Room temperature curing phenyl silicone rubber and preparation method thereof

Abstract

The invention belongs to the technical field of silicone rubber, and particularly discloses room temperature curing phenyl silicone rubber, which is prepared from the following raw materials in parts by weight: 100 parts of silicone rubber, 20 to 40 parts of reinforcing filler, 5 to 10 parts of antibacterial material, 5 to 10 parts of heat conduction material and 0.5 to 2.0 parts of vulcanizing agent. According to the room-temperature curing phenyl silicone rubber provided by the invention, the heat-conducting filler and the antibacterial filler are added, and by preparing the composite heat-conducting filler and controlling the addition amount of the heat-conducting filler, the mechanical property of the phenyl silicone rubber is improved while the heat-conducting property of the phenyl silicone rubber is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of silicone rubber, and in particular relates to room temperature curing phenyl silicone rubber and a preparation method thereof. Background Art

[0002] Methylphenyl silicone rubber introduces phenyl groups on the side groups of polysiloxane, which destroys the regularity of the dimethylsiloxane structure and greatly reduces the crystallization temperature and glass transition temperature of the polymer. Therefore, in addition to the compression permanent deformation, wide operating temperature range, oxidation resistance, weather resistance, shock resistance, moisture resistance and good electrical insulation properties of silicone rubber, methylphenyl silicone rubber also has excellent low temperature resistance, ablation resistance and radiation resistance. Methylphenyl silicone rubber can maintain good physical properties and chemical stability in high temperature environments, so it is widely used in aerospace, automobile manufacturing, petrochemical and other fields.

[0003] In recent years, polymer-based thermally conductive composite materials have played an irreplaceable role in the heat dissipation design of electronic equipment. During the research process, different types of thermally conductive fillers are often used to fill the polymer matrix to improve the thermal conductivity of the thermally conductive composite materials. However, the filling of a large amount of thermally conductive fillers will also reduce the processing performance and mechanical properties of the polymer. Summary of the invention

[0004] The purpose of the present invention is to overcome the above problems existing in the prior art and provide a room temperature curing phenyl silicone rubber, which is added with a thermally conductive filler and an antibacterial filler. By preparing a composite thermally conductive filler and controlling the amount of thermally conductive filler added, the thermal conductivity of the phenyl silicone rubber is improved while its mechanical properties are improved.

[0005] In order to achieve the above technical objectives and the above technical effects, the present invention is implemented through the following technical solutions:

[0006] The embodiment of the first aspect of the present invention provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 20-40 parts of reinforcing filler, 5-10 parts of antibacterial material, 5-10 parts of thermal conductive material, and 0.5-2.0 parts of vulcanizing agent.

[0007] Furthermore, the silicone rubber is a phenyl silicone rubber rubber with a phenyl content of 15-25 mol% and a molecular weight of 450,000-800,000.

[0008] Furthermore, the reinforcing filler is fumed silica;

[0009] The vulcanizing agent is a dipentadienyl vulcanizing agent.

[0010] Furthermore, the preparation process of the antibacterial material is as follows:

[0011] S11: ultrasonically dispersing a zinc source in deionized water to prepare a zinc source solution;

[0012] S12: stirring the zinc source solution, adding alkali solution into the zinc source solution, stirring for 2-6 hours and then filtering to prepare zinc ammonia solution;

[0013] S13: adding aluminum oxide to the zinc ammonia solution and adding an appropriate amount of deionized water, distilling ammonia at 85-95° C. for 2-6 hours, cooling and aging for 0.5-2 hours, filtering, washing with water, and washing with ethanol to prepare a crude product;

[0014] S14: The crude product is dried at 100-120° C. for 0.5-2 h, and then placed in a muffle furnace and calcined at 300-500° C. for 1-4 h to prepare an antibacterial material.

[0015] Further, in step S11, the zinc source is zinc oxide or a zinc salt;

[0016] In the zinc source solution, the mass ratio of the zinc source to deionized water is 1:(5-10).

[0017] Further, in step S12, the alkali solution is any one or more of ammonia water and ammonium bicarbonate mixed in any proportion;

[0018] Wherein, the mass ratio of the zinc source to the alkali solution in the zinc source solution is 1:(2-10);

[0019] In step S13, the aluminum oxide is γ-type aluminum oxide;

[0020] Wherein, the mass ratio of the aluminum oxide to the zinc source in the zinc source solution in step S11 is (1-2):1.

