CN114874630B - High-magnification platinum hot vulcanization foaming silicone rubber and preparation method thereof - Google Patents
High-magnification platinum hot vulcanization foaming silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of silicone rubber foaming, and in particular relates to high-rate platinum hot vulcanization foaming silicone rubber and a preparation method thereof, wherein the mass ratio of the high-rate platinum hot vulcanization foaming silicone rubber is as follows: 100-110 parts of methyl vinyl silicone rubber raw rubber, 40-50 parts of reinforcing agent, 0.1-2 parts of vinyl content regulator, 0.3-0.5 part of hydrogen-containing silicone oil, 0.1-0.3 part of zinc stearate, 4-6 parts of hydroxyl silicone oil, 0.1-0.6 part of auxiliary foaming agent, 2-4 parts of foaming agent, 0.1-0.5 part of catalyst and 0.05-0.3 part of inhibitor; the foaming agent is compounded by adopting a thermosensitive foaming agent and a microsphere foaming agent, the auxiliary foaming agent is propanol, the catalyst is a platinum catalyst, and a corresponding preparation method is provided. The invention solves the defects of the prior foaming silicone rubber material, forms a high-rate foaming structure by utilizing the synergistic cooperation of the composite foaming agent and the auxiliary foaming agent, and has strong structural controllability.
Description
Technical Field
The invention belongs to the field of silicone rubber foaming, and particularly relates to high-magnification platinum hot vulcanization foaming silicone rubber and a preparation method thereof.
Background
The silicone rubber has excellent high and low temperature resistance, weather resistance, waterproof performance, chemical corrosion resistance, electrical insulation performance, adhesive performance, flame retardant performance, biocompatibility and physiological inertia, and is often applied to various fields of life of people and various industries of national economy, such as aerospace, aviation, automobiles, roads and bridges, building doors and windows, power environmental protection, electronic appliances, medical health, new energy and the like. The number and variety of applications of silicone rubber products are continuously increasing, and market potential is continuously developed. Foam silicone rubber is used as one of special purposes of the organic silicone rubber, and has the characteristics of excellent performance of the organic silicone rubber and foam materials. However, the traditional foaming silicon rubber has pollution and low foaming rate and cannot be applied to related industries.
The application field of the foam silicone rubber material in the future will be wider and wider, and the traditional silicone rubber foaming generally adopts halogen-containing peroxide (2, 4-dichloro benzoyl peroxide) as a vulcanizing agent, so that the foaming rate is high, the reaction is controllable, and the pollution is serious. The other uses platinum catalyst, and adds heat sensitive foaming agent or microsphere foaming agent. The thermosensitive foaming agent belongs to decomposition foaming, and has the advantages of large foaming pore, low mechanical property, high shrinkage rate, severe reaction and difficult control. The microsphere foaming agent has small foaming pores, low foaming multiplying power and uneven surface. Therefore, the foaming silicon rubber material is expected to have the development of high multiplying power, controllable structure, low compression permanent deformation rate, environmental protection and the like, and is a problem to be solved in the field.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the high-rate platinum hot vulcanization foaming silicone rubber, which solves the defects of the existing foaming silicone rubber material, and forms a high-rate foaming structure by utilizing the synergistic cooperation of the composite foaming agent and the auxiliary foaming agent, and has strong structural controllability.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a high-rate platinum heat vulcanization foaming silicone rubber comprises the following components in parts by mass:
100-110 parts of methyl vinyl silicone rubber raw rubber, 40-50 parts of reinforcing agent, 0.1-2 parts of vinyl content regulator, 0.3-0.5 part of hydrogen-containing silicone oil, 0.1-0.3 part of zinc stearate, 4-6 parts of hydroxyl silicone oil, 0.1-0.6 part of auxiliary foaming agent, 2-4 parts of foaming agent, 0.1-0.5 part of catalyst and 0.05-0.3 part of inhibitor; the foaming agent is compounded by adopting a thermosensitive foaming agent and a microsphere foaming agent, the auxiliary foaming agent is propanol, and the catalyst is a platinum catalyst; the inhibitor adopts ethynyl cyclohexanol.
