A tackifier, two-component addition-type silicone rubber, and preparation method and application thereof

Abstract

The present invention belongs to the technical field of organic silicon polymer materials, and particularly relates to a tackifier, a two-component addition-type silicone rubber, and a preparation method and application thereof. A tackifier, wherein the raw materials for preparing the tackifier include end-side hydrogenated silicone oil, aminosilane, epoxysilane, and a solid acid catalyst; at 23°C, the viscosity of the end-side hydrogenated silicone oil is less than 200mPa·s, and the hydrogen content of the end-side hydrogenated silicone oil is less than 0.8wt%; the aminosilane does not include dodecyltrimethoxysilane. In the present invention, under the action of a solid acid catalyst, aminosilane and epoxysilane are bonded to the hydrogenated silicone oil molecule through the alkoxy group in the molecule and the silicon-hydrogen bond reaction in the hydrogenated silicone oil; when the tackifier is applied to the two-component addition-type silicone rubber, the silicone rubber has good bonding properties, which can meet the sealing performance requirements of the product.

Description

Technical Field

[0001] The invention belongs to the technical field of organic silicon polymer materials, and particularly relates to a tackifier, a two-component addition-type silicone rubber, and a preparation method and application thereof. Background Art

[0002] Silicone materials are widely used in the field of electronics and electrical appliances because of their good electrical insulation and weather resistance. Silicone potting adhesives are divided into two categories: condensation type and addition type. The silicone potting adhesives on the market are mainly addition type. With the rapid development of the electronics and electrical appliance industry, the use conditions of electronics and electrical appliances are becoming more and more stringent. Addition type silicone rubber has poor adhesion to metals, plastics, PCB boards and other substrates. It is easy to separate from the potted products under the alternating effects of high and low temperatures, resulting in large gaps, which greatly reduces the protective performance and cannot meet the product's requirements for sealing performance.

[0003] Some studies have linked KH560 and KH570 to hydroxy silicone oil through organic tin catalysis. The organic tin used will make the platinum catalyst inactive, which has a great impact on the performance of the potting compound. At the same time, there are also studies on the preparation method of thickeners for addition-type silicone thermal conductive potting compounds, but the preparation process requires the use of graphene, which has a high preparation cost, and the synthesis temperature reaches 150°C, which consumes a lot of energy and does not meet the needs of energy saving and consumption reduction.

[0004] Therefore, there is an urgent need to provide a tackifier with low cost and simple preparation process. The tackifier is used in the preparation of two-component addition-type silicone rubber to make the silicone rubber have good bonding properties and can well meet the sealing performance requirements of the product. Summary of the invention

[0005] The present invention aims to solve one or more technical problems existing in the prior art, and at least provide a beneficial choice or create conditions. The present invention provides a tackifier, which has low cost and simple preparation process. The tackifier is used in the preparation of two-component addition-type silicone rubber, so that the silicone rubber has good bonding performance and can well meet the sealing performance requirements of the product.

[0006] The inventive concept of the present invention is as follows: the tackifier of the present invention contains end-side hydrogen-containing silicone oil, aminosilane, epoxysilane, and a solid acid catalyst; under the action of the solid acid catalyst, the aminosilane and epoxysilane are bonded to the hydrogen-containing silicone oil molecules through the alkoxy groups in the molecules and the silicon-hydrogen bonds in the hydrogen-containing silicone oil; when the tackifier is applied to two-component addition-type silicone rubber, during the curing process of the silicone rubber, the hydrogen-containing silicone oil with aminosilane and epoxysilane on the molecular chain participates in the curing reaction, and the amino groups and epoxy groups in the aminosilane and epoxysilane form hydrogen bonds or covalent bonds with the hydroxyl groups on the surface of the substrate, so that the substrate and the silicone rubber are well bonded, so that the prepared silicone rubber has good bonding properties and can meet the sealing performance requirements of the product.

[0007] Therefore, a first aspect of the present invention provides a tackifier.

[0008] Specifically, a tackifier, wherein the raw materials for preparing the tackifier include end-side hydrogen-containing silicone oil, aminosilane, epoxysilane, and a solid acid catalyst;

[0009] At 23° C., the viscosity of the end-side hydrogen-containing silicone oil is less than 200 mPa·s, and the hydrogen content of the end-side hydrogen-containing silicone oil is less than 0.8 wt %;

[0010] The aminosilane does not include dodecyltrimethoxysilane.

[0011] Specifically, the catalyst used in the present invention is a solid acid catalyst. In the reaction system, the catalyst is solid and the other raw materials are liquid, forming heterogeneous catalysis. After the reaction is completed, the catalyst can be filtered out by filtering through a filter and can be recycled, saving costs.

[0012] Preferably, at 23° C., the viscosity of the end-side hydrogen-containing silicone oil is 27-110 mPa·s, and the hydrogen content of the end-side hydrogen-containing silicone oil is 0.08-0.6 wt %.

