CN107815123B - Organic reinforced silicon rubber foam material and preparation method thereof - Google Patents
Organic reinforced silicon rubber foam material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an organic reinforced silicon rubber foam material and a preparation method thereof, wherein the silicon rubber foam material comprises the following components in parts by weight: 100 parts of silicone rubber base material, 50-200 parts of organic reinforcing agent, 4.5-9 parts of structure control agent, 200-450 parts of pore-forming agent and 1.5-3 parts of radiation sensitizer. Compared with the prior art, the invention uses the ethylene propylene diene monomer as the organic reinforcing agent to be blended with the silicon rubber through a simple formula process, the ethylene propylene diene monomer is dissolved out to form holes after radiation crosslinking, and then the foam material with low density, high elongation at break and good tensile strength is obtained through air-blast drying.
Description
Technical Field
The invention belongs to the technical field of rubber materials and advanced composite materials thereof, and particularly relates to an organic reinforced silicone rubber foam material and a preparation method thereof.
Background
The silicon rubber foam material is a high-molecular elastic porous material prepared by foaming a silicon rubber base material in a certain form, integrates the characteristics of silicon rubber and the foam material, has good electrical insulation, chemical stability, weather resistance, radiation resistance, impact resistance and the like, and is widely applied to the fields of transportation, electronics, chemical industry, war industry, aerospace and the like as an ideal material for shock absorption, heat insulation, filling, positioning and the like.
The existing silicone rubber foam material usually adopts inorganic materials such as white carbon black, chopped fiber and the like as reinforcing agents to enhance the mechanical properties (such as tensile strength and the like), but when the reinforcing agents with higher content are required to be added for obtaining higher mechanical strength, the material shows the conditions of larger density, lower elongation at break, weaker interface bonding strength and the like, and simultaneously, the load of rubber is increased, and the difficulty and safety risk of mixing processing are increased. How to maintain the performance advantages of the silicon rubber foam material and avoid the performance disadvantages and processing difficulty of the silicon rubber foam material is a difficult point of industrial research. Therefore, the research on the novel reinforced silicone rubber foam material with simple and environment-friendly preparation process has very positive significance, and no report about the pure organic reinforced silicone rubber foam material is found at present.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided an organic reinforcing type silicone rubber foam having a formulation consisting of, in parts by weight: 100 parts of silicone rubber base material, 50-200 parts of organic reinforcing agent, 4.5-9 parts of structure control agent, 200-450 parts of pore-forming agent and 1.5-3 parts of radiation sensitizer.
Preferably, the formula of the silicone rubber composite material comprises the following components in parts by weight: 100 parts of silicone rubber base material, 100 parts of organic reinforcing agent, 6 parts of structure control agent, 300 parts of pore-forming agent and 2 parts of radiation sensitizer.
Preferably, the silicone rubber is methyl vinyl silicone rubber or methyl vinyl phenyl silicone rubber;
the organic reinforcing agent is any one of 1705, 4570, 4770R, CP80 and 4045 ethylene propylene diene monomer rubber;
the structure control agent is hydroxyl silicone oil;
the pore-forming agent is urea;
the radiation sensitizer is any one of 1, 6-hexanediol diacrylate, trimethylolpropane trimethacrylate and triallyl isocyanurate.
The invention also provides the organic reinforcing type silicon rubber foam material, which comprises the following steps:
adding 100 parts by weight of silicone rubber base material, 50-200 parts by weight of organic reinforcing agent, 4.5-9 parts by weight of structure control agent, 200-450 parts by weight of pore-forming agent and 1.5-3 parts by weight of radiation sensitizer into an open mill, mixing for 15-20 minutes at 80-120 ℃, then standing the primarily mixed rubber material for 12-36 hours, then remilling for 10-15 minutes at 80-120 ℃, and then performing compression molding at 110-120 ℃ to form a sheet or block;
step two, after the formed sheet or block rubber material is subjected to plastic packaging, placing the rubber material in a gamma ray radiation field for radiation crosslinking at room temperature, wherein the absorbed dose is 50-100 kGy, and the rubber material is subjected to crosslinking at one time;
and step three, removing the plastic package of the sample subjected to radiation crosslinking, placing the sample into a pure water bath at 70-90 ℃ for stirring or shaking for soaking for 24-72 hours, taking out the sample, and performing air drying in an air drying oven at 60-90 ℃ for 10-15 hours to obtain the organic reinforced silicone rubber foam material.