[0021] Furthermore, the preparation process of the thermal conductive material is as follows:

[0022] S21: mixing nano zinc oxide and deionized water to prepare slurry A;

[0023] S22: Slurry A is mixed with titanium sulfate solution, and then urea solution and DBS solution are added respectively, and the mixture is stirred at high speed, reacted at 70-80° C. for 1-4 hours, and a reaction solution is prepared, and the temperature is raised to 90-100° C., and the reaction is continued for 1-4 hours, and a precipitate is obtained by filtration;

[0024] S23: drying the precipitate, and then calcining it in a muffle furnace at 400° C. for 1-4 h to prepare zinc oxide-coated titanium dioxide powder;

[0025] S24: Disperse the prepared zinc oxide-coated titanium dioxide powder in deionized water to prepare slurry B, add sodium bicarbonate solution to slurry B under high-speed stirring, and then drop aluminum sulfate solution. After the addition is completed, heat to 40-60°C and continue to react for 0.5-1h. Filter, wash, dry, grind and sieve the prepared precipitate, and then roast at 400-800°C for 1-2h to prepare a thermal conductive material.

[0026] Further, in step S22, the molar ratio of nano zinc oxide in slurry A, titanium sulfate in titanium sulfate solution, urea in urea solution and DBS in DBS solution is 1:(0.10-0.50):(2-6):(0.10-1.0);

[0027] In step S21, in slurry A, the mass ratio of nano zinc oxide to deionized water is 1:(5-10);

[0028] In step S24, the mass ratio of zinc oxide-coated titanium dioxide powder to deionized water is 1:(5-10);

[0029] The mass ratio of slurry B to sodium bicarbonate solution is 1:(2-4).

[0030] Furthermore, the mass ratio of the zinc oxide-coated titanium dioxide powder in slurry B to the aluminum sulfate in the aluminum sulfate solution is 1:(0.01-0.10).

[0031] The embodiment of the second aspect of the present invention provides a method for preparing room temperature curing phenyl silicone rubber, the method comprising the following steps:

[0032] S31: A double-roll rubber mixer is used for processing. First, the silicone rubber is added to the roller, and the double-roll rubber mixer is started. After the silicone rubber is wrapped around the roller, reinforcing fillers, antibacterial materials and thermal conductive materials are added one by one for mixing. After continuing to mix for 15-30 minutes, a thin pass is performed for 5-10 times to prepare a mixed rubber;

[0033] S32: heat treating the mixed rubber in an oven for 20-40 minutes, and re-refining after cooling;

[0034] S33: adding a vulcanizing agent to the re-mixed rubber, performing two-stage thin pass 5-10 times, rolling the sheet, molding it on a flat vulcanizer, and performing one-stage vulcanization for 20 minutes at 10 MPa and 160° C. to prepare a first-stage vulcanized rubber;

[0035] S34: Place the first stage vulcanized rubber in an oven and perform second stage vulcanization at 180°C for 2h to prepare phenyl silicone rubber.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] 1. The present invention provides a room temperature curing phenyl silicone rubber, which is added with a thermal conductive filler and an antibacterial filler. By preparing a composite thermal conductive filler and controlling the amount of the thermal conductive filler added, the thermal conductivity of the phenyl silicone rubber is improved while its mechanical properties are improved.

[0038] 2. In the present invention, the antibacterial material is prepared as a composite of aluminum oxide loaded with zinc oxide, that is, a zinc oxide film is covered on the surface of the aluminum oxide, and the antibacterial material is mixed with silicone rubber. The prepared phenyl silicone rubber has antibacterial properties, which broadens the scope of use of the phenyl silicone rubber.

[0039] 3. In the present invention, the thermally conductive material is prepared into a multi-layer core-shell structure. The multi-layer metal oxide structure not only has excellent thermal conductivity, but also has anti-corrosion, acid resistance, alkali resistance, antibacterial and other properties. The thermally conductive material is used to prepare phenyl silicone rubber, which can improve the overall thermal conductivity of the prepared phenyl silicone rubber, so that the prepared phenyl silicone rubber can be used in places requiring good heat dissipation performance.

[0040] 4. In the present invention, by adding self-made antibacterial materials and thermal conductive fillers during the preparation of phenyl silicone rubber, the mechanical properties and thermal conductivity of the prepared phenyl silicone rubber are further improved, and the prepared phenyl silicone rubber also has antibacterial properties. DETAILED DESCRIPTION

[0041] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0042] The embodiment of the first aspect of the present invention provides a room temperature curing phenyl silicone rubber, which comprises the following raw materials in parts by weight: 100 parts of silicone rubber, 20-40 parts of reinforcing filler, 5-10 parts of antibacterial material, 5-10 parts of thermal conductive material, and 0.5-2.0 parts of vulcanizing agent;

[0043] The silicone rubber is a phenyl silicone rubber with a phenyl content of 15-25 mol% and a molecular weight of 450,000-800,000.

