CN106701012B - Light-weight heat-conducting organic silicon pouring sealant base rubber material, composition and preparation method of light-weight heat-conducting organic silicon pouring sealant base rubber material - Google Patents
Light-weight heat-conducting organic silicon pouring sealant base rubber material, composition and preparation method of light-weight heat-conducting organic silicon pouring sealant base rubber material Download PDFInfo
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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
- 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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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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Abstract
The invention discloses a light-weight heat-conducting organic silicon pouring sealant base sizing material which comprises unsaturated alkyl terminated polydiorganosiloxane and also comprises polydiorganosiloxane with the density of 0.1-2.0 g/cm3The invention aims to provide a light-weight heat-conducting organic silicon pouring sealant base rubber material, a preparation method of the base rubber material, a composition adopting the base rubber material and a preparation method of the base rubber material.
Description
Technical Field
The invention relates to the technical field of organic silicon materials, in particular to a light-weight heat-conducting organic silicon pouring sealant base rubber material, a light-weight heat-conducting organic silicon pouring sealant composition and a preparation method of the light-weight heat-conducting organic silicon pouring sealant base rubber material.
Background
The common encapsulating materials in the market mainly comprise materials such as polyurethane, epoxy resin, silicon rubber and the like. The polyurethane material has the advantages of good low temperature resistance and weather resistance, small viscosity, good fluidity, simple processing equipment and process, and easy realization of automatic operation. The disadvantages are that the polyurethane material is toxic and harmful to human health; the epoxy resin has no by-product during curing, small shrinkage, and excellent heat resistance, electric insulation and dielectric property. The defects of large brittleness, insufficient toughness, certain internal stress during curing and easy crack generation after curing; the silicon rubber is not endothermic or exothermic during curing, is not shrunk after curing, has excellent electrical property and chemical stability, does not corrode metal and is non-toxic. Particularly, when the addition type organic silicon encapsulating material is cured, the surface and the deep layer are simultaneously vulcanized, and the vulcanized silicone rubber material has high strength and low shrinkage rate and has good functions of moisture prevention, corrosion prevention, shock prevention, dust prevention and the like.
In recent years, with the high energy, miniaturization, and high performance of various products such as electric vehicle batteries, portable power sources, and LEDs, higher requirements have been placed on the stability, high and low temperature resistance, insulating heat dissipation, and flame retardancy of potting products. The organic silicon electronic encapsulating material has good stability, excellent insulativity, high and low temperature resistance, high oxygen index and other performances, and is always a hot spot concerned by academia. Japanese patent JP5140456[ P ] has found that a silicone rubber having high thermal conductivity and good flame retardancy can be obtained by filling a silicone rubber with a metal powder (e.g., aluminum powder, aluminum nitride powder) and stearic acid-treated aluminum hydroxide powder. JP06234920[ P ] discloses that a silicone rubber material with flame retardant properties can be prepared by filling a silicone rubber with silver powder, boron nitride and a platinum-based flame retardant, the flame retardant rating of which is UL 94-V1. Patent US6448329 teaches that the thermal conductivity of the silicone elastomer is at least 0.8W/m.k, and can even reach 1.5W/m.k, by adding to the organosiloxane 60 to 90% by weight of an aluminum powder filler treated with a silane coupling agent. In patent CN103102689A [ P ], 100 parts of vinyl silicone oil is adopted to prepare the high-thermal-conductivity organic silicon potting material by matching with 400-1000 parts of organic silicon-coated alumina powder.
At this stage, with the rapid development of electric vehicles, safety problems about electric vehicles are endless. How to avoid or reduce hidden dangers such as combustion and explosion generated in the processes of overcharging, short circuit, soaking, collision and the like of a power battery pack of an electric automobile, and personal safety is guaranteed to become a new hotspot of the electric automobile industry. The specific gravity of the traditional pouring sealant is about 1.5-1.6, the specific gravity can reach 1.2-2.0 with special requirements, and the specific gravity of the pouring sealant without heat conduction can reach 1.0-1.2; but generally will not be below 1.0. Therefore, in the related art in this field, there is no disclosure of a proposal for unifying the specific gravity and the heat conductive property well.
Disclosure of Invention
In view of the above disadvantages, the present invention provides a light-weight heat-conducting silicone potting adhesive base adhesive, a preparation method of the base adhesive, a composition using the base adhesive, and a preparation method of the base adhesive.