Preferably, the silicone rubber is methyl vinyl silicone rubber or methyl vinyl phenyl silicone rubber; the organic reinforcing agent is any one of 1705, 4570, 4770R, CP80 and 4045 ethylene propylene diene monomer rubber; the structure control agent is hydroxyl silicone oil; the pore-forming agent is urea; the radiation sensitizer is any one of 1, 6-hexanediol diacrylate, trimethylolpropane trimethacrylate and triallyl isocyanurate.
Preferably, the organic reinforcing agent is modified ethylene propylene diene monomer; the preparation method of the modified ethylene propylene diene monomer rubber comprises the following steps: adding 25-35 parts by weight of ethylene propylene diene monomer into 100-150 parts by weight of xylene, stirring for dissolving, adding into a supercritical reaction device, simultaneously adding 20-30 parts by weight of vinyl siloxane and 0.1-0.3 part by weight of an initiator, introducing carbon dioxide to 50-60 MPa after the device is sealed, stirring for reacting for 2-3 hours at 70-80 ℃, removing the pressure of the carbon dioxide, adding 0.05-0.1 part by weight of the initiator, 10-15 parts by weight of allyl thiourea and 3-5 parts by weight of styrene, injecting the carbon dioxide again until the pressure is 60-80 MPa, stirring for 1-2 hours at 70-80 ℃, releasing the pressure, filtering, washing with butanone, and drying to obtain the modified ethylene propylene diene monomer.
Preferably, the following processes are further included before and after the filtration: heating the reacted materials to 80-90 ℃, then quickly adding the materials into a stainless steel spherical container, simultaneously adding 10-15 parts of titanate coupling agent, placing the spherical container on a four-axis grinding instrument, starting the four-axis grinding instrument, and driving the stainless steel spherical container to randomly rotate for 90-120 min; then filtering, washing with butanone, and drying to obtain modified ethylene propylene diene monomer; the feed inlet of the stainless steel spherical container is sealed by a threaded cover, and the threaded cover is flush with the surface of the stainless steel spherical container after being connected in a sealing way; the rotating shaft rotating speed of the four-shaft grinding instrument is 150-200 rpm, and the random conversion frequency is 10-20 s.
Preferably, the vinyl siloxane is any one of vinyl triacetoxysilane, vinyl triisopropoxysilane, vinyl tri-tert-butoxysilane, and vinyl tributyroximosilane; the initiator is any one of benzoyl peroxide, azobisisobutyronitrile and cumene hydroperoxide.
Preferably, the vinyl siloxane is vinyltriisopropoxysilane and vinyltributketoximosilane in a weight ratio of 3: 1.
Preferably, the titanate coupling agent is any one of titanate coupling agent TMC-201, titanate coupling agent TMC-102, titanate coupling agent TMC-101, titanate coupling agent TMC-TTS, titanate coupling agent TMC-931 and titanate coupling agent TMC-2.
The invention at least comprises the following beneficial effects:
(1) compared with the prior art, the invention uses the ethylene propylene diene monomer as the organic reinforcing agent to effectively blend with the silicon rubber through a simple formula process, dissolves out and forms holes after radiation crosslinking, and then obtains the foam material with low density, high elongation at break and good tensile strength through air-blast drying.
(2) The invention has simple formula, not only can well and effectively blend the components in a compatible way, but also has excellent performance of the prepared material, and simultaneously, the preparation method is simple, environment-friendly and good in reproducibility, the mixing processing process is easy to control, and the difficulty and safety hazard caused by the high load of the rubber material can not occur.