[0013] Further preferably, at 23° C., the viscosity of the end-side hydrogen-containing silicone oil is 30-100 mPa·s, and the hydrogen content of the end-side hydrogen-containing silicone oil is 0.1-0.5 wt %.

[0014] Preferably, the raw materials for preparing the tackifier include, by weight, 180-270 parts of end-side hydrogenated silicone oil, 35-88 parts of aminosilane, 45-110 parts of epoxysilane, and 4-12 parts of solid acid catalyst.

[0015] Further preferably, the raw materials for preparing the tackifier include, by weight, 200-250 parts of end-side hydrogenated silicone oil, 40-80 parts of aminosilane, 50-100 parts of epoxysilane, and 5-10 parts of solid acid catalyst.

[0016] Preferably, the aminosilane is selected from at least one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-aminopropylmethyldimethoxysilane, 3-aminopropylmethyldiethoxysilane, N-cyclohexyl-3-aminopropylmethyldimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, 3-(N-cyclohexylamino)propyltrimethoxysilane, N-(n-butyl)-3-aminopropyltriethoxysilane, N-(n-butyl)-3-aminopropyltrimethoxysilane and N,N-diethyl-3-aminopropyltrimethoxysilane.

[0017] Preferably, the epoxysilane is selected from at least one of γ-glycidyloxypropyltrimethoxysilane, γ-glycidyloxypropyltriethoxysilane, 3-glycidyloxypropylmethyldimethoxysilane and 3-glycidyloxypropylmethyldiethoxysilane.

[0018] Preferably, the solid acid catalyst is a strong acid cation exchange resin.

[0019] The second aspect of the present invention provides a method for preparing the tackifier described in the first aspect of the present invention.

[0020] Specifically, a method for preparing a tackifier comprises the following steps:

[0021] The various raw material components are mixed to prepare the viscosity enhancing agent.

[0022] Preferably, the aminosilane, epoxysilane and solid acid catalyst are mixed, and then the end-side hydrogen-containing silicone oil is added and mixed, and the solid acid catalyst is filtered out to obtain the tackifier.

[0023] Preferably, the aminosilane, epoxysilane and solid acid catalyst are mixed and then heated and stirred.

[0024] Preferably, the stirring temperature is 65-110° C., the stirring rate is 180-550 r / min, and the stirring time is 1.5-5.5 h.

[0025] Further preferably, the stirring temperature is 70-100° C., the stirring rate is 200-500 r / min, and the stirring time is 2-5 h.

[0026] Preferably, the mixing after adding the end-side hydrogenated silicone oil is carried out by stirring.

[0027] Preferably, the stirring rate is 90-330 r / min, and the stirring time is 2.5-6.5 h.

[0028] Further preferably, the stirring rate is 100-300 r / min, and the stirring time is 3-6 h.

[0029] Preferably, the solid acid catalyst is filtered out using a filter.

[0030] Preferably, after filtering out the solid acid catalyst, the temperature is increased and vacuum is drawn to obtain the viscosity increasing agent.

[0031] Preferably, stirring is performed while vacuuming.

[0032] Preferably, the heating temperature is 90-120° C.; the stirring rate is 45-110 r / min; and the stirring time is 0.4-2.0 h.

[0033] Further preferably, the heating temperature is 100-110° C.; the stirring rate is 50-100 r / min; and the stirring time is 0.5-1.5 h.

[0034] A third aspect of the present invention provides a two-component addition-type silicone rubber.

[0035] Specifically, a two-component addition-type silicone rubber includes a component A and a component B;

[0036] Wherein, component A comprises hydrogen-containing silicone oil, carbon black, and the tackifier according to any one of claims 1 to 5;

[0037] Component B includes a platinum catalyst and divinyltetramethyldisiloxane;

[0038] The component A and / or component B independently include vinyl silicone oil, dimethyl silicone oil, aluminum oxide and aluminum hydroxide.

[0039] Preferably, in parts by weight, the component A comprises 100 parts of vinyl silicone oil, 4-16 parts of dimethyl silicone oil, 4-16 parts of hydrogenated silicone oil, 180-440 parts of aluminum oxide, 70-220 parts of aluminum hydroxide, 0.4-1.6 parts of carbon black, and 5-20 parts of the tackifier described in the first aspect of the present invention;

[0040] The component B comprises 100 parts of vinyl silicone oil, 4-16 parts of dimethyl silicone oil, 180-440 parts of aluminum oxide, 45-165 parts of aluminum hydroxide, 0.4-2.2 parts of platinum catalyst, and 0.4-1.4 parts of divinyltetramethyldisiloxane.