The former technical scheme of the invention is as follows: a light-weight heat-conducting organic silicon pouring sealant base sizing material comprises unsaturated alkyl end-blocked polydiorganosiloxane and also comprises a density of 0.1-2.0 g/cm3The lightweight heat conductive filler.
In the light-weight heat-conducting organic silicon pouring sealant base rubber material, the using amount of the light-weight heat-conducting filler is 1-180 parts by mass relative to 100 parts by weight of unsaturated alkyl terminated polydiorganosiloxane.
In the light-weight heat-conducting organic silicon pouring sealant base sizing material, the light-weight heat-conducting filler is one or a combination of hollow glass microspheres, hollow ceramic microspheres, hollow alumina microspheres, hollow aluminum nitride microspheres and hollow aluminum carbide microspheres.
In the light-weight heat-conducting organic silicon pouring sealant base rubber material, the density of the light-weight heat-conducting filler is 0.1-1.5g/cm3And the particle size of the lightweight heat-conducting filler is 1um-100 um.
The light-weight heat-conducting organic silicon pouring sealant base sizing material also comprises alkoxy end-blocked polydimethylsiloxane, and the alkoxy end-blocked polydimethylsiloxane accounts for 5-18 parts by weight relative to 100 parts by weight of unsaturated alkyl end-blocked polydiorganosiloxane.
In the light-weight heat-conducting organic silicon pouring sealant base sizing material, the structural formula of the alkoxy-terminated polydimethylsiloxane is shown in the following formula 1:
wherein w is 5-60;
r is C1-C3 alkyl, such as methyl, ethyl, propyl.
In the practical application process, the alkoxy-terminated polydimethylsiloxane can be obtained by adopting the addition reaction of hydroxyl-terminated polydimethylsiloxane and a corresponding end-capping auxiliary agent, and the addition reaction is a more common reaction in the field, so that the invention is not limited too much.
In the light-weight heat-conducting organic silicon pouring sealant base sizing material, w is 10-30.
In the light-weight heat-conducting silicone pouring sealant base rubber material, the unsaturated alkyl-terminated polydiorganosiloxane has the following structure of formula 2:
wherein, x is 10-500, y is 0-50; preferably, x is 20-400, and y is 0-30; more preferably, x is 20 to 400 and y is 0 to 10.
R1、R3Is a C2-C3 aliphatic unsaturated hydrocarbon group; for example, any of vinyl and allyl, preferably vinyl.
R2Is any of C1-C3 alkyl. Such as methyl, ethyl, propyl, C2-C3 alkenyl such as vinyl, allyl;
the light-weight heat-conducting organic silicon pouring sealant base sizing material also comprises saturated alkyl end-blocked polydiorganosiloxane, and the using amount of the saturated alkyl end-blocked polydiorganosiloxane is 20-80 parts by mass relative to 100 parts by weight of unsaturated alkyl end-blocked polydiorganosiloxane.
In the above light weight heat conductive silicone potting adhesive base compound, the saturated hydrocarbon group terminated polydiorganosiloxane has the following formula 3:
wherein z is 10-100, preferably z is 10-50; r4、R5Is C1-C2 alkyl such as methyl, ethyl.
The light-weight heat-conducting organic silicon pouring sealant base rubber material also comprises a flame-retardant filler, and the using amount of the flame-retardant filler is 5-180 parts by mass relative to 100 parts by weight of unsaturated alkyl terminated polydiorganosiloxane.
In the light-weight heat-conducting organosilicon potting adhesive base sizing material, the flame-retardant filler is one or a mixture of aluminum hydroxide, magnesium hydroxide, zinc carbonate and zinc borate.
In the light-weight heat-conducting organic silicon pouring sealant base rubber material, the particle size of the flame-retardant filler is 0.1-50 um.
The light-weight heat-conducting organic silicon pouring sealant base rubber material also comprises a filler treating agent, and the using amount of the filler treating agent is 5-18 parts by mass relative to 100 parts by weight of unsaturated alkyl terminated polydiorganosiloxane.
In the above light-weight heat-conducting silicone pouring sealant base compound, the filler treating agent is any one of epoxy silane, vinyl silane and acyl silane or a mixture thereof.
