle size of the quartz powder is 3 μm to 10 μm, and the particle size of the alumina is 3 μm to 10 μm.
8. The potting adhesive of claim 5, wherein the hydrogen-containing silicone oil has a hydrogen content of 0.4% to 0.75% and a viscosity of 50 to 500mPa · s at 25 ℃.
9. The pouring sealant as claimed in claim 5, wherein the catalyst is one of chloroplatinic acid or a complex thereof, the platinum content of the catalyst is 1000ppm to 5000ppm, and the fumed silica is hydrophilic fumed silica.
10. The pouring sealant as claimed in claim 5, wherein the inhibitor is a mixture of acetylene cyclohexanol and vinyl silicone oil, wherein the acetylene cyclohexanol accounts for 0.5-1.5% by mass of the inhibitor, and the vinyl silicone oil in the inhibitor has a viscosity of 150-500 mPa · s at a temperature of 25 ℃.
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| CN114231040A (en) * | 2021-12-29 | 2022-03-25 | 中国化工集团曙光橡胶工业研究设计院有限公司 | Flame-retardant silicone rubber self-adhesive tape and preparation method thereof |
| CN115819771A (en) * | 2022-12-06 | 2023-03-21 | 广东普赛达密封粘胶有限公司 | Adhesion promoter polymer, preparation method and application thereof, pouring sealant composition and preparation method thereof |
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| CN114231040A (en) * | 2021-12-29 | 2022-03-25 | 中国化工集团曙光橡胶工业研究设计院有限公司 | Flame-retardant silicone rubber self-adhesive tape and preparation method thereof |
| CN114231040B (en) * | 2021-12-29 | 2023-10-20 | 中国化工集团曙光橡胶工业研究设计院有限公司 | Flame-retardant silicone rubber self-adhesive tape and preparation method thereof |
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