The foaming agent is compounded by adopting a thermosensitive foaming agent E and a microsphere foaming agent F; the decomposition temperature of the thermosensitive foaming agent E is 130-160 ℃, and the gas generation amount is 160mL/g; the particle size of the microsphere foaming agent F is 20-30 mu m at normal temperature, the decomposition temperature is 100-140 ℃, and the gas generation amount is 140mL/g; the heat-sensitive foaming agent is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is foamed by a closed pore at a certain temperature, the heat-sensitive foaming agent is foamed by an open pore, the microsphere foaming agent is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer which is taken as a shell, and spheres of potassium bicarbonate and isopentane are wrapped in the microsphere foaming agent, so that the auxiliary foaming further reduces the density of the sizing material, and the sizing material has better mechanical properties. Wherein, the auxiliary foaming agent is matched with platinum to generate hydrogen auxiliary foaming, and the mechanism is as follows:
the methyl vinyl silicone rubber raw rubber is formed by methyl vinyl silicone rubber raw rubber A and methyl vinyl silicone rubber raw rubber B, wherein the vinyl content of the methyl vinyl silicone rubber raw rubber A is 0.050-0.053%, and the molecular weight is 61 ten thousand-63 ten thousand; the vinyl content of the methyl vinyl silicone rubber raw rubber B is 0.160-0.162%, and the molecular weight is 62-64 ten thousand.
The vinyl content regulator is one of high-ethylene raw silicone rubber C, vinyl trimethoxy silane and polyvinyl hydroxyl silicone oil, wherein the vinyl content of the high-ethylene raw silicone rubber C is 3.00-3.10%, and the molecular weight is 50-55 ten thousand; the weight percent of vinyl trimethoxy silane is 99.9; viscosity of polyvinyl hydroxyl silicone oil (25 ℃ C.) mm 2 S is less than or equal to 40, hydroxyThe base content is as follows: more than or equal to 5.5 percent, vinyl content: 5.5-6.5%; the vulcanized rubber with different vinyl contents and molecular weights and the vinyl content regulator added into the raw rubber with different crosslinking densities can be debugged, the speed is different in the vulcanization process, and the excellent proper foaming curing speed of the rubber material and the catalyst can be ensured, so that the synergistic improvement of the mechanical property and the foaming multiplying power is achieved.
The reinforcing agent adopts precipitated white carbon black, and the specific surface area of the precipitated white carbon black is 180-210m 2 /g。
The preparation method of the silicone rubber comprises the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the defects of the prior foaming silicone rubber material, forms a high-rate foaming structure by utilizing the synergistic cooperation of the composite foaming agent and the auxiliary foaming agent, and has strong structural controllability; meanwhile, the system has better appearance and elasticity, ensures the tightness of equipment, has bright color, and can be used in the field of toys.
2. The invention utilizes the vinyl content regulator to effectively control the vinyl content by being matched with methyl vinyl silicone rubber raw rubber and to form stable curing reaction by being matched with platinum catalyst, and simultaneously effectively controls the reaction efficiency; meanwhile, the activity of the reaction is controlled by the contents of vinyl, hydrogen and platinum catalyst, so that the surface gloss of the silica gel is smooth.
3. The invention has low cost and strong industrial mass production feasibility.
Detailed Description
The invention is described in detail with reference to examples, but without any limitation to the claims of the invention.
Example 1
High-magnification platinum hot vulcanization foaming silicone rubber material
The mass ratio is as follows: 60 parts of methyl vinyl silicone rubber raw rubber A, 40 parts of methyl vinyl silicone rubber raw rubber B, 2 parts of methyl vinyl silicone rubber raw rubber C, 45 parts of reinforcing agent, 0.5 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate, 6 parts of hydroxyl silicone oil, 0.2 part of auxiliary foaming agent, 3 parts of foaming agent, 0.1 part of catalyst and 0.2 part of inhibitor, wherein the foaming agent is a mixture of foaming agent E and F, the mass ratio is 1:1, the reinforcing agent is precipitated white carbon black, the auxiliary foaming agent is propanol, the catalyst is platinum catalyst, the inhibitor adopts ethynyl cyclohexanol, the heat-sensitive foaming agent E is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is a sphere which is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer, and the interior of the sphere wraps potassium bicarbonate and isopentane.