Specifically, the filler treating agent may be an epoxysilane such as 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane; also vinyl silanes such as vinyltriethoxysilane, vinylmethyldiethoxysilane, vinyltrimethoxysilane, vinylmethyldimethoxysilane; it may be any one of acylsilanes such as 3- (methacryloyloxy) propyltrimethoxysilane, 3- (methacryloyloxy) propyltriethoxysilane, 3- (methacryloyloxy) propylmethyldimethoxysilane, 3- (methacryloyloxy) propylmethyldiethoxysilane, 3- (methacryloyloxy) propyltriisopropoxysilane or a mixture thereof.
Meanwhile, the invention also provides a preparation method of the light-weight heat-conducting organic silicon pouring sealant base sizing material, which comprises the following steps:
step 1: adding unsaturated alkyl end-blocked polydiorganosiloxane into a vacuum kneading machine, then adding light heat-conducting filler for multiple times, and stirring and mixing for 0.5-2.0 hours;
step 2: heating to 120-160 ℃, and mixing for 2.0-6.0 hours;
and step 3: removing low molecular substances in vacuum for 1.0-4.0 hours;
and 4, step 4: and cooling and filtering to prepare the light-weight heat-conducting organic silicon pouring sealant base rubber material.
In the preparation method of the light-weight heat-conducting silicone pouring sealant base rubber material, in step 1, saturated hydrocarbyl-terminated polydiorganosiloxane is also added when the unsaturated hydrocarbyl-terminated polydiorganosiloxane is added into a vacuum kneader.
In the preparation method of the light-weight heat-conducting organic silicon pouring sealant base rubber material, in the step 1, the flame-retardant filler and the filler treating agent are added while the light-weight heat-conducting filler is added for multiple times.
In the preparation method of the light-weight heat-conducting organic silicon pouring sealant base rubber material, a step 1-1 is also included between the step 1 and the step 2;
the step 1-1 is as follows: alkoxy-terminated polydimethylsiloxane was added, and the mixture was stirred and mixed for 0.5 to 2.0 hours and then subjected to step 2.
And step 1-1, adding alkoxy end-capped polydimethylsiloxane, continuously stirring and mixing for 0.5-2.0 hours, forming flexible chain links between the heat-conducting filler and the polydiorganosiloxane, and improving the toughness of the product. If the stirring and mixing time is less than 0.5 hour, the reaction is insufficient.
In addition, the invention also provides a lightweight heat-conducting organic silicon pouring sealant composition which is prepared from the component A and the component B in a weight ratio of 1: 1;
wherein, the component A comprises: 100 parts by mass of the light-weight heat-conducting organic silicon pouring sealant base rubber material and 0.02-0.4 part by mass of an addition reaction catalyst;
the component B comprises: 100 parts by mass of the light-weight heat-conducting organic silicon pouring sealant base rubber material, 1-10 parts by mass of a cross-linking agent and 0.01-0.1 part by mass of an addition reaction inhibitor.
The addition reaction catalyst is any one of palladium catalyst, platinum catalyst or rhodium catalyst; the platinum catalyst is any one of chloroplatinic acid, platinum tetrachloride or a complex of platinum and a vinyl compound and platinum diacetylacetate;
the crosslinking agent is organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent is shown as the following formula 4:
in the formula: m is 0-100, n is 2-30;
r6, R7 are independently methyl or hydrogen radicals, but contain at least two hydrogen radicals, preferably three or more hydrogen radicals, per molecule.
The addition reaction inhibitor is a vinyl-containing compound, preferably selected from: tetramethyltetravinylcyclotetrasiloxane, hexamethyldivinylcyclotetrasiloxane, tetramethyldivinylsilane, trimethyltrivinylsilane, dimethyltetravinylsilane, dimethyldivinylsilane, methyltrivinylsilane, dimethylvinylmethoxysilane, dimethylvinylethoxysilane.
Meanwhile, the invention also provides a preparation method of the lightweight heat-conducting organic silicon pouring sealant composition, which comprises the following steps:
step 1: adding the light-weight heat-conducting organic silicon pouring sealant base rubber material into an addition reaction catalyst, uniformly stirring, degassing, and filtering to obtain a component A;
step 2: adding a crosslinking agent and an addition reaction inhibitor into the light-weight heat-conducting organic silicon pouring sealant base rubber material, uniformly stirring, degassing, and filtering to obtain a component B;
and step 3: the component A and the component B are mixed according to the proportion of 1:1, pouring the mixture into a mold, and standing for 48 hours at 25 ℃.