[0044] The reinforcing filler is fumed silica;

[0045] The vulcanizing agent is dipentadienyl vulcanizing agent;

[0046] The preparation process of antibacterial materials is as follows:

[0047] S11: ultrasonically dispersing a zinc source in deionized water to prepare a zinc source solution; wherein the zinc source is zinc oxide or a zinc salt; and in the zinc source solution, the mass ratio of the zinc source to the deionized water is 1:(5-10);

[0048] S12: stirring the zinc source solution, adding alkali solution to the zinc source solution, continuing stirring for 2-6 hours and then filtering to prepare a zinc ammonia solution; wherein the alkali solution is any one or more of ammonia water and ammonium bicarbonate mixed in any proportion; the mass ratio of the zinc source in the zinc source solution to the alkali solution is 1:(2-10);

[0049] S13: adding alumina to the zinc ammonia solution and adding an appropriate amount of deionized water, distilling ammonia at 85-95° C. for 2-6 hours, cooling and aging for 0.5-2 hours, filtering, washing with water, and washing with ethanol to prepare a crude product; the alumina is γ-type alumina; the mass ratio of the alumina to the zinc source in the zinc source solution in step S11 is (1-2):1;

[0050] S14: drying the crude product at 100-120° C. for 0.5-2 h, and then calcining the crude product at 300-500° C. for 1-4 h in a muffle furnace to prepare an antibacterial material;

[0051] The antibacterial material is prepared by mixing the antibacterial material with silicone rubber, and the prepared antibacterial material is a composite of aluminum oxide loaded with zinc oxide, that is, a zinc oxide film is covered on the surface of the aluminum oxide. The antibacterial material is mixed with silicone rubber, and the prepared phenyl silicone rubber has antibacterial properties, which broadens the application range of the phenyl silicone rubber.

[0052] The preparation process of thermal conductive materials is as follows:

[0053] S21: mixing nano zinc oxide and deionized water to prepare slurry A; wherein the mass ratio of nano zinc oxide to deionized water in slurry A is 1:(5-10);

[0054] S22: Mix slurry A with titanium sulfate solution, then add urea solution and DBS solution respectively, stir at high speed to mix, react at 70-80°C for 1-4h, prepare reaction solution, heat to 90-100°C, continue to react for 1-4h, and filter to obtain precipitate; wherein the molar ratio of zinc oxide added in slurry A to titanium sulfate in titanium sulfate solution is (0.01-0.10):1; wherein the molar ratio of nano zinc oxide in slurry A, titanium sulfate in titanium sulfate solution, urea in urea solution and DBS in DBS solution is 1:(0.10-0.50):(2-6):(0.10-1.0);

[0055] S23: drying the precipitate, and then calcining it in a muffle furnace at 400° C. for 1-4 h to prepare zinc oxide-coated titanium dioxide powder;

[0056] S24: dispersing the prepared zinc oxide-coated titanium dioxide powder in deionized water to prepare slurry B, adding sodium bicarbonate solution to slurry B under high-speed stirring, and then dropping aluminum sulfate solution. After the dropping is completed, the temperature is raised to 40-60°C, and the reaction is continued for 0.5-1h. The prepared precipitate is filtered, washed, dried, ground, and sieved, and then roasted at 400-800°C for 1-2h to prepare a thermal conductive material; wherein, in step S24, the mass ratio of zinc oxide-coated titanium dioxide powder to deionized water is 1:(5-10); the mass ratio of slurry B to sodium bicarbonate solution is 1:(2-4);

[0057] Through the preparation of thermal conductive materials, the prepared thermal conductive material has a multi-layer core-shell structure; the use of this multi-layer metal oxide structure not only has excellent thermal conductivity, but also has anti-corrosion, acid resistance, alkali resistance, antibacterial and other properties; the thermal conductive material is used to prepare phenyl silicone rubber, which can improve the overall thermal conductivity of the prepared phenyl silicone rubber, so that the prepared phenyl silicone rubber can be used in places that require good heat dissipation performance.