(3) The invention is a preferred method for preparing the novel silicon rubber foam material, on the basis of the method, pilot-scale research can be conveniently carried out, and a very simple and quick technical path with good reproducibility is provided for further researching the multipurpose silicon rubber foam material with excellent comprehensive performance.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is a scanning electron microscope image of a cross section of an organic reinforcing type silicone rubber foam material prepared in example 1 of the present invention and a preparation method thereof;
the specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
the organic reinforced silicone rubber foam material is characterized by comprising the following components in parts by weight: 100 parts of silicon rubber base material, 50 parts of organic reinforcing agent, 4.5 parts of structure control agent, 225 parts of pore-forming agent and 1.5 parts of radiation sensitizer; the silicone rubber is methyl vinyl silicone rubber; the organic reinforcing agent is 1705 type ethylene propylene diene monomer; the structure control agent is hydroxyl silicone oil; the pore-forming agent is urea; the radiation sensitizer is triallyl isocyanurate.
The organic reinforcing type silicon rubber foam material comprises the following steps:
step one, adding 100 parts by weight of silicone rubber base material, 50 parts by weight of organic reinforcing agent, 4.5 parts by weight of structure control agent, 225 parts by weight of pore-forming agent and 1.5 parts by weight of radiation sensitizer into an open mill, mixing for 15 minutes at 80 ℃, then standing the primarily mixed rubber for 36 hours, then re-mixing for 10 minutes at 80 ℃, and then performing compression molding at 110 ℃ to form a sheet with the thickness of 2 mm;
step two, after the formed sheet or block rubber material is subjected to plastic packaging, placing the rubber material in a gamma ray radiation field for radiation crosslinking at room temperature, wherein the absorbed dose is 100kGy, and the rubber material is subjected to crosslinking at one time;
and step three, removing the plastic package of the sample subjected to radiation crosslinking, placing the sample into a pure water bath at 70 ℃ for stirring or shaking for soaking for 72 hours, taking out the sample, and placing the sample into an air-blast drying oven for air-blast drying for 15 hours at 60 ℃ to obtain the organic reinforced silicone rubber foam material.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 271.51%; apparent density, 0.21g.cm-3(ii) a Tensile strength, 0.38 MPa; compressive strength (25%), 118.60 kPa.
Example 2:
the organic reinforced silicone rubber foam material is characterized by comprising the following components in parts by weight: 100 parts of silicone rubber base material, 100 parts of organic reinforcing agent, 6 parts of structure control agent, 300 parts of pore-forming agent and 2 parts of radiation sensitizer; the silicone rubber is methyl vinyl silicone rubber; the organic reinforcing agent is 4570 type ethylene propylene diene monomer rubber; the structure control agent is hydroxyl silicone oil; the pore-forming agent is urea; the radiation sensitizer is triallyl isocyanurate.
The organic reinforcing type silicon rubber foam material comprises the following steps:
step one, adding 100 parts of silicone rubber base material, 100 parts of organic reinforcing agent, 6 parts of structure control agent, 300 parts of pore-forming agent and 2 parts of radiation sensitizer into an open mill, mixing for 18 minutes at 100 ℃, then standing the primarily mixed rubber for 20 hours, then back-mixing for 15 minutes at 100 ℃, and then performing compression molding at 120 ℃ to form a sheet with the thickness of 1 mm;
step two, after the formed sheet or block rubber material is subjected to plastic packaging, placing the rubber material in a gamma ray radiation field for radiation crosslinking at room temperature, wherein the absorbed dose is 50kGy, and the rubber material is subjected to crosslinking at one time;
and step three, removing the plastic package of the sample subjected to radiation crosslinking, placing the sample into a pure water bath at 70 ℃ for stirring or shaking for soaking for 1 day, taking out the sample, and performing air blast drying in an air blast drying oven at 60 ℃ for 10 hours to obtain the organic reinforced silicone rubber foam material.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 510.4%; apparent density, 0.16g.cm-3(ii) a Tensile strength, 0.86 MPa; compressive strength (25%), 191.40 kPa.
Example 3:
the organic reinforced silicone rubber foam material is characterized by comprising the following components in parts by weight: 100 parts of silicon rubber base material, 200 parts of organic reinforcing agent, 9 parts of structure control agent, 450 parts of pore-forming agent and 3 parts of radiation sensitizer; the silicone rubber is methyl vinyl silicone rubber; the organic reinforcing agent is 4770R type ethylene propylene diene monomer rubber; the structure control agent is hydroxyl silicone oil; the pore-forming agent is urea; the radiation sensitizer is triallyl isocyanurate.