Compared with the traditional method, the method has the following advantages:
(1) the lightweight heat-conducting filler is adopted, so that the heat-conducting property can be effectively improved, the product density is reduced, and the lightweight of the product is realized;
(2) the invention adopts alkoxy end-capped polydimethylsiloxane, which can effectively improve the tensile strength and tensile elongation of the product;
(3) the invention adopts the flame-retardant filler and the filler treating agent, and can improve the flame retardant property of the product while realizing the light weight of the product. More specifically, the heat-conducting filler and the flame-retardant filler are subjected to surface treatment through the comprehensive action of the filler treating agent and alkoxy-terminated polydimethylsiloxane, so that the compatibility of the filler in the rubber material is improved, and the flowability of the rubber material is improved. The introduction of the alkoxy end-capped polydimethylsiloxane can effectively improve the mechanical strength of the pouring sealant and improve the flexibility.
The lightweight heat-conducting organic silicon pouring sealant composition has good fluidity, can be cured at room temperature or at high temperature, has high molding speed, no by-product in the curing process, less material loss and is convenient for realizing continuous pouring operation; the pouring sealant has the characteristics of good thermal conductivity, high flame retardant efficiency, low specific gravity, small permanent compression deformation, outstanding electrical property and the like after being cured,
the light-weight heat-conducting organic silicon pouring sealant composition generally has Shore A hardness of 10-60, preferably Shore A hardness of 15-35, tensile strength of 0.5-5.0 MPa, elongation of 20-150% and tear strength of 1.0-12.0 kN/m. In addition, it also generally has an insulation resistor 1012-1015Ω·cm。
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The following claims are hereby incorporated into the detailed description of the invention, with the understanding that the present disclosure is to be considered as a full and non-limiting example, and any limited number of modifications that may be made within the scope of the claims are intended to be included within the scope of the invention.
Example 1
100 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 0 part by mass of a saturated hydrocarbon group-terminated polydiorganosiloxane (b) were added to a vacuum kneader, and then 50 parts by mass of a polydiorganosiloxane (b) having a particle diameter of 1um and a density of 0.4g/cm were added in multiple portions3Stirring and mixing the hollow glass microsphere heat-conducting filler (c), 30 parts by mass of aluminum hydroxide flame-retardant filler (d) with the particle size of 5 mu m and 10 parts by mass of 3-glycidoxypropyltrimethoxysilane treating agent (e) for 1.0 hour, then adding 0 part by mass of alkoxy-terminated polydimethylsiloxane (f), and continuously stirring and mixing for 0.5 hour; heating to 120 ℃ and mixing for 2.0 hours; removing low molecules for 1.0 hour in vacuum; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 100 parts by mass of the base sizing material of the organic silicon pouring sealant into 0.02 part by mass of chloroplatinic acid catalyst (g), stirring uniformly, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organosilicon potting adhesive base rubber material into 10 parts by mass of a cross-linking agent (h) and 0.01 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor (i), stirring uniformly, degassing bubbles, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
vi is an abbreviation for vinyl.
The structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 2
100 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 20 parts by mass of a saturated hydrocarbon group-terminated polydiorganosiloxane (b) were added to a vacuum kneader, and 1 part by mass of a polydiorganosiloxane (b) having a particle diameter of 5 μm and a density of 2.0g/cm was added in multiple portions3The hollow ceramic microsphere heat-conducting filler (c), 90 parts by mass of magnesium hydroxide flame-retardant filler (d) with the particle size of 2um and 5 parts by mass of 3-glycidyl ether oxypropyl methyldiethoxysilane treating agent (e) are stirred and mixed for 2.0 hours, then 8 parts by mass of alkoxy-terminated polydimethylsiloxane (f) is added, and the stirring and mixing are continued for 0.8 hours; heating to 130 ℃ and mixing for 3.0 hours; removing low molecules in vacuum for 2.0 hours; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 100 parts by mass of the organic silicon pouring sealant basic rubber material into 0.04 part by mass of platinum tetrachloride catalyst (g), stirring uniformly, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organosilicon potting adhesive base rubber material into 8 parts by mass of a cross-linking agent (h) and 0.02 part by mass of a hexamethyl divinyl cyclo-tetrasiloxane inhibitor (i), stirring uniformly, degassing bubbles, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 3
100 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 40 parts by mass of a saturated hydrocarbon group-terminated polydiorganosiloxane (b) were added to a vacuum kneader, and 25 parts by mass of a polydiorganosiloxane (b) having a particle diameter of 20 μm and a density of 0.1g/cm were added in multiple portions3Stirring and mixing the hollow alumina microsphere heat-conducting filler (c), 5 parts by mass of aluminum hydroxide flame-retardant filler (d) with the particle size of 2um and 7 parts by mass of 3-glycidyl ether oxypropyl trimethoxy silane treating agent (e) for 0.8 hour, then adding 5 parts by mass of alkoxy-terminated polydimethylsiloxane (f), and continuously stirring and mixing for 0.8 hour; heating to 140 ℃ and mixing for 4.0 hours; removing low molecules in vacuum for 3.0 hours; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 0.06 part by mass of diacetyl acetic acid platinum catalyst (g) into 100 parts by mass of the organic silicon pouring sealant base rubber material, uniformly stirring, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organic silicon pouring sealant base rubber material into 6 parts by mass of a cross-linking agent (h) and 0.03 part by mass of a tetramethyldivinylsilane inhibitor (i), uniformly stirring, degassing, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 4
Adding 100 parts by mass of unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 80 parts by mass of saturated hydrocarbon group-terminated polydiorganosiloxane (b) into a vacuum kneader, and adding 180 parts by mass of a mixture of 100um particles having a particle size and 1.0g/cm density3The hollow glass microsphere heat-conducting filler (c), 0 mass part of flame-retardant filler (d) and 18 mass parts of vinyl triethoxy siliconThe alkane treating agent (e) is stirred and mixed for 0.5 hour, 5 parts by mass of alkoxy-terminated polydimethylsiloxane (f) is added, and the mixture is continuously stirred and mixed for 1.0 hour; heating to 150 ℃ and mixing for 5.0 hours; removing low molecules in vacuum for 4.0 hours; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 100 parts by mass of the organic silicon pouring sealant basic rubber material into 0.1 part by mass of platinum tetrachloride catalyst (g), stirring uniformly, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the base rubber material of the organic silicon pouring sealant into 2 parts by mass of a cross-linking agent (h) and 0.04 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor (i), stirring uniformly, degassing bubbles, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 5
100 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 20 parts by mass of a saturated hydrocarbon group-terminated polydiorganosiloxane (b) were added to a vacuum kneader, and then 30 parts by mass of a polydiorganosiloxane (b) having a particle diameter of 20 μm and a density of 0.5g/cm were added in multiple portions3Stirring and mixing the hollow aluminum nitride microsphere heat-conducting filler (c), 120 parts by mass of zinc carbonate flame-retardant filler (d) with the particle size of 0.1um and 10 parts by mass of vinyl triethoxysilane treating agent (e) for 1.0 hour, then adding 10 parts by mass of alkoxy-terminated polydimethylsiloxane (f), and continuously stirring and mixing for 1.5 hours; heating to 160 ℃ and mixing for 6.0 hours; removing low molecules in vacuum for 3.0 hours; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 0.2 part by mass of complex catalyst (g) of platinum and vinyl compound into 100 parts by mass of the organic silicon pouring sealant base rubber material, uniformly stirring, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organic silicon pouring sealant base rubber material into 8 parts by mass of a cross-linking agent (h) and 0.05 part by mass of a dimethyl tetravinyl silane inhibitor (i), uniformly stirring, degassing bubbles, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 6