[0041] Further preferably, the component A comprises, by weight, 100 parts of vinyl silicone oil, 5-15 parts of dimethyl silicone oil, 5-15 parts of hydrogenated silicone oil, 200-400 parts of aluminum oxide, 80-200 parts of aluminum hydroxide, 0.5-1.5 parts of carbon black, and 7-15 parts of the tackifier according to any one of claims 1 to 5;

[0042] The B component comprises 100 parts of vinyl silicone oil, 5-15 parts of dimethyl silicone oil, 200-400 parts of aluminum oxide, 50-150 parts of aluminum hydroxide, 0.5-2 parts of platinum catalyst, and 0.5-1.2 parts of divinyltetramethyldisiloxane.

[0043] Preferably, at 25°C, the viscosity of the vinyl silicone oil is 85-550 mPa·s; at 25°C, the viscosity of the dimethyl silicone oil is 70-90 mPa·s.

[0044] Further preferably, at 25°C, the viscosity of the vinyl silicone oil is 95-510 mPa·s; at 25°C, the viscosity of the dimethyl silicone oil is 75-85 mPa·s.

[0045] Preferably, the particle size of the aluminum oxide is 6-14 μm.

[0046] More preferably, the particle size of the aluminum oxide is 8-12 μm.

[0047] Preferably, the particle size of the aluminum hydroxide is 10-18 μm.

[0048] More preferably, the aluminum hydroxide has a particle size of 12-16 μm.

[0049] Preferably, the platinum content of the platinum catalyst is 4000-6000 ppm.

[0050] More preferably, the platinum content of the platinum catalyst is 4500-5500 ppm.

[0051] Specifically, the above viscosity and particle size are applicable to the corresponding raw materials in component A and component B.

[0052] The fourth aspect of the present invention provides a method for preparing the two-component addition-type silicone rubber described in the third aspect of the present invention.

[0053] Specifically, a method for preparing a two-component addition-type silicone rubber comprises the following steps:

[0054] (1) mixing the raw materials of component A to obtain the component A;

[0055] (2) The raw materials of component B are mixed to obtain the component B; the component A and the component B constitute the two-component addition-type silicone rubber.

[0056] Preferably, in step (1), vinyl silicone oil, dimethyl silicone oil, aluminum oxide, aluminum hydroxide and carbon black are first mixed, heated and stirred under vacuum conditions to obtain a mixture.

[0057] Preferably, the mixing is carried out by stirring, and the stirring time is 10-20 minutes.

[0058] More preferably, the stirring time is 12-18 min.

[0059] Preferably, the heating temperature is 110-130° C.; the vacuum degree of the vacuum condition is -0.090 to -0.099 MPa; and the stirring time under the vacuum condition is 1.0-2.0 h.

[0060] Further preferably, the heating temperature is 115-125° C.; the vacuum degree of the vacuum condition is -0.095 to -0.099 MPa; and the stirring time under the vacuum condition is 1.2 to 1.8 h.

[0061] Preferably, after the mixture is cooled, hydrogen-containing silicone oil and the tackifier described in the first aspect of the present invention are added, and the mixture is stirred under vacuum conditions to obtain the component A.

[0062] Preferably, cooling water is used for cooling.

[0063] Preferably, the vacuum degree of the vacuum condition is -0.090 to -0.099 MPa; and the stirring time under the vacuum condition is 20 to 40 min.

[0064] Further preferably, the vacuum degree of the vacuum condition is -0.095 to -0.099 MPa; and the stirring time under the vacuum condition is 25 to 35 min.

[0065] Preferably, in step (2), vinyl silicone oil, dimethyl silicone oil, aluminum oxide and aluminum hydroxide are first mixed, heated and stirred under vacuum conditions to obtain a mixture.

[0066] Preferably, the mixing is carried out by stirring, and the stirring time is 10-20 minutes.

[0067] More preferably, the stirring time is 12-18 min.

[0068] Preferably, the heating temperature is 110-130° C.; the vacuum degree of the vacuum condition is -0.090 to -0.099 MPa; and the stirring time under the vacuum condition is 1.0-2.0 h.

[0069] Further preferably, the heating temperature is 115-125° C.; the vacuum degree of the vacuum condition is -0.095 to -0.099 MPa; and the stirring time under the vacuum condition is 1.2 to 1.8 h.

[0070] Preferably, after cooling the mixture, a platinum catalyst and divinyltetramethyldisiloxane are added, and the mixture is stirred under vacuum conditions to obtain the B component.

[0071] Preferably, cooling water is used for cooling.

[0072] Preferably, the vacuum degree of the vacuum condition is -0.090 to -0.099 MPa; and the stirring time under the vacuum condition is 20 to 40 min.

[0073] Further preferably, the vacuum degree of the vacuum condition is -0.095 to -0.099 MPa; and the stirring time under the vacuum condition is 25 to 35 min.

[0074] Specifically, the component A and the component B are packaged separately and mixed in a mass ratio of 1:1 before use.