[0058] The embodiment of the second aspect of the present invention provides a method for preparing a room temperature curing phenyl silicone rubber, wherein the formula is a room temperature curing phenyl silicone rubber formula provided by the embodiment of the first aspect of the present invention, and the method comprises the following steps:

[0059] S31: A double-roll rubber mixer is used for processing. First, the silicone rubber is added to the roller, and the double-roll rubber mixer is started. After the silicone rubber is wrapped around the roller, reinforcing fillers, antibacterial materials and thermal conductive materials are added one by one for mixing. After continuing to mix for 15-30 minutes, a thin pass is performed for 5-10 times to prepare a mixed rubber;

[0060] S32: heat treating the mixed rubber in an oven for 20-40 minutes, and re-refining after cooling;

[0061] S33: adding a vulcanizing agent to the re-mixed rubber, performing two-stage thin pass 5-10 times, rolling the sheet, molding it on a flat vulcanizer, and performing one-stage vulcanization for 20 minutes at 10 MPa and 160° C. to prepare a first-stage vulcanized rubber;

[0062] S34: Place the first stage vulcanized rubber in an oven and perform second stage vulcanization at 180°C for 2h to prepare phenyl silicone rubber.

[0063] The following are specific examples. Unless otherwise specified, all raw materials in the following examples can be obtained from commercial sources.

[0064] Example 1

[0065] The present embodiment provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 30 parts of reinforcing filler, 7 parts of antibacterial material, 7 parts of thermal conductive material, and 0.7 parts of vulcanizing agent.

[0066] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0067] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, namely, 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane.

[0068] Among them, the preparation process of antibacterial materials is as follows:

[0069] S11: ultrasonically dispersing a zinc source in deionized water to prepare a zinc source solution; wherein the zinc source is zinc oxide, and the mass ratio of zinc oxide to deionized water is 1:8;

[0070] S12: stirring the zinc source solution, adding alkali solution into the zinc source solution, stirring for 4 hours and then filtering to prepare zinc ammonia solution; the alkali solution is ammonia water; wherein the mass ratio of the zinc source in the zinc source solution to the alkali solution is 1:5;

[0071] S13: adding alumina to the zinc ammonia solution and adding an appropriate amount of deionized water, distilling ammonia at 90°C for 3 hours, cooling and aging for 1 hour, filtering, washing with water, and washing with ethanol to prepare a crude product; the alumina is γ-type alumina, and the mass ratio of the alumina to the zinc source in the zinc source solution in step S11 is 1.5:1;

[0072] S14: The crude product was dried at 105° C. for 1 h, and then placed in a muffle furnace and calcined at 400° C. for 2 h to prepare an antibacterial material.

[0073] Among them, the preparation process of thermal conductive materials is as follows:

[0074] S21: mixing nano zinc oxide and deionized water to prepare slurry A; wherein the mass ratio of nano zinc oxide to deionized water in slurry A is 1:7;

[0075] S22: Mix slurry A with titanium sulfate solution, then add urea solution and DBS solution respectively, stir and mix at high speed, react at 75°C for 2 hours, prepare reaction solution, heat to 95°C, continue to react for 2 hours, and filter to obtain precipitate; wherein the molar ratio of nano zinc oxide in slurry A, titanium sulfate in titanium sulfate solution, urea in urea solution and DBS in DBS solution is 1:0.3:4:0.2;

[0076] S23: drying the precipitate, and then calcining it in a muffle furnace at 400° C. for 2 h to prepare zinc oxide-coated titanium dioxide powder;

[0077] S24: The prepared zinc oxide coated titanium dioxide powder is dispersed in deionized water, the mass ratio of zinc oxide coated titanium dioxide powder to deionized water is 1:6, and slurry B is prepared. Under high-speed stirring, sodium bicarbonate solution is added to slurry B, the mass ratio of slurry B to sodium bicarbonate solution is 1:3, after the addition is completed, aluminum sulfate solution is added dropwise, after the addition is completed, the temperature is raised to 50°C, and the reaction is continued for 0.75h, the prepared precipitate is filtered, washed, dried, ground, sieved, and calcined at 600°C for 1.5h to prepare a thermal conductive material; wherein, the mass ratio of zinc oxide coated titanium dioxide powder in slurry B and aluminum sulfate in aluminum sulfate solution is 1:0.5.

[0078] This embodiment also provides a method for preparing room temperature curing phenyl silicone rubber, the preparation method comprising the following steps:

[0079] S31: A double-roll rubber mixer is used for processing. First, the silicone rubber is added to the roller, and the double-roll rubber mixer is started to wrap the silicone rubber around the roller. Then, reinforcing fillers, antibacterial materials, and thermal conductive materials are added one by one for mixing. After mixing for 20 minutes, the mixing is performed for 6 times to prepare a mixed rubber.