100 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 60 parts by mass of a saturated hydrocarbon group-terminated polydiorganosiloxane (b) were added to a vacuum kneader, and 120 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) having a particle diameter of 20 μm and a density of 0.4g/cm were added in multiple portions3Stirring and mixing the hollow glass microsphere heat-conducting filler (c), 10 parts by mass of aluminum hydroxide flame-retardant filler (d) with the particle size of 5um and 10 parts by mass of vinyl methyl dimethoxy silane treating agent (e) for 1.2 hours, then adding 8 parts by mass of alkoxy-terminated polydimethylsiloxane (f), and continuously stirring and mixing for 1.8 hours; heating to 120 ℃ and mixing for 5.0 hours; removing low molecules in vacuum for 2.0 hours; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 100 parts by mass of the organic silicon pouring sealant basic rubber material into 0.3 part by mass of chloroplatinic acid catalyst (g), stirring uniformly, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organosilicon potting adhesive base rubber material into 3 parts by mass of a cross-linking agent (h) and 0.07 part by mass of a tetramethyltetravinylcyclotetrasiloxane inhibitor (i), stirring uniformly, degassing bubbles, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 7
100 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 40 parts by mass of a saturated hydrocarbon group-terminated polydiorganosiloxane (b) were added to a vacuum kneader, and then 20 parts by mass of a polydiorganosiloxane (b) having a particle diameter of 5 μm and a density of 0.8g/cm were added in multiple portions3Stirring and mixing the hollow ceramic microsphere heat-conducting filler (c), 20 parts by mass of magnesium hydroxide flame-retardant filler (d) with the particle size of 50um and 0 part by mass of 3- (methacryloyloxy) propyl trimethoxy silane treating agent (e) for 1.0 hour, then adding 18 parts by mass of alkoxy-terminated polydimethylsiloxane (f), and continuously stirring and mixing for 1.5 hours; heating to 140 ℃ and mixing for 4.0 hours; removing low molecules for 1.0 hour in vacuum; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 100 parts by mass of the organic silicon pouring sealant basic rubber material into 0.4 part by mass of platinum tetrachloride catalyst (g), stirring uniformly, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organosilicon potting adhesive base rubber material into 5 parts by mass of a cross-linking agent (h) and 0.1 part by mass of a dimethyl divinyl silane inhibitor (i), uniformly stirring, degassing, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 8
100 parts by mass of an unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) and 80 parts by mass of a saturated hydrocarbon group-terminated polydiorganosiloxane (b) were added to a vacuum kneader, and 5 parts by mass of a polydiorganosiloxane (b) having a particle diameter of 10 μm and a density of 0.5g/cm were added in multiple portions3Stirring and mixing the hollow aluminum carbide microsphere heat-conducting filler (c), 180 parts by mass of zinc borate flame-retardant filler (d) with the particle size of 10um and 5 parts by mass of 3- (methacryloyloxy) propyl triethoxysilane treating agent (e) for 0.5 hour, adding 15 parts by mass of alkoxy-terminated polydimethylsiloxane (f), and continuing to addStirring and mixing for 2.0 hours; heating to 150 ℃ and mixing for 3.0 hours; removing low molecules in vacuum for 4.0 hours; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 100 parts by mass of the organic silicon pouring sealant basic rubber material into 0.25 part by mass of chloroplatinic acid catalyst (g), stirring uniformly, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organic silicon pouring sealant base rubber material into 1 part by mass of a cross-linking agent (h) and 0.06 part by mass of a dimethyl vinyl ethoxy silane inhibitor (i), uniformly stirring, degassing bubbles, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
example 9
100 parts by mass ofAdding unsaturated alkyl terminated polydiorganosiloxane (a) and 20 parts by mass of saturated alkyl terminated polydiorganosiloxane (b) into a vacuum kneader, and adding 30 parts by mass of polydiorganosiloxane (a) with a particle size of 20um and a density of 0.5g/cm3Stirring and mixing the hollow aluminum nitride microsphere heat-conducting filler (c), 120 parts by mass of zinc carbonate flame-retardant filler (d) with the particle size of 0.1um and 10 parts by mass of vinyl triethoxysilane treating agent (e) for 1.0 hour, then adding 0 part by mass of alkoxy-terminated polydimethylsiloxane (f), and continuously stirring and mixing for 1.5 hours; heating to 160 ℃ and mixing for 6.0 hours; removing low molecules in vacuum for 3.0 hours; and cooling and filtering to prepare the light-weight heat-conducting flame-retardant organic silicon pouring sealant base rubber material.
Adding 0.2 part by mass of complex catalyst (g) of platinum and vinyl compound into 100 parts by mass of the organic silicon pouring sealant base rubber material, uniformly stirring, degassing, and filtering to obtain a component (A);
adding 100 parts by mass of the organic silicon pouring sealant base rubber material into 8 parts by mass of a cross-linking agent (h) and 0.05 part by mass of a dimethyl tetravinyl silane inhibitor (i), uniformly stirring, degassing bubbles, and filtering to obtain a component (B);
the components (A) and (B) are mixed according to the proportion of 1:1, pouring the mixture into a mold with the depth of 2mm, standing for 48 hours at 25 ℃ to obtain the light-weight heat-conducting flame-retardant organic silicon pouring sealant film, and testing the performance.