A high-rate platinum hot vulcanization foaming silicone rubber and a product method thereof comprise the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
Example 2
A high-magnification platinum heat vulcanization foaming silicon rubber material,
the mass ratio is as follows: 60 parts of methyl vinyl silicone rubber raw rubber A, 40 parts of methyl vinyl silicone rubber raw rubber B, 0.2 part of vinyl trimethoxy silane, 42 parts of reinforcing agent, 0.5 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate, 5.7 parts of hydroxyl silicone oil, 0.2 part of auxiliary foaming agent, 3 parts of foaming agent and 0.1 part of catalyst, and 0.2 part of inhibitor, wherein the foaming agent is a mixture of foaming agent E and F, the mass ratio is 1:1, the reinforcing agent is precipitated white carbon black, the auxiliary foaming agent is propanol, the catalyst is platinum catalyst, the inhibitor adopts ethynyl cyclohexanol, the heat-sensitive foaming agent E is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is a sphere which is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer, and the interior of the sphere wraps potassium bicarbonate and isopentane.
A high-rate platinum hot vulcanization foaming silicone rubber and a product method thereof comprise the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
Example 3
A high-magnification platinum heat vulcanization foaming silicon rubber material,
the mass ratio is as follows: 60 parts of methyl vinyl silicone rubber raw rubber A, 40 parts of methyl vinyl silicone rubber raw rubber B, 0.6 part of polyvinyl hydroxyl silicone oil, 44 parts of reinforcing agent, 0.5 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate, 5.6 parts of hydroxyl silicone oil, 0.2 part of auxiliary foaming agent, 3 parts of foaming agent and 0.1 part of catalyst, and 0.2 part of inhibitor, wherein the foaming agent is a mixture of foaming agent E and F, the mass ratio is 1:1, the reinforcing agent is precipitated white carbon black, the auxiliary foaming agent is propanol, the catalyst is platinum catalyst, the inhibitor adopts ethynyl cyclohexanol, the heat-sensitive foaming agent E is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is a sphere which is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer, and the interior of the sphere wraps potassium bicarbonate and isopentane.
A high-rate platinum hot vulcanization foaming silicone rubber and a product method thereof comprise the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
Example 4
A high-magnification platinum heat vulcanization foaming silicon rubber material,
the mass ratio is as follows: 60 parts of methyl vinyl silicone rubber raw rubber A, 40 parts of methyl vinyl silicone rubber raw rubber B, 0.6 part of polyvinyl hydroxyl silicone oil, 44 parts of reinforcing agent, 0.5 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate, 5.6 parts of hydroxyl silicone oil, 0.2 part of auxiliary foaming agent, 3 parts of foaming agent and 0.1 part of catalyst, and 0.2 part of inhibitor, wherein the foaming agent is a mixture of foaming agent E and F, the mass ratio is 1:2, the reinforcing agent is precipitated white carbon black, the auxiliary foaming agent is propanol, the catalyst is platinum catalyst, the inhibitor adopts ethynyl cyclohexanol, the heat-sensitive foaming agent E is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is a sphere which is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer, and the interior of the sphere wraps potassium bicarbonate and isopentane.
A high-rate platinum hot vulcanization foaming silicone rubber and a product method thereof comprise the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
Example 5
A high-magnification platinum heat vulcanization foaming silicon rubber material,
the mass ratio is as follows: 60 parts of methyl vinyl silicone rubber raw rubber A, 40 parts of methyl vinyl silicone rubber raw rubber B, 0.6 part of polyvinyl hydroxyl silicone oil, 44 parts of reinforcing agent, 0.5 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate, 5.6 parts of hydroxyl silicone oil, 0.20 part of auxiliary foaming agent, 3.2 parts of foaming agent, 0.1 part of catalyst and 0.2 part of inhibitor, wherein the foaming agent is a mixture of foaming agent E and F, the mass ratio is 1:3, the reinforcing agent is precipitated white carbon black, the auxiliary foaming agent is propanol, the catalyst is platinum catalyst, the inhibitor adopts ethynyl cyclohexanol, the heat-sensitive foaming agent E is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is a sphere which is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer, and the inside of the sphere wraps potassium bicarbonate and isopentane.