The organic reinforcing type silicon rubber foam material comprises the following steps:
step one, adding 100 parts of silicone rubber base material, 200 parts of organic reinforcing agent, 9 parts of structure control agent, 450 parts of pore-forming agent and 3 parts of radiation sensitizer into an open mill, mixing for 20 minutes at 120 ℃, then standing the primarily mixed rubber for 12 hours, then back-mixing for 15 minutes at 120 ℃, and then performing compression molding at 120 ℃ to form a sheet with the thickness of 4 mm;
step two, after the formed sheet or block rubber material is subjected to plastic packaging, placing the rubber material in a gamma ray radiation field for radiation crosslinking at room temperature, wherein the absorbed dose is 50kGy, and the rubber material is subjected to crosslinking at one time;
and step three, removing the plastic package of the sample subjected to radiation crosslinking, placing the sample into a pure water bath at 70 ℃ for stirring or shaking for soaking for 1 day, taking out the sample, and performing air blast drying in an air blast drying oven at 70 ℃ for 10 hours to obtain the organic reinforced silicone rubber foam material.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 583.31%; apparent density, 0.09g.cm-3(ii) a Tensile strength, 1.14 MPa; compressive strength (25%), 209 kPa.
Example 4:
the organic reinforced silicone rubber foam material is characterized by comprising the following components in parts by weight: 100 parts of silicone rubber base material, 150 parts of organic reinforcing agent, 7 parts of structure control agent, 400 parts of pore-forming agent and 3 parts of radiation sensitizer; the silicone rubber is methyl vinyl silicone rubber; the organic reinforcing agent is CP80 type ethylene propylene diene monomer; the structure control agent is hydroxyl silicone oil; the pore-forming agent is urea; the radiation sensitizer is triallyl isocyanurate.
The organic reinforcing type silicon rubber foam material comprises the following steps:
step one, adding 100 parts of silicone rubber base material, 150 parts of organic reinforcing agent, 7 parts of structure control agent, 400 parts of pore-forming agent and 3 parts of radiation sensitizer into an open mill, mixing for 20 minutes at 110 ℃, then standing the primarily mixed rubber for 16 hours, then back-mixing for 15 minutes at 120 ℃, and then performing compression molding at 120 ℃ to form a sheet with the thickness of 10 mm;
step two, after the formed sheet or block rubber material is subjected to plastic packaging, placing the rubber material in a gamma ray radiation field for radiation crosslinking at room temperature, wherein the absorbed dose is 80kGy, and the rubber material is subjected to crosslinking at one time;
and step three, removing the plastic package of the sample subjected to radiation crosslinking, placing the sample into a pure water bath at 80 ℃ for stirring or shaking for soaking for 2 days, taking out the sample, and performing forced air drying in a forced air drying oven at 65 ℃ for 12 hours to obtain the organic reinforcing type silicon rubber foam material.
Taking the prepared organic reinforced siliconThe performance test of the rubber foam material is as follows: elongation at break, 507.63%; apparent density, 0.13g.cm-3(ii) a Tensile strength, 1.07 MPa; compressive strength (25%), 165.8 kPa.
Example 5:
the organic reinforced silicone rubber foam material is characterized by comprising the following components in parts by weight: 100 parts of silicone rubber base material, 80 parts of organic reinforcing agent, 6 parts of structure control agent, 300 parts of pore-forming agent and 2 parts of radiation sensitizer; the silicone rubber is methyl vinyl silicone rubber; the organic reinforcing agent is CP80 type ethylene propylene diene monomer; the structure control agent is hydroxyl silicone oil; the pore-forming agent is urea; the radiation sensitizer is triallyl isocyanurate.