[0075] The fifth aspect of the present invention provides an application of the tackifier described in the first aspect of the present invention and / or the two-component addition-type silicone rubber described in the third aspect of the present invention in the field of electronic appliances.

[0076] Compared with the prior art, the technical solution provided by the present invention has the following beneficial effects:

[0077] (1) In the present invention, under the action of a solid acid catalyst, aminosilane and epoxysilane are bonded to the hydrogenated silicone oil molecules through the alkoxy groups in the molecules and the silicon-hydrogen bonds in the hydrogenated silicone oil; when the tackifier is applied to a two-component addition-type silicone rubber, during the curing process of the silicone rubber, the hydrogenated silicone oil with aminosilane and epoxysilane on the molecular chain participates in the curing reaction, and the amino and epoxy groups in the aminosilane and epoxysilane form hydrogen bonds or covalent bonds with the hydroxyl groups on the surface of the substrate, so that the substrate and the silicone rubber are well bonded, so that the silicone rubber has good bonding properties and can meet the sealing performance requirements of the product.

[0078] (2) The aminosilane, epoxysilane and hydrogen-containing silicone oil of the present invention are commonly used materials with low cost.

[0079] (3) The present invention connects aminosilane and epoxysilane to the molecular chain of hydrogen-containing silicone oil through chemical reaction, and utilizes the larger molecular structure of hydrogen-containing silicone oil to effectively shield the poisoning effect of nitrogen element in aminosilane on platinum catalyst in addition-type silicone rubber, thereby greatly improving the storage stability of addition-type silicone rubber.

[0080] (3) The catalyst of the present invention adopts a solid strong acid cation exchange resin, which belongs to heterogeneous catalysis in the system. After the reaction is completed, the solid catalyst can be filtered out by filtering through a filter and can be recycled, saving costs. DETAILED DESCRIPTION

[0081] In order to make the technical scheme of the present invention more clearly understood by those skilled in the art, the following embodiments are listed for illustration. It should be pointed out that the following embodiments do not limit the protection scope of the present invention.

[0082] Unless otherwise specified, the raw materials, reagents or devices used in the following examples can be obtained from conventional commercial sources or by existing known methods.

[0083] Example 1

[0084] A tackifier comprises 200 parts of end-side hydrogenated silicone oil with a viscosity of 30 mPa·s and a hydrogen content of 0.5 wt% at 23° C., 40 parts of 3-aminopropyltrimethoxysilane, 80 parts of γ-glycidyloxypropyltrimethoxysilane, and 5 parts of a strong acid cation exchange resin.

[0085] A method for preparing a tackifier comprises the following steps:

[0086] (1) 3-aminopropyltrimethoxysilane, γ-glycidyloxypropyltrimethoxysilane, and strong acid cation exchange resin were placed in a three-necked flask with a condensation reflux and heating device according to weight, the temperature was raised to 70° C., and the mixture was stirred at a rate of 200 r / min for 2 h; then, end-side hydrogenated silicone oil was added, and the mixture was stirred at a rate of 100 r / min for 3 h to obtain a mixture;

[0087] (2) Using a filter screen, filter out a strong acid cation exchange resin from the mixture obtained in step (1), raise the temperature to 100° C., evacuate, and stir at a rate of 50 r / min for 0.5 h. Cool and discharge the mixture to obtain a tackifier.

[0088] Example 2

[0089] A tackifier comprises 200 parts of end-side hydrogenated silicone oil with a viscosity of 40 mPa·s and a hydrogen content of 0.3 wt% at 23° C., 70 parts of 3-aminopropyltriethoxysilane, 100 parts of gamma-glycidyloxypropyltriethoxysilane, and 7 parts of a strong acid cation exchange resin.

[0090] A method for preparing a tackifier comprises the following steps:

[0091] (1) 3-aminopropyl triethoxysilane, γ-glycidyloxypropyl triethoxysilane, and a strong acid cation exchange resin were placed in a three-necked flask with a condensation reflux and heating device according to weight, the temperature was raised to 80° C., and the mixture was stirred at a rate of 300 r / min for 3 h; then, end-side hydrogenated silicone oil was added, and the mixture was stirred at a rate of 200 r / min for 4 h to obtain a mixture;

[0092] (2) Using a filter screen, filter out a strong acid cation exchange resin from the mixture obtained in step (1), raise the temperature to 100° C., evacuate, and stir at a rate of 60 r / min for 1 h, cool and discharge the mixture to obtain a tackifier.

[0093] Example 3

[0094] A tackifier comprises 200 parts of end-side hydrogenated silicone oil with a viscosity of 80 mPa·s and a hydrogen content of 0.18 wt% at 23° C., 50 parts of 3-aminopropylmethyldimethoxysilane, 80 parts of γ-glycidyloxypropyltriethoxysilane, and 10 parts of a strong acid cation exchange resin.