The unsaturated hydrocarbon group-terminated polydiorganosiloxane (a) described above has the following structural formula:
the structure of the saturated hydrocarbon group-terminated polydiorganosiloxane (b) is as follows:
the alkoxy-terminated polydimethylsiloxane (f) has the following structural formula:
the crosslinking agent (h) is an organic hydrogen polysiloxane, and the molecular general formula of the crosslinking agent (h) is as follows:
the 2mm thick films of the above examples were used to measure physical properties, wherein the hardness (Shore A) was tested according to the standard GB/T531-1999; tensile strength, elongation at break were tested according to the standard GB/T528-; the tear strength is tested according to the standard GB/T529-; detecting the material density according to GB/T533-; the volume resistivity detection is carried out according to the standard GB/T1410-2006 material volume resistivity and surface resistivity test method, and the test results are shown in Table 1.
TABLE 1 results of physical and mechanical properties and dielectric properties of films
From the above table it can be seen that:
1. when the addition amount of the heat-conducting filler is more, the density is smaller, and the density of the film is smaller; it can be seen from the above table that the larger the specific gravity and the larger the addition amount of the heat conductive filler, the higher the heat conductivity coefficient of the heat conductive filler, and in addition, the hydroxide or carbonate flame retardant has a certain contribution to the improvement of the heat conductivity coefficient, and the both cooperate to improve the heat conductive effect of the potting adhesive.
2. Increasing f increases strength at the same amount of filler; if the amount of the filler is changed, the strength is reduced due to the increase of the heat-conducting filler and the flame-retardant filler, and the combined action of the heat-conducting filler and the flame-retardant filler causes the change of the strength, not only the change of the amount f. More specifically, the reason why the alkoxy-terminated polydimethylsiloxane can effectively improve the strength of the pouring sealant is that the introduction of alkoxy-terminated polydimethylsiloxane, which is another surface treatment agent capable of being used as a filler, can effectively improve the mechanical strength of the pouring sealant and improve the flexibility.
3. The volume resistivity is an important consideration of the pouring sealant, which is an important reference for the insulation performance of the pouring sealant, and the volume resistivity of the conventional pouring sealant is generally 1013-1014Ω · CM, however, in example 3, the volume resistivity thereof reached 1015And (4) grading, and having a very excellent insulation effect.
The above description is only exemplary of the invention, and any modification, equivalent replacement, and improvement made within the spirit and scope of the present invention should be considered within the scope of the present invention.
Claims (15)
1. A light-weight heat-conducting organic silicon pouring sealant base sizing material comprises unsaturated alkyl terminated polydiorganosiloxane and is characterized by further comprising polydiorganosiloxane with the density of 0.1-2.0 g/cm3The light-weight heat-conducting filler is also added with alkoxy-terminated polydimethylsiloxane and saturated alkyl-terminated polydiorganosiloxane; 5 to 18 parts by weight of an alkoxy-terminated polydimethylsiloxane per 100 parts by weight of an unsaturated hydrocarbon-terminated polydiorganosiloxane;
the structural formula of the alkoxy-terminated polydimethylsiloxane is shown as the following formula 1:
formula 1;
wherein w = 5-60;
r is C1-C3 alkyl;
the saturated hydrocarbon group-terminated polydiorganosiloxane is used in an amount of 20 to 80 parts by weight relative to 100 parts by weight of the unsaturated hydrocarbon group-terminated polydiorganosiloxane;
the saturated hydrocarbyl terminated polydiorganosiloxane has the formula 3 below:
formula 3
Wherein z = 10-100; r4、R5Is C1-C2 alkyl.
2. The light-weight heat-conducting silicone potting adhesive base stock as claimed in claim 1, wherein the light-weight heat-conducting filler is used in an amount of 1 to 180 parts by weight per 100 parts by weight of the unsaturated hydrocarbon group-terminated polydiorganosiloxane.
3. The light-weight heat-conducting silicone pouring sealant base rubber material as claimed in claim 1, wherein the light-weight heat-conducting filler is one or a combination of hollow glass microspheres, hollow ceramic microspheres, hollow alumina microspheres, hollow aluminum nitride microspheres and hollow aluminum carbide microspheres.