The organic reinforcing type silicon rubber foam material comprises the following steps:
step one, adding 100 parts of silicone rubber base material, 80 parts of organic reinforcing agent, 6 parts of structure control agent, 300 parts of pore-forming agent and 2 parts of radiation sensitizer into an open mill, mixing for 15 minutes at 100 ℃, then standing the primarily mixed rubber for 30 hours, then back-mixing for 15 minutes at 110 ℃, and then performing compression molding at 115 ℃ to form a sheet with the thickness of 15 mm;
step two, after the formed sheet or block rubber material is subjected to plastic packaging, placing the rubber material in a gamma ray radiation field for radiation crosslinking at room temperature, wherein the absorbed dose is 60kGy, and the rubber material is subjected to crosslinking at one time;
and step three, removing the plastic package of the sample subjected to radiation crosslinking, placing the sample into a pure water bath at 80 ℃ for stirring or shaking for soaking for 3 days, taking out the sample, and performing air blast drying in an air blast drying oven at 70 ℃ for 15 hours to obtain the organic reinforced silicone rubber foam material.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 411.1%; apparent density, 0.16g.cm-3(ii) a Tensile strength, 0.76 MPa; compressive strength (25%), 119.70 kPa.
Example 6:
the organic reinforcing agent is modified ethylene propylene diene monomer; the preparation method of the modified ethylene propylene diene monomer rubber comprises the following steps: adding 25 parts by weight of ethylene propylene diene monomer into 100 parts by weight of dimethylbenzene, stirring for dissolving, adding into a supercritical reaction device, simultaneously adding 20 parts by weight of vinyl siloxane and 0.1 part by weight of initiator, introducing carbon dioxide to 50MPa after the device is sealed, stirring for reacting for 2 hours at 70 ℃, removing the pressure of carbon dioxide, adding 0.05 part by weight of initiator, 10 parts by weight of allyl thiourea and 3 parts by weight of styrene, injecting carbon dioxide again until the pressure is 60MPa, stirring for 1 hour at 70 ℃, relieving the pressure, filtering, washing with butanone, and drying to obtain the modified ethylene propylene diene monomer. The vinyl siloxane is vinyl triacetoxysilane; the initiator is benzoyl peroxide; the modified ethylene propylene diene monomer prepared by the modification method of the invention not only further effectively improves the compatibility and blending with other components, but also improves the mechanical property of the silicon rubber foam material to a certain extent.
The rest of the process is exactly the same as in example 1.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 342.23%; apparent density, 0.22g.cm-3(ii) a Tensile strength, 0.45 MPa; compressive strength (25%), 128.60 kPa.
Example 7:
the organic reinforcing agent is modified ethylene propylene diene monomer; the preparation method of the modified ethylene propylene diene monomer rubber comprises the following steps: according to the weight portion, 30 portions of ethylene propylene diene monomer are added into 120 portions of dimethylbenzene, stirred and dissolved, then added into a supercritical reaction device, 25 portions of vinyl siloxane and 0.2 portion of initiator are added at the same time, carbon dioxide is introduced to 50MPa after the device is sealed, the mixture is stirred and reacted for 2 hours at the temperature of 70 ℃, then the pressure of the carbon dioxide is removed, 0.05 portion of initiator, 12 portions of allyl thiourea and 4 portions of styrene are added, then the carbon dioxide is injected again until the pressure is 60MPa, the mixture is stirred for 1 hour at the temperature of 70 ℃, pressure relief is carried out, filtration is carried out, washing with butanone and drying are carried out, and the modified ethylene propylene diene monomer is obtained. The vinyl siloxane is vinyl triisopropoxysilane and vinyl tributyloximosilane in a weight ratio of 3: 1; the initiator is benzoyl peroxide;
the rest of the process is exactly the same as in example 1.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 350.25%; apparent density, 0.20g.cm-3(ii) a Tensile strength, 0.47 MPa; compressive strength (25%), 132.88 kPa.