[0095] A method for preparing a tackifier comprises the following steps:

[0096] (1) 3-aminopropylmethyldimethoxysilane, γ-glycidyloxypropyltriethoxysilane, and strong acid cation exchange resin were placed in a three-necked flask with a condensation reflux and heating device according to weight, heated to 85° C., stirred at a rate of 300 r / min for 4 h; then, end-side hydrogenated silicone oil was added, stirred at a rate of 200 r / min for 5 h, and a mixture was obtained;

[0097] (2) Using a filter screen, filter out a strong acid cation exchange resin from the mixture obtained in step (1), raise the temperature to 110° C., evacuate, and stir at a rate of 80 r / min for 1.5 h. Cool and discharge the mixture to obtain a tackifier.

[0098] Example 4

[0099] A tackifier comprises 230 parts of end-side hydrogenated silicone oil with a viscosity of 80 mPa·s and a hydrogen content of 0.24 wt% at 23° C., 80 parts of N-cyclohexyl-3-aminopropylmethyldimethoxysilane, 60 parts of γ-glycidyloxypropyltriethoxysilane, and 9 parts of a strong acid cation exchange resin.

[0100] A method for preparing a tackifier comprises the following steps:

[0101] (1) According to weight parts, N-cyclohexyl-3-aminopropylmethyldimethoxysilane, γ-glycidyloxypropyltriethoxysilane, and strong acid cation exchange resin are placed in a three-necked flask with a condensation reflux and heating device, the temperature is raised to 90° C., and the mixture is stirred at a rate of 300 r / min for 5 h; then, the end-side hydrogenated silicone oil is added, and the mixture is stirred at a rate of 200 r / min for 4 h to obtain a mixture;

[0102] (2) Using a filter screen, filter out a strong acid cation exchange resin from the mixture obtained in step (1), raise the temperature to 100° C., evacuate, and stir at a rate of 100 r / min for 1 h, cool and discharge the mixture to obtain a tackifier.

[0103] Example 5

[0104] A tackifier comprises 240 parts of end-side hydrogenated silicone oil with a viscosity of 100 mPa·s and a hydrogen content of 0.1 wt% at 23° C., 80 parts of 3-(N-cyclohexylamino)propyltrimethoxysilane, 90 parts of 3-glycidyloxypropylmethyldiethoxysilane, and 9 parts of a strong acid cation exchange resin.

[0105] A method for preparing a tackifier comprises the following steps:

[0106] (1) 3-(N-cyclohexylamino)propyltrimethoxysilane, 3-glycidyloxypropylmethyldiethoxysilane, and a strong acid cation exchange resin were placed in a three-necked flask with a condensation reflux and heating device according to weight, heated to 90° C., and stirred at a rate of 300 r / min for 5 h; then, end-side hydrogenated silicone oil was added, stirred at a rate of 200 r / min for 4 h, and a mixture was obtained;

[0107] (2) Using a filter screen, filter out a strong acid cation exchange resin from the mixture obtained in step (1), raise the temperature to 105° C., evacuate, and stir at a rate of 90 r / min for 1.5 h. Cool and discharge the mixture to obtain a tackifier.

[0108] Application Example 1

[0109] A two-component addition-type silicone rubber, comprising component A and component B;

[0110] Wherein, component A includes 100 parts of vinyl silicone oil with a viscosity of 300 mPa·s at 25°C, 10 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 350 parts of aluminum oxide with a particle size of 10 μm, 100 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of carbon black, 12 parts of hydrogenated silicone oil and 7 parts of the tackifier of Example 1;

[0111] Component B includes 100 parts of vinyl silicone oil with a viscosity of 300 mPa·s at 25°C, 15 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 350 parts of aluminum oxide with a particle size of 10 μm, 90 parts of aluminum hydroxide with a particle size of 14 μm, 0.8 parts of a platinum catalyst with a platinum content of 5000 ppm, and 0.6 parts of divinyltetramethyldisiloxane.

[0112] A method for preparing a two-component addition-type silicone rubber comprises the following steps:

[0113] (1) According to weight, vinyl silicone oil, dimethyl silicone oil, aluminum oxide, aluminum hydroxide, and carbon black were placed in a planetary machine with a heating function, stirred for 15 minutes, shoveled, heated to 120° C., evacuated to a vacuum degree of -0.095 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water was passed to cool the mixture to 40° C., hydrogen silicone oil and the tackifier of Example 1 were added to the mixture, evacuated to a vacuum degree of -0.095 MPa, and stirred for 30 minutes to obtain component A;

[0114] (2) Vinyl silicone oil, dimethyl silicone oil, alumina and aluminum hydroxide are mixed by weight, stirred for 15 minutes, shoveled, heated to 120°C, evacuated to a vacuum degree of -0.095 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water is passed to cool the material to 40°C, platinum catalyst and vinyltetramethyldisiloxane are added to the mixture, and stirred for 30 minutes under a pressure condition of a vacuum degree of -0.095 MPa to obtain component B.