[0080] S32: heat treating the mixed rubber in an oven for 30 minutes, and then re-mixing after cooling;

[0081] S33: adding a vulcanizing agent to the re-mixed rubber, performing two-stage thin pass 6 times, rolling the sheet, molding on a flat vulcanizer, and performing one-stage vulcanization for 20 minutes at 10 MPa and 160° C. to prepare a first-stage vulcanized rubber;

[0082] S34: Place the first stage vulcanized rubber in an oven and perform second stage vulcanization at 180°C for 2h to prepare phenyl silicone rubber.

[0083] Example 2

[0084] The present embodiment provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 20 parts of reinforcing filler, 10 parts of antibacterial material, 10 parts of thermal conductive material, and 2.0 parts of vulcanizing agent.

[0085] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0086] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, namely, 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane.

[0087] Among them, the preparation process of antibacterial materials is as follows:

[0088] S11: ultrasonically dispersing a zinc source in deionized water to prepare a zinc source solution; wherein the zinc source is zinc oxide, and the mass ratio of zinc oxide to deionized water is 1:5;

[0089] S12: stirring the zinc source solution, adding alkali solution into the zinc source solution, stirring for 2 hours and then filtering to prepare zinc ammonia solution; the alkali solution is ammonia water; wherein the mass ratio of the zinc source in the zinc source solution to the alkali solution is 1:2;

[0090] S13: adding alumina to the zinc ammonia solution and adding an appropriate amount of deionized water, distilling ammonia at 85°C for 2h, cooling and aging for 0.5h, filtering, washing with water, and washing with ethanol to prepare a crude product; the alumina is γ-type alumina, and the mass ratio of the alumina to the zinc source in the zinc source solution in step S11 is 1:1;

[0091] S14: The crude product was dried at 100° C. for 0.5 h, and then placed in a muffle furnace and calcined at 300° C. for 4 h to prepare an antibacterial material.

[0092] Among them, the preparation process of thermal conductive materials is as follows:

[0093] S21: mixing nano zinc oxide and deionized water to prepare slurry A; wherein the mass ratio of nano zinc oxide to deionized water in slurry A is 1:5;

[0094] S22: Mix slurry A with titanium sulfate solution, then add urea solution and DBS solution respectively, stir and mix at high speed, react at 70°C for 1 hour, prepare reaction solution, heat to 90°C, continue to react for 1 hour, and filter to obtain precipitate; wherein the molar ratio of nano zinc oxide in slurry A, titanium sulfate in titanium sulfate solution, urea in urea solution and DBS in DBS solution is 1:0.10:6:1.0;

[0095] S23: drying the precipitate, and then calcining it in a muffle furnace at 400° C. for 1 h to prepare zinc oxide-coated titanium dioxide powder;

[0096] S24: The prepared zinc oxide coated titanium dioxide powder is dispersed in deionized water, the mass ratio of zinc oxide coated titanium dioxide powder to deionized water is 1:5, and slurry B is prepared. Under high-speed stirring, sodium bicarbonate solution is added to slurry B, the mass ratio of slurry B to sodium bicarbonate solution is 1:2, after the addition is completed, aluminum sulfate solution is added dropwise, after the addition is completed, the temperature is raised to 40°C, and the reaction is continued for 0.5h, the prepared precipitate is filtered, washed, dried, ground, sieved, and calcined at 400°C for 1h to prepare a thermal conductive material; wherein, the mass ratio of zinc oxide coated titanium dioxide powder in slurry B and aluminum sulfate in aluminum sulfate solution is 1:0.01.

[0097] This embodiment also provides a method for preparing room temperature curing phenyl silicone rubber, the preparation method comprising the following steps:

[0098] S31: A double-roll rubber mixer is used for processing. First, the silicone rubber is added to the roller, and the double-roll rubber mixer is started to coat the roller with the silicone rubber. Then, reinforcing fillers, antibacterial materials, and thermal conductive materials are added one by one for mixing. After mixing for 15 minutes, the mixing is performed for 5 times to prepare a mixed rubber.

[0099] S32: heat treating the mixed rubber in an oven for 20 minutes, and then re-mixing after cooling;

[0100] S33: adding a vulcanizing agent to the re-mixed rubber, performing two-stage thin pass 5 times, rolling the sheet, molding on a flat vulcanizer, and performing one-stage vulcanization for 20 minutes at 10 MPa and 160° C. to prepare a first-stage vulcanized rubber;

[0101] S34: Place the first stage vulcanized rubber in an oven and perform second stage vulcanization at 180°C for 2h to prepare phenyl silicone rubber.