Example 8:
the process before and after the filtration also comprises the following steps: heating the reacted materials to 80 ℃, then quickly adding the materials into a stainless steel spherical container, simultaneously adding 10 parts of titanate coupling agent TMC-201, placing the spherical container on a four-axis grinding instrument, starting the four-axis grinding instrument, and driving the stainless steel spherical container to randomly rotate for 90 min; then filtering, washing with butanone, and drying to obtain modified ethylene propylene diene monomer; the feed inlet of the stainless steel spherical container is sealed by a threaded cover, and the threaded cover is flush with the surface of the stainless steel spherical container after being connected in a sealing way; the rotating speed of the rotating shaft of the four-shaft grinding instrument is 150rpm, and the random conversion frequency is 10 s.
The rest of the process was exactly the same as in example 6.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 355.25%; apparent density, 0.21g.cm-3(ii) a Tensile strength, 0.52 MPa; compressive strength (25%), 140.56 kPa.
Example 9:
the process before and after the filtration also comprises the following steps: heating the reacted materials to 80 ℃, then quickly adding the materials into a stainless steel spherical container, simultaneously adding 10 parts of titanate coupling agent TMC-931, placing the spherical container on a four-axis grinding instrument, starting the four-axis grinding instrument, and driving the stainless steel spherical container to randomly rotate for 120 min; then filtering, washing with butanone, and drying to obtain modified ethylene propylene diene monomer; the feed inlet of the stainless steel spherical container is sealed by a threaded cover, and the threaded cover is flush with the surface of the stainless steel spherical container after being connected in a sealing way; the rotating speed of the rotating shaft of the four-shaft grinding instrument is 150rpm, and the random conversion frequency is 15 s.
The rest of the process was exactly the same as in example 6.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 357.25%; apparent density, 0.23g.cm-3(ii) a Tensile strength, 0.55 MPa; compressive strength (25%), 142.48 kPa.
Example 10:
the organic reinforcing agent is modified ethylene propylene diene monomer; the preparation method of the modified ethylene propylene diene monomer rubber comprises the following steps: according to the weight portion, 35 portions of ethylene propylene diene monomer are added into 120 portions of dimethylbenzene, stirred and dissolved, then added into a supercritical reaction device, 25 portions of vinyl siloxane and 0.2 portion of initiator are added at the same time, carbon dioxide is introduced to 50MPa after the device is sealed, the mixture is stirred and reacted for 2 hours at the temperature of 70 ℃, then the pressure of the carbon dioxide is removed, 0.05 portion of initiator, 12 portions of allyl thiourea and 4 portions of styrene are added, then the carbon dioxide is injected again until the pressure is 60MPa, the mixture is stirred for 1 hour at the temperature of 70 ℃, pressure relief is carried out, filtration is carried out, washing with butanone and drying are carried out, and the modified ethylene propylene diene monomer is obtained. The vinyl siloxane is vinyl triisopropoxysilane and vinyl tributyloximosilane in a weight ratio of 3: 1; the initiator is benzoyl peroxide;
the rest of the process is exactly the same as in example 2.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 520.35%; apparent density, 0.17g.cm-3(ii) a Tensile strength, 0.95 MPa; compressive strength (25%), 196.86 kPa.
Example 11:
the process before and after the filtration also comprises the following steps: heating the reacted materials to 85 ℃, then quickly adding the materials into a stainless steel spherical container, simultaneously adding 10 parts of titanate coupling agent TMC-931, placing the spherical container on a four-axis grinding instrument, starting the four-axis grinding instrument, and driving the stainless steel spherical container to randomly rotate for 120 min; then filtering, washing with butanone, and drying to obtain modified ethylene propylene diene monomer; the feed inlet of the stainless steel spherical container is sealed by a threaded cover, and the threaded cover is flush with the surface of the stainless steel spherical container after being connected in a sealing way; the rotating speed of the rotating shaft of the four-shaft grinding instrument is 150rpm, and the random conversion frequency is 15 s.
The rest of the process was exactly the same as in example 10.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 528.23%; apparent density, 0.18g.cm-3(ii) a Tensile strength, 1.06 MPa; compressive strength (25%), 201.57 kPa.