4. The light-weight heat-conducting silicone pouring sealant base rubber material as claimed in claim 3, wherein the density of the light-weight heat-conducting filler is 0.1-1.5g/cm3And the particle size of the lightweight heat-conducting filler is 1um-100 um.
5. The light-weight heat-conducting silicone pouring sealant base compound according to claim 1, wherein w = 10-30.
6. The light weight, heat conductive silicone potting adhesive base stock of any of claims 1 to 4, wherein the unsaturated hydrocarbon group-terminated polydiorganosiloxane has the following structure 2:
formula 2
Wherein x =10-500, y = 0-50;
R1、R3is a C2-C3 aliphatic unsaturated hydrocarbon group;
R2is any one of C1-C3 alkyl.
7. The light-weight heat-conducting silicone pouring sealant base stock according to any one of claims 1 to 4, further comprising a flame-retardant filler in an amount of 5 to 180 parts by weight relative to 100 parts by weight of the unsaturated hydrocarbon group-terminated polydiorganosiloxane.
8. The light-weight heat-conducting silicone pouring sealant base stock according to claim 7, wherein the flame-retardant filler is one or a mixture of aluminum hydroxide, magnesium hydroxide, zinc carbonate and zinc borate.
9. The light-weight heat-conducting silicone pouring sealant base stock according to claim 8, wherein the particle size of the flame-retardant filler is 0.1-50 um.
10. The light-weight heat-conductive silicone potting adhesive base stock of claim 7, further comprising a filler treating agent in an amount of 5 to 18 parts by weight per 100 parts by weight of the unsaturated hydrocarbon group-terminated polydiorganosiloxane.
11. The light-weight heat-conducting silicone pouring sealant base stock according to claim 10, wherein the filler treating agent is any one of epoxy silane, vinyl silane, acyl silane, or a mixture thereof.
12. The preparation method of the light-weight heat-conducting silicone pouring sealant base compound according to any one of claims 1 to 11, characterized by comprising the following steps:
step 1: adding unsaturated alkyl end-blocked polydiorganosiloxane into a vacuum kneading machine, then adding light heat-conducting filler for multiple times, and stirring and mixing for 0.5-2.0 hours;
step 2: heating to 120-160 ℃, and mixing for 2.0-6.0 hours;
and step 3: removing low molecular substances in vacuum for 1.0-4.0 hours;
and 4, step 4: cooling and filtering to prepare a light-weight heat-conducting organic silicon pouring sealant base rubber material;
in step 1, a saturated hydrocarbon group-terminated polydiorganosiloxane is also added while the unsaturated hydrocarbon group-terminated polydiorganosiloxane is added to the vacuum kneader;
a step 1-1 is also included between the step 1 and the step 2;
the step 1-1 is as follows: alkoxy-terminated polydimethylsiloxane was added, and the mixture was stirred and mixed for 0.5 to 2.0 hours and then subjected to step 2.
13. The preparation method of the light-weight heat-conducting silicone pouring sealant base rubber material according to claim 12, wherein in step 1, the flame-retardant filler and the filler treating agent are added while the light-weight heat-conducting filler is added for a plurality of times.
14. The lightweight heat-conducting organic silicon pouring sealant composition is characterized by comprising a component A and a component B in a weight ratio of 1: 1;
wherein, the component A comprises: 100 parts by mass of the light-weight heat-conducting silicone potting adhesive base compound as claimed in any of claims 1 to 11 and 0.02 to 0.4 part by mass of an addition reaction catalyst;
the component B comprises: 100 parts by mass of the light-weight heat-conducting silicone pouring sealant base rubber compound as defined in any one of claims 1 to 11, 1 to 10 parts by mass of a crosslinking agent, and 0.01 to 0.1 part by mass of an addition reaction inhibitor.
15. The preparation method of the light-weight heat-conducting silicone pouring sealant composition as claimed in claim 14, characterized by comprising the following steps:
step 1: adding the light-weight heat-conducting organic silicon pouring sealant base rubber material into an addition reaction catalyst, uniformly stirring, degassing, and filtering to obtain a component A;
step 2: adding a crosslinking agent and an addition reaction inhibitor into the light-weight heat-conducting organic silicon pouring sealant base rubber material, uniformly stirring, degassing, and filtering to obtain a component B;
and step 3: the component A and the component B are mixed according to the proportion of 1:1, pouring the mixture into a mold, and standing at 25 ℃ for a period of time to obtain the product.
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