[0102] Example 3

[0103] The present embodiment provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 40 parts of reinforcing filler, 5 parts of antibacterial material, 5 parts of thermal conductive material, and 0.5 parts of vulcanizing agent.

[0104] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0105] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, namely, 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane.

[0106] Among them, the preparation process of antibacterial materials is as follows:

[0107] S11: ultrasonically dispersing a zinc source in deionized water to prepare a zinc source solution; wherein the zinc source is zinc oxide, and the mass ratio of zinc oxide to deionized water is 1:10;

[0108] S12: stirring the zinc source solution, adding alkali solution into the zinc source solution, stirring for 6 hours and then filtering to prepare zinc ammonia solution; the alkali solution is ammonia water; wherein the mass ratio of the zinc source in the zinc source solution to the alkali solution is 1:10;

[0109] S13: adding alumina to the zinc ammonia solution and adding an appropriate amount of deionized water, distilling ammonia at 95°C for 6 hours, cooling and aging for 2 hours, filtering, washing with water, and washing with ethanol to prepare a crude product; the alumina is γ-type alumina, and the mass ratio of the alumina to the zinc source in the zinc source solution in step S11 is 2:1;

[0110] S14: The crude product was dried at 120° C. for 2 h, and then placed in a muffle furnace and calcined at 500° C. for 1 h to prepare an antibacterial material.

[0111] Among them, the preparation process of thermal conductive materials is as follows:

[0112] S21: mixing nano zinc oxide and deionized water to prepare slurry A; wherein the mass ratio of nano zinc oxide to deionized water in slurry A is 1:10;

[0113] S22: Mix slurry A with titanium sulfate solution, then add urea solution and DBS solution respectively, stir and mix at high speed, react at 80°C for 4 hours, prepare reaction solution, heat to 100°C, continue to react for 4 hours, and filter to obtain precipitate; wherein the molar ratio of nano zinc oxide in slurry A, titanium sulfate in titanium sulfate solution, urea in urea solution and DBS in DBS solution is 1:0.50:2:0.10;

[0114] S23: drying the precipitate, and then calcining it in a muffle furnace at 400° C. for 4 h to prepare zinc oxide-coated titanium dioxide powder;

[0115] S24: The prepared zinc oxide coated titanium dioxide powder is dispersed in deionized water, the mass ratio of zinc oxide coated titanium dioxide powder to deionized water is 1:10, and slurry B is prepared. Under high-speed stirring, sodium bicarbonate solution is added to slurry B, the mass ratio of slurry B to sodium bicarbonate solution is 1:4, after the addition is completed, aluminum sulfate solution is added dropwise, after the addition is completed, the temperature is raised to 60°C, and the reaction is continued for 1 hour, the prepared precipitate is filtered, washed, dried, ground, sieved, and then calcined at 800°C for 2 hours to prepare a thermal conductive material; wherein, the mass ratio of zinc oxide coated titanium dioxide powder in slurry B and aluminum sulfate in aluminum sulfate solution is 1:0.10.

[0116] This embodiment also provides a method for preparing room temperature curing phenyl silicone rubber, the preparation method comprising the following steps:

[0117] S31: A double-roll rubber mixer is used for processing. First, the silicone rubber is added to the roller, and the double-roll rubber mixer is started. After the silicone rubber is wrapped around the roller, reinforcing fillers, antibacterial materials and thermal conductive materials are added one by one for mixing. After continuing to mix for 30 minutes, the rubber mixer is thinly passed 10 times to prepare a mixed rubber.

[0118] S32: heat treating the mixed rubber in an oven for 40 minutes, and re-mixing after cooling;

[0119] S33: adding a vulcanizing agent to the re-mixed rubber, performing two-stage thin pass 10 times, rolling the sheet, molding it on a flat vulcanizer, and performing one-stage vulcanization for 20 minutes at 10 MPa and 160° C. to prepare a first-stage vulcanized rubber;

[0120] S34: Place the first stage vulcanized rubber in an oven and perform second stage vulcanization at 180°C for 2h to prepare phenyl silicone rubber.

[0121] Example 4

[0122] The present embodiment provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 20 parts of reinforcing filler, 10 parts of antibacterial material, 10 parts of thermal conductive material, and 2.0 parts of vulcanizing agent.

[0123] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0124] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, i.e., 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane;

[0125] The preparation of the antibacterial material and the thermal conductive material are both carried out using the preparation process of the antibacterial material provided in Example 1.