Example 12:
the organic reinforcing agent is modified ethylene propylene diene monomer; the preparation method of the modified ethylene propylene diene monomer rubber comprises the following steps: according to the weight portion, 35 portions of ethylene propylene diene monomer are added into 120 portions of dimethylbenzene, stirred and dissolved, then added into a supercritical reaction device, 25 portions of vinyl siloxane and 0.2 portion of initiator are added at the same time, carbon dioxide is introduced to 50MPa after the device is sealed, the mixture is stirred and reacted for 2 hours at the temperature of 70 ℃, then the pressure of the carbon dioxide is removed, 0.05 portion of initiator, 12 portions of allyl thiourea and 4 portions of styrene are added, then the carbon dioxide is injected again until the pressure is 60MPa, the mixture is stirred for 1 hour at the temperature of 70 ℃, pressure relief is carried out, filtration is carried out, washing with butanone and drying are carried out, and the modified ethylene propylene diene monomer is obtained. The vinyl siloxane is vinyl triisopropoxysilane and vinyl tributyloximosilane in a weight ratio of 3: 1; the initiator is benzoyl peroxide;
the rest of the process was exactly the same as in example 3.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 588.65%; apparent density, 0.10g.cm-3(ii) a Tensile strength, 1.28 MPa; compressive strength (25%), 216.89 kPa.
Example 13:
the process before and after the filtration also comprises the following steps: heating the reacted materials to 85 ℃, then quickly adding the materials into a stainless steel spherical container, simultaneously adding 10 parts of titanate coupling agent TMC-931, placing the spherical container on a four-axis grinding instrument, starting the four-axis grinding instrument, and driving the stainless steel spherical container to randomly rotate for 120 min; then filtering, washing with butanone, and drying to obtain modified ethylene propylene diene monomer; the feed inlet of the stainless steel spherical container is sealed by a threaded cover, and the threaded cover is flush with the surface of the stainless steel spherical container after being connected in a sealing way; the rotating speed of the rotating shaft of the four-shaft grinding instrument is 150rpm, and the random conversion frequency is 15 s.
The rest of the process was exactly the same as in example 12.
Taking the prepared organic reinforced silicone rubber foam material for performance test: elongation at break, 595.24%; apparent density, 0.12g.cm-3(ii) a Tensile strength, 1.45 MPa; compressive strength (25%), 225.57 kPa.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (6)
1. The organic reinforced silicone rubber foam material is characterized by comprising the following components in parts by weight: 100 parts of silicone rubber base material, 50-200 parts of organic reinforcing agent, 4.5-9 parts of structure control agent, 200-450 parts of pore-forming agent and 1.5-3 parts of radiation sensitizer;
the preparation method of the organic reinforcing type silicon rubber foam material comprises the following steps:
adding 100 parts by weight of silicone rubber base material, 50-200 parts by weight of organic reinforcing agent, 4.5-9 parts by weight of structure control agent, 200-450 parts by weight of pore-forming agent and 1.5-3 parts by weight of radiation sensitizer into an open mill, mixing for 15-20 minutes at 80-120 ℃, then standing the primarily mixed rubber material for 12-36 hours, then remilling for 10-15 minutes at 80-120 ℃, and then performing compression molding at 110-120 ℃ to form a sheet or block;
step two, after the formed sheet or block rubber material is subjected to plastic packaging, placing the rubber material in a gamma ray radiation field for radiation crosslinking at room temperature, wherein the absorbed dose is 50-100 kGy, and the rubber material is subjected to crosslinking at one time;
removing the plastic package of the sample subjected to radiation crosslinking, placing the sample into a pure water bath at 70-90 ℃, stirring or shaking for soaking for 24-72 hours, taking out the sample, and performing forced air drying in a forced air drying oven at 60-90 ℃ for 10-15 hours to obtain an organic reinforced silicone rubber foam material;
the silicone rubber is methyl vinyl silicone rubber or methyl vinyl phenyl silicone rubber; the structure control agent is hydroxyl silicone oil; the pore-forming agent is urea; the radiation sensitizer is any one of 1, 6-hexanediol diacrylate, trimethylolpropane trimethacrylate and triallyl isocyanurate;
the organic reinforcing agent is modified ethylene propylene diene monomer; the preparation method of the modified ethylene propylene diene monomer rubber comprises the following steps: adding 25-35 parts by weight of ethylene propylene diene monomer into 100-150 parts by weight of xylene, stirring for dissolving, adding into a supercritical reaction device, simultaneously adding 20-30 parts by weight of vinyl siloxane and 0.1-0.3 part by weight of an initiator, introducing carbon dioxide to 50-60 MPa after the device is sealed, stirring for reacting for 2-3 hours at 70-80 ℃, removing the pressure of the carbon dioxide, adding 0.05-0.1 part by weight of the initiator, 10-15 parts by weight of allyl thiourea and 3-5 parts by weight of styrene, injecting the carbon dioxide again until the pressure is 60-80 MPa, stirring for 1-2 hours at 70-80 ℃, releasing the pressure, filtering, washing with butanone, and drying to obtain the modified ethylene propylene diene monomer.