[0115] Application Example 2

[0116] A two-component addition-type silicone rubber, comprising component A and component B;

[0117] Wherein, component A includes 100 parts of vinyl silicone oil with a viscosity of 100 mPa·s at 25°C, 7 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 380 parts of aluminum oxide with a particle size of 10 μm, 150 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of carbon black, 14 parts of hydrogenated silicone oil and 8 parts of the tackifier of Example 2;

[0118] Component B includes 100 parts of vinyl silicone oil with a viscosity of 100 mPa·s at 25°C, 10 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 380 parts of aluminum oxide with a particle size of 10 μm, 90 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of a platinum catalyst with a platinum content of 5000 ppm, and 0.6 parts of divinyltetramethyldisiloxane.

[0119] A method for preparing a two-component addition-type silicone rubber comprises the following steps:

[0120] (1) According to weight, vinyl silicone oil, dimethyl silicone oil, aluminum oxide, aluminum hydroxide, and carbon black were placed in a planetary machine with a heating function, stirred for 15 minutes, shoveled, heated to 115° C., evacuated to a vacuum degree of -0.096 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water was passed to cool the mixture to 35° C., hydrogen-containing silicone oil and the tackifier of Example 2 were added to the mixture, evacuated to a vacuum degree of -0.096 MPa, and stirred for 30 minutes to obtain component A;

[0121] (2) Vinyl silicone oil, dimethyl silicone oil, alumina and aluminum hydroxide are mixed by weight, stirred for 15 minutes, shoveled, heated to 115°C, evacuated to a vacuum degree of -0.096 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water is passed to cool the mixture to 35°C, platinum catalyst and divinyltetramethyldisiloxane are added to the mixture, and stirred for 30 minutes under a pressure condition of a vacuum degree of -0.096 MPa to obtain component B.

[0122] Application Example 3

[0123] A two-component addition-type silicone rubber, comprising component A and component B;

[0124] Wherein, component A includes 100 parts of vinyl silicone oil with a viscosity of 500 mPa·s at 25°C, 12 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 250 parts of aluminum oxide with a particle size of 10 μm, 100 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of carbon black, 9 parts of hydrogenated silicone oil and 12 parts of the tackifier of Example 3;

[0125] Component B includes 100 parts of vinyl silicone oil with a viscosity of 100 mPa·s at 25°C, 10 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 380 parts of aluminum oxide with a particle size of 10 μm, 90 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of a platinum catalyst with a platinum content of 5000 ppm, and 0.6 parts of divinyltetramethyldisiloxane.

[0126] A method for preparing a two-component addition-type silicone rubber comprises the following steps:

[0127] (1) According to weight, vinyl silicone oil, dimethyl silicone oil, aluminum oxide, aluminum hydroxide, and carbon black were placed in a planetary machine with a heating function, stirred for 18 minutes, shoveled, heated to 125° C., evacuated to a vacuum degree of −0.095 MPa, and stirred for 2 hours to obtain a mixture; cooling water was passed to cool the mixture to 30° C., hydrogen-containing silicone oil and the tackifier of Example 3 were added to the mixture, evacuated to a vacuum degree of −0.095 MPa, and stirred for 35 minutes to obtain component A;

[0128] (2) Vinyl silicone oil, dimethyl silicone oil, alumina and aluminum hydroxide are mixed by weight, stirred for 18 minutes, shoveled, heated to 125°C, evacuated to a vacuum degree of -0.095 MPa, stirred for 2 hours, and a mixture is obtained; cooling water is passed to cool the mixture to 35°C, a platinum catalyst and divinyltetramethyldisiloxane are added to the mixture, and stirred for 35 minutes under a pressure condition of a vacuum degree of -0.095 MPa to obtain component B.

[0129] Application Example 4

[0130] A two-component addition-type silicone rubber, comprising component A and component B;

[0131] Wherein, component A includes 100 parts of vinyl silicone oil with a viscosity of 300 mPa·s at 25°C, 10 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 250 parts of aluminum oxide with a particle size of 10 μm, 100 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of carbon black, 9 parts of hydrogenated silicone oil and 13 parts of the tackifier of Example 4;

[0132] Component B includes 100 parts of vinyl silicone oil with a viscosity of 300 mPa·s at 25°C, 9 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 370 parts of aluminum oxide with a particle size of 10 μm, 85 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of a platinum catalyst with a platinum content of 5000 ppm, and 0.6 parts of divinyltetramethyldisiloxane.