A high-rate platinum hot vulcanization foaming silicone rubber and a product method thereof comprise the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
Example 6
A high-magnification platinum heat vulcanization foaming silicon rubber material,
the mass ratio is as follows: 60 parts of methyl vinyl silicone rubber raw rubber A, 40 parts of methyl vinyl silicone rubber raw rubber B, 0.6 part of polyvinyl hydroxyl silicone oil, 44 parts of reinforcing agent, 0.5 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate, 5.6 parts of hydroxyl silicone oil, 0.4 part of auxiliary foaming agent, 3 parts of foaming agent, 0.1 part of catalyst and 0.2 part of inhibitor, wherein the foaming agent is a mixture of foaming agent E and F, the mass ratio is 1:2, the reinforcing agent is precipitated white carbon black, the auxiliary foaming agent is propanol, the catalyst is platinum catalyst, the inhibitor adopts ethynyl cyclohexanol, the heat-sensitive foaming agent E is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is a sphere which is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer, and the interior of the sphere wraps potassium bicarbonate and isopentane.
A high-rate platinum hot vulcanization foaming silicone rubber and a product method thereof comprise the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
Example 7
A high-magnification platinum heat vulcanization foaming silicon rubber material,
the mass ratio is as follows: 60 parts of methyl vinyl silicone rubber raw rubber A, 40 parts of methyl vinyl silicone rubber raw rubber B, 0.6 part of polyvinyl hydroxyl silicone oil, 44 parts of reinforcing agent, 0.5 part of hydrogen-containing silicone oil, 0.15 part of zinc stearate, 5.6 parts of hydroxyl silicone oil, 0.6 part of auxiliary foaming agent, 3 parts of foaming agent and 0.1 part of catalyst, and 0.2 part of inhibitor, wherein the foaming agent is a mixture of foaming agent E and F, the mass ratio is 1:2, the reinforcing agent is precipitated white carbon black, the auxiliary foaming agent is propanol, the catalyst is platinum catalyst, the inhibitor is ethynyl cyclohexanol, the heat-sensitive foaming agent E is 4, 4-diphenyl sulfonyl hydrazine, the microsphere foaming agent is a sphere which is formed by polymerizing alpha-methyl methacrylate and butenenitrile into a thermoplastic polymer, and the interior of the sphere wraps potassium bicarbonate and isopentane.
A high-rate platinum hot vulcanization foaming silicone rubber and a product method thereof comprise the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
The foamed silicone rubber products prepared in the 7 groups of examples are respectively numbered and tested for performance, and the results are shown in the following table:
the silicone rubber compound provided by the invention has low cost and extremely strong industrial mass production feasibility. Furthermore, it can be seen from the above data that: through the comparative analysis of 7 groups of examples, the silicone rubber product prepared in the example 6 has higher foaming multiplying power (low foaming density and high multiplying power), better compression permanent deformation rate and volume shrinkage rate, and in addition, the excellent compression permanent deformation rate proves that the silicone rubber product has excellent ageing resistance, so that the silicone rubber product can meet the performance requirements of most elastomer industries.