[0126] This embodiment also provides a method for preparing room temperature curing phenyl silicone rubber, and the preparation method is carried out using the method for preparing room temperature curing phenyl silicone rubber provided in Example 1.

[0127] Example 5

[0128] The present embodiment provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 40 parts of reinforcing filler, 5 parts of antibacterial material, 5 parts of thermal conductive material, and 0.5 parts of vulcanizing agent.

[0129] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0130] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, i.e., 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane;

[0131] The preparation of the antibacterial material and the thermal conductive material are both carried out using the preparation process of the antibacterial material provided in Example 1.

[0132] This embodiment also provides a method for preparing room temperature curing phenyl silicone rubber, and the preparation method is carried out using the method for preparing room temperature curing phenyl silicone rubber provided in Example 1.

[0133] Comparative Example 1

[0134] This comparative example provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 30 parts of reinforcing filler, and 0.7 parts of vulcanizing agent.

[0135] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0136] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, i.e., 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane;

[0137] Compared with Example 1, no antibacterial material and thermal conductive material are added in this comparative example.

[0138] This comparative example also provides a method for preparing room temperature curing phenyl silicone rubber, and the preparation method is carried out using the method for preparing room temperature curing phenyl silicone rubber provided in Example 1.

[0139] Comparative Example 2

[0140] This comparative example provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 30 parts of reinforcing filler, 7 parts of antibacterial material, and 0.7 parts of vulcanizing agent.

[0141] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0142] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, i.e., 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane;

[0143] Compared with Example 1, no thermal conductive material is added in this comparative example.

[0144] This comparative example also provides a method for preparing room temperature curing phenyl silicone rubber, and the preparation method is carried out using the method for preparing room temperature curing phenyl silicone rubber provided in Example 1.

[0145] Comparative Example 3

[0146] This comparative example provides a room temperature curing phenyl silicone rubber, which includes the following raw materials in parts by weight: 100 parts of silicone rubber, 30 parts of reinforcing filler, 7 parts of thermal conductive material, and 0.7 parts of vulcanizing agent.

[0147] Among them, the phenyl content of the silicone rubber is 25 mol%, and the molecular weight is 800,000;

[0148] The reinforcing filler is fumed silica; the vulcanizing agent is a dipentadienyl vulcanizing agent, i.e., 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane;

[0149] Compared with Example 1, no antibacterial material is added in this comparative example.

[0150] This comparative example also provides a method for preparing room temperature curing phenyl silicone rubber, and the preparation method is carried out using the method for preparing room temperature curing phenyl silicone rubber provided in Example 1.

[0151] Experimental example

[0152] The performance tests were performed on the phenyl silicone rubbers prepared in Examples 1-5 and Comparative Examples 1-3. The test results are shown in Table 1.

[0153] Among them, the hardness test is carried out in accordance with GB / T531.1-2008.

[0154] The tensile strength and elongation at break are measured in accordance with GB / T528-2009;

[0155] The tear strength is measured in accordance with GB / T12829-2006.

[0156] Table 1

[0157]

[0158] It can be seen from the data in Table 1 that after adding antibacterial materials and thermal conductive fillers to the phenyl silicone rubber, its mechanical properties did not decrease, but were improved compared with the control example, indicating that the phenyl silicone rubber prepared in the present application has thermal conductivity and antibacterial properties, while its mechanical properties are also enhanced.

[0159] The present invention provides a room temperature curing phenyl silicone rubber and a preparation method thereof. During the preparation of the phenyl silicone rubber, a self-made antibacterial material and a thermal conductive filler are added to further improve the mechanical properties and thermal conductivity of the prepared phenyl silicone rubber, and the prepared phenyl silicone rubber also has antibacterial properties.

[0160] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0161] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.

Claims

1. A room temperature curing phenyl silicone rubber, characterized in that: The raw materials include the following parts by weight: 100 parts of silicone rubber, 20-40 parts of reinforcing filler, 5-10 parts of antibacterial material, 5-10 parts of thermal conductive material, and 0.5-2.0 parts of vulcanizing agent.

2. A room temperature curing phenyl silicone rubber according to claim 1, characterized in that: The silicone rubber is a phenyl silicone rubber rubber with a phenyl content of 15-25 mol% and a molecular weight of 450,000-800,000.

3. A room temperature curing phenyl silicone rubber according to claim 1, characterized in that: The reinforcing filler is fumed silica; The vulcanizing agent is a dipentadienyl vulcanizing agent.