[0133] A method for preparing a two-component addition-type silicone rubber comprises the following steps:

[0134] (1) According to weight, vinyl silicone oil, dimethyl silicone oil, aluminum oxide, aluminum hydroxide, and carbon black were placed in a planetary machine with a heating function, stirred for 15 minutes, shoveled, heated to 120° C., evacuated to a vacuum degree of -0.096 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water was passed to cool the mixture to 40° C., hydrogen-containing silicone oil and the tackifier of Example 4 were added to the mixture, evacuated to a vacuum degree of -0.096 MPa, and stirred for 30 minutes to obtain component A;

[0135] (2) Vinyl silicone oil, dimethyl silicone oil, alumina and aluminum hydroxide are mixed by weight, stirred for 15 minutes, shoveled, heated to 120°C, evacuated to a vacuum degree of -0.096 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water is passed to cool the mixture to 40°C, platinum catalyst and divinyltetramethyldisiloxane are added to the mixture, and stirred for 30 minutes under a pressure condition of a vacuum degree of -0.096 MPa to obtain component B.

[0136] Application Example 5

[0137] A two-component addition-type silicone rubber, comprising component A and component B;

[0138] Wherein, component A includes 100 parts of vinyl silicone oil with a viscosity of 300 mPa·s at 25°C, 10 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 280 parts of aluminum oxide with a particle size of 10 μm, 100 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of carbon black, 9 parts of hydrogenated silicone oil and 13 parts of the tackifier of Example 5;

[0139] Component B includes 100 parts of vinyl silicone oil with a viscosity of 300 mPa·s at 25°C, 9 parts of dimethyl silicone oil with a viscosity of 80 mPa·s at 25°C, 360 parts of aluminum oxide with a particle size of 10 μm, 90 parts of aluminum hydroxide with a particle size of 14 μm, 1 part of a platinum catalyst with a platinum content of 5000 ppm, and 0.6 parts of divinyltetramethyldisiloxane.

[0140] A method for preparing a two-component addition-type silicone rubber comprises the following steps:

[0141] (1) According to weight, vinyl silicone oil, dimethyl silicone oil, aluminum oxide, aluminum hydroxide, and carbon black were placed in a planetary machine with a heating function, stirred for 15 minutes, shoveled, heated to 115° C., evacuated to a vacuum degree of -0.095 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water was passed to cool the mixture to 40° C., hydrogen-containing silicone oil and the tackifier of Example 5 were added to the mixture, evacuated to a vacuum degree of -0.095 MPa, and stirred for 35 minutes to obtain component A;

[0142] (2) Vinyl silicone oil, dimethyl silicone oil, alumina and aluminum hydroxide are mixed by weight, stirred for 15 minutes, shoveled, heated to 115°C, evacuated to a vacuum degree of -0.095 MPa, and stirred for 1.5 hours to obtain a mixture; cooling water is passed to cool the mixture to 40°C, platinum catalyst and divinyltetramethyldisiloxane are added to the mixture, and stirred for 35 minutes under a pressure condition of a vacuum degree of -0.095 MPa to obtain component B.

[0143] Comparative Example 1

[0144] The difference between Comparative Example 1 and Example 1 is that Comparative Example 1 uses an equal amount of dodecyltrimethoxysilane to replace 3-aminopropyltrimethoxysilane, and the rest is the same as Example 1.

[0145] Comparative Example 2

[0146] The only difference between Comparative Example 2 and Example 2 is that Comparative Example 2 uses an equal amount of end-side hydrogenated silicone oil with a viscosity of 200 mPa·s and a hydrogen content of 0.8 wt% to replace the end-side hydrogenated silicone oil with a viscosity of 40 mPa·s and a hydrogen content of 0.3 wt%, and the rest is the same as Example 2.

[0147] Comparative Example 3

[0148] The difference between Comparative Example 3 and Application Example 1 is that the tackifier in component A of the two-component addition-type silicone rubber of Comparative Example 3 is the tackifier of Comparative Example 1, and the rest is the same as Application Example 1.

[0149] Comparative Example 4

[0150] The difference between Comparative Example 4 and Application Example 2 is that the tackifier in component A of the two-component addition-type silicone rubber of Comparative Example 4 is the tackifier of Comparative Example 2, and the rest is the same as Application Example 2.

[0151] Performance Testing

[0152] The viscosity of the tackifiers of Examples 1-5 and Comparative Examples 1-2 was tested according to GB / T 2794-2013. The test results are shown in Table 1:

[0153] Table 1

[0154]

[0155] It can be seen from Table 1 that the viscosity of the tackifier of Examples 1-5 is less than the viscosity of the tackifier of Comparative Examples 1-2.

[0156] Corresponding to Example 1-5, the two-component addition-type silicone rubber of Example 3-4 was subjected to performance test, and the test results are shown in Table 2, wherein the test items and test methods are as follows:

[0157] Viscosity: Tested according to GB / T 2794-2013.