It is to be understood that the foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (5)
1. A high-rate platinum hot vulcanization foaming silicone rubber is characterized in that: the mass ratio of the material is as follows:
100-110 parts of methyl vinyl silicone rubber raw rubber, 40-50 parts of reinforcing agent, 0.1-2 parts of vinyl content regulator, 0.3-0.5 part of hydrogen-containing silicone oil, 0.1-0.3 part of zinc stearate, 4-6 parts of hydroxyl silicone oil, 0.1-0.6 part of auxiliary foaming agent, 2-4 parts of foaming agent, 0.1-0.5 part of catalyst and 0.05-0.3 part of inhibitor; the foaming agent is compounded by adopting a thermosensitive foaming agent and a microsphere foaming agent, the auxiliary foaming agent is propanol, and the catalyst is a platinum catalyst;
the foaming agent is compounded by adopting a thermosensitive foaming agent E and a microsphere foaming agent F; the mass ratio of the thermosensitive foaming agent E to the microsphere foaming agent F is 1:1, 1:2 or 1:3;
the decomposition temperature of the thermosensitive foaming agent E is 130-160 ℃, and the gas generation amount is 160mL/g; the thermosensitive foaming agent is 4, 4-diphenyl sulfonyl hydrazine,
the particle size of the microsphere foaming agent F is 20-30 mu m at normal temperature, the decomposition temperature is 100-140 ℃, and the gas generation amount is 140mL/g; the microsphere foaming agent is a sphere which takes thermoplastic polymer polymerized by alpha-methyl methacrylate and butenenitrile as a shell and internally wraps potassium bicarbonate and isopentane;
the preparation method of the silicone rubber comprises the following steps:
step 1, weighing raw materials according to mass ratio, and adding raw methyl vinyl silicone rubber, a vinyl content regulator, zinc stearate, hydroxyl silicone oil and 26-30% of reinforcing agent into a kneader for kneading and agglomerating;
step 2, adding 26-30% of reinforcing agent into the step 1, and kneading into a block;
step 3, dividing the rest reinforcing agent into three parts, sequentially adding the three parts into the step 2, adding hydrogen-containing silicone oil while adding the last part, kneading into a mass, kneading for 20min, and standing for one hour;
step 4, heating the sizing material in the step 3 to 165-175 ℃ for continuous kneading, closing the cover for 1h, vacuumizing for 1h to form semi-finished silicone rubber, and then standing the semi-finished silicone rubber for 12h; the cover closing time is counted from the temperature of the sizing material to 150 ℃, and the vacuum degree of vacuumizing is minus 0.08MPa to minus 0.06MPa;
step 5, sequentially adding auxiliary foaming agent, foaming agent and inhibitor into the standing mixture in the step 4, fully mixing and stirring the mixture with the first semi-finished product silicone rubber in a kneader to form silicone rubber, and standing for 24 hours at normal temperature;
step 6, putting the synthetic silicone rubber obtained in the step 5 on an open mill, adding a platinum catalyst, fully open-milling and mixing, and uniformly mixing to form vulcanizable foaming silicone rubber, wherein the roll gap of the open mill is 5nm;
and 7, putting the vulcanizable foaming silicone rubber obtained in the step 6 into an extruder, extruding the profile by using a screw, and dynamically heating for 5min in a conveying drying tunnel to vulcanize and foam the profile to obtain a foaming silicone rubber pipe, wherein the temperature of the conveying drying tunnel is controlled between 180 ℃ and 220 ℃.
2. The high-rate platinum heat-curable foam silicone rubber according to claim 1, wherein: the methyl vinyl silicone rubber raw rubber is formed by methyl vinyl silicone rubber raw rubber A and methyl vinyl silicone rubber raw rubber B, wherein the vinyl content of the methyl vinyl silicone rubber raw rubber A is 0.050-0.053%, and the molecular weight is 61 ten thousand-63 ten thousand; the vinyl content of the methyl vinyl silicone rubber raw rubber B is 0.160-0.162%, and the molecular weight is 62-64 ten thousand.
3. The high-rate platinum heat-curable foam silicone rubber according to claim 1, wherein: the vinyl content regulator is one of high-ethylene silicone rubber raw rubber C, vinyl trimethoxy silane and polyvinyl hydroxyl silicone oil.
4. The high-rate platinum heat-curable foam silicone rubber according to claim 3, wherein: the vinyl content of the high-ethylene raw silicone rubber C is 3.00-3.10%, and the molecular weight is 50-55 ten thousand; the weight percent of vinyl trimethoxy silane is 99.9; the viscosity of the polyvinyl hydroxyl silicone oil is less than or equal to 40mm at 25 DEG C 2 S, hydroxyl content: more than or equal to 5.5 percent, vinyl content: 5.5-6.5%.
5. The high-rate platinum heat-curable foam silicone rubber according to claim 1, wherein: the reinforcing agent adopts precipitated white carbon black, and the specific surface area of the precipitated white carbon black is 180-210m 2 /g。
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