4. The room temperature curing phenyl silicone rubber according to claim 1, characterized in that: The preparation process of the antibacterial material is as follows: S11: ultrasonically dispersing a zinc source in deionized water to prepare a zinc source solution; S12: stirring the zinc source solution, adding alkali solution into the zinc source solution, stirring for 2-6 hours and then filtering to prepare zinc ammonia solution; S13: adding aluminum oxide to the zinc ammonia solution and adding an appropriate amount of deionized water, distilling ammonia at 85-95° C. for 2-6 hours, cooling and aging for 0.5-2 hours, filtering, washing with water, and washing with ethanol to prepare a crude product; S14: The crude product is dried at 100-120° C. for 0.5-2 h, and then placed in a muffle furnace and calcined at 300-500° C. for 1-4 h to prepare an antibacterial material.

5. A room temperature curing phenyl silicone rubber according to claim 4, characterized in that: In step S11, the zinc source is zinc oxide or a zinc salt; In the zinc source solution, the mass ratio of the zinc source to deionized water is 1:(5-10).

6. A room temperature curing phenyl silicone rubber according to claim 4, characterized in that: In step S12, the alkali solution is any one or more of ammonia water and ammonium bicarbonate mixed in any proportion; Wherein, the mass ratio of the zinc source to the alkali solution in the zinc source solution is 1:(2-10); In step S13, the aluminum oxide is γ-type aluminum oxide; Wherein, the mass ratio of the aluminum oxide to the zinc source in the zinc source solution in step S11 is (1-2):

1.

7. The room temperature curing phenyl silicone rubber according to claim 1, characterized in that: The preparation process of the thermal conductive material is as follows: S21: mixing nano zinc oxide and deionized water to prepare slurry A; S22: Slurry A is mixed with titanium sulfate solution, and then urea solution and DBS solution are added respectively, and the mixture is stirred at high speed, reacted at 70-80° C. for 1-4 hours, and a reaction solution is prepared, and the temperature is raised to 90-100° C., and the reaction is continued for 1-4 hours, and a precipitate is obtained by filtration; S23: drying the precipitate, and then calcining it in a muffle furnace at 400° C. for 1-4 h to prepare zinc oxide-coated titanium dioxide powder; S24: Disperse the prepared zinc oxide-coated titanium dioxide powder in deionized water to prepare slurry B, add sodium bicarbonate solution to slurry B under high-speed stirring, and then drop aluminum sulfate solution. After the addition is completed, heat to 40-60°C and continue to react for 0.5-1h. Filter, wash, dry, grind and sieve the prepared precipitate, and then roast at 400-800°C for 1-2h to prepare a thermal conductive material.

8. The room temperature curing phenyl silicone rubber according to claim 7, characterized in that: In step S22, the molar ratio of nano zinc oxide in slurry A, titanium sulfate in titanium sulfate solution, urea in urea solution and DBS in DBS solution is 1:(0.10-0.50):(2-6):(0.10-1.0); In step S21, in slurry A, the mass ratio of nano zinc oxide to deionized water is 1:(5-10); In step S24, the mass ratio of zinc oxide-coated titanium dioxide powder to deionized water is 1:(5-10); The mass ratio of slurry B to sodium bicarbonate solution is 1:(2-4).

9. The room temperature curing phenyl silicone rubber according to claim 7, characterized in that: The mass ratio of the zinc oxide-coated titanium dioxide powder in slurry B to the aluminum sulfate in the aluminum sulfate solution is 1:(0.01-0.10).

10. A method for preparing the room temperature curing phenyl silicone rubber according to any one of claims 1 to 9, characterized in that: The method comprises the following steps: S31: A double-roll rubber mixer is used for processing. First, the silicone rubber is added to the roller, and the double-roll rubber mixer is started. After the silicone rubber is wrapped around the roller, reinforcing fillers, antibacterial materials and thermal conductive materials are added one by one for mixing. After continuing to mix for 15-30 minutes, a thin pass is performed for 5-10 times to prepare a mixed rubber; S32: heat treating the mixed rubber in an oven for 20-40 minutes, and re-refining after cooling; S33: adding a vulcanizing agent to the re-mixed rubber, performing two-stage thin pass 5-10 times, rolling the sheet, molding it on a flat vulcanizer, and performing one-stage vulcanization for 20 minutes at 10 MPa and 160° C. to prepare a first-stage vulcanized rubber; S34: Place the first stage vulcanized rubber in an oven and perform second stage vulcanization at 180°C for 2h to prepare phenyl silicone rubber.

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