[0158] Hardness: Mix component A and component B in a weight ratio of 1:1, pour into a mold with a length, width and depth of 4 cm, 4 cm and 0.8 cm respectively, bake at 80℃ for 30 minutes to form a solidified block, and test according to GB / T 531.1-2008.

[0159] Thermal conductivity: Mix component A and component B in a weight ratio of 1:1, pour into a mold with a diameter of 10 cm and a thickness of 1 mm, bake at 80°C for 30 minutes to form a cured sheet, and test according to ISO / DIS 22007.

[0160] Volume resistivity: Mix component A and component B in a weight ratio of 1:1, pour into a mold with a diameter of 10 cm and a thickness of 1 mm, bake at 80°C for 30 minutes to form a cured sheet, and test according to GB / T 1410-2006.

[0161] Shear strength: tested according to GB / T 13936-2014.

[0162] Failure type: When doing shear strength test, observe the colloid failure. If there is no glue residue on one side of the substrate, it is interfacial failure. If there is residual glue on the surfaces of the two substrates, it is cohesive failure.

[0163] Table 2

[0164]

[0165]

[0166] It can be seen from Table 2 that the shear strength of the two-component addition-type silicone rubber of Application Examples 1-5 is significantly greater than that of Comparative Examples 3 and 4, and the failure type of the two-component addition-type silicone rubber of Application Examples 1-5 is cohesive failure, while the failure type of the silicone rubber of Comparative Examples 3 and 4 is interface failure. This indicates that the bonding performance of the two-component addition-type silicone rubber of Application Examples 1-5 is significantly better than that of Comparative Examples 3 and 4.

[0167] Component A of the two-component addition-type silicone rubber of Comparative Example 3 includes the tackifier of Comparative Example 1, and the other components are the same as those of Application Example 1, that is, the aminosilane of the tackifier of Comparative Example 3 is dodecyltrimethoxysilane. As a result, the shear strength of the product of Comparative Example 3 is significantly worse than that of Application Example 1, indicating that the tackifier obtained by using the aminosilane of the present invention can make the two-component addition-type silicone rubber have good bonding properties.

[0168] Component A of the two-component addition-type silicone rubber of Comparative Example 4 includes the tackifier of Comparative Example 2, and the rest is the same as that of Application Example 2. As a result, the shear strength of the product of Comparative Example 4 is significantly worse than that of Application Example 2, indicating that only the tackifier obtained by using the hydrogen-containing silicone oil with a specific viscosity and hydrogen content of the present invention can make the two-component addition-type silicone rubber have good bonding properties.

[0169] The above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A tackifier, characterized in that The raw materials for preparing the tackifier include 180-270 parts of end-side hydrogenated silicone oil, 35-88 parts of aminosilane, 45-110 parts of epoxysilane, and 4-12 parts of solid acid catalyst; At 23° C., the viscosity of the end-side hydrogen-containing silicone oil is less than 200 mPa·s, and the hydrogen content of the end-side hydrogen-containing silicone oil is less than 0.8 wt %; The aminosilane is selected from at least one of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-aminopropylmethyldimethoxysilane, 3-aminopropylmethyldiethoxysilane, N-cyclohexyl-3-aminopropylmethyldimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, 3-(N-cyclohexylamino)propyltrimethoxysilane, N-(n-butyl)-3-aminopropyltriethoxysilane, N-(n-butyl)-3-aminopropyltrimethoxysilane and N,N-diethyl-3-aminopropyltrimethoxysilane; The epoxy silane is selected from at least one of γ-glycidyloxypropyl trimethoxysilane, γ-glycidyloxypropyl triethoxysilane, 3-glycidyloxypropyl methyl dimethoxysilane, and 3-glycidyloxypropyl methyl diethoxysilane; The solid acid catalyst is a strong acid cation exchange resin.

2. The method for preparing the tackifier according to claim 1, characterized in that: The following steps are involved: The various raw material components are mixed to prepare the viscosity enhancing agent.

3. The preparation method according to claim 2, characterized in that: The following steps are involved: The aminosilane, epoxysilane and solid acid catalyst are mixed, and then the end-side hydrogen-containing silicone oil is added and mixed, and the solid acid catalyst is filtered out to obtain the tackifier.

4. A silicone rubber, characterized in that: It includes component A and component B; Wherein, component A comprises hydrogen-containing silicone oil, carbon black, and the tackifier according to claim 1; Component B includes a platinum catalyst and divinyltetramethyldisiloxane; The component A and / or component B independently include vinyl silicone oil, dimethyl silicone oil, aluminum oxide and aluminum hydroxide.

5. The method for preparing silicone rubber according to claim 4, characterized in that: The following steps are involved: (1) mixing the raw materials of component A to obtain the component A; (2) The raw materials of component B are mixed to obtain the component B; the component A and the component B constitute the silicone rubber.

6. Use of the tackifier according to claim 1 and / or the silicone rubber according to claim 4 in the field of electronic appliances.

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