2. An organic reinforcing type silicone rubber foam material as set forth in claim 1, wherein said silicone rubber composite is formulated by weight: 100 parts of silicone rubber base material, 100 parts of organic reinforcing agent, 6 parts of structure control agent, 300 parts of pore-forming agent and 2 parts of radiation sensitizer.
3. An organic reinforcing silicone rubber foam as defined in claim 1, further comprising the following steps before and after said filtering: heating the reacted materials to 80-90 ℃, then quickly adding the materials into a stainless steel spherical container, simultaneously adding 10-15 parts of titanate coupling agent, placing the spherical container on a four-axis grinding instrument, starting the four-axis grinding instrument, and driving the stainless steel spherical container to randomly rotate for 90-120 min; then filtering, washing with butanone, and drying to obtain modified ethylene propylene diene monomer; the feed inlet of the stainless steel spherical container is sealed by a threaded cover, and the threaded cover is flush with the surface of the stainless steel spherical container after being connected in a sealing way; the rotating shaft rotating speed of the four-shaft grinding instrument is 150-200 rpm, and the random conversion frequency is 10-20 s.
4. The organic reinforcing silicone rubber foam according to claim 1, wherein the vinyl-based siloxane is any one of vinyltriacetoxysilane, vinyltriisopropoxysilane, vinyltri-tert-butoxysilane, vinyltributyrindoxysilane; the initiator is any one of benzoyl peroxide, azobisisobutyronitrile and cumene hydroperoxide.
5. An organic reinforcing silicone rubber foam as defined in claim 1, wherein said vinyl silicone is vinyltriisopropoxysilane and vinyltributketoximosilane in a weight ratio of 3: 1.
6. An organic reinforcing silicone rubber foam as defined in claim 3, wherein said titanate coupling agent is any one of titanate coupling agent TMC-201, titanate coupling agent TMC-102, titanate coupling agent TMC-101, titanate coupling agent TMC-TTS, titanate coupling agent TMC-931, and titanate coupling agent TMC-2.
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| CN103289411A (en) * | 2013-05-22 | 2013-09-11 | 易宝（福建）高分子材料股份公司 | Silicone rubber/ethylene-propylene-diene rubber binary blend closed-cell foamed material and preparation method thereof |
| GB2521995A (en) * | 2013-08-16 | 2015-07-15 | Thermoseal Group Ltd | Elastomeric blend composition and use in window spacers |
| CN104788967A (en) * | 2015-04-16 | 2015-07-22 | 中国工程物理研究院核物理与化学研究所 | Silicone rubber microporous foam material adopting mixed cellular structure and preparation method of silicone rubber microporous foam material |
| CN105348655A (en) * | 2015-11-27 | 2016-02-24 | 中国工程物理研究院核物理与化学研究所 | Ethylene-propylene-diene monomer rubber-based microporous foam material and preparation method thereof |
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| CN103289411A (en) * | 2013-05-22 | 2013-09-11 | 易宝（福建）高分子材料股份公司 | Silicone rubber/ethylene-propylene-diene rubber binary blend closed-cell foamed material and preparation method thereof |
| GB2521995A (en) * | 2013-08-16 | 2015-07-15 | Thermoseal Group Ltd | Elastomeric blend composition and use in window spacers |
| CN104788967A (en) * | 2015-04-16 | 2015-07-22 | 中国工程物理研究院核物理与化学研究所 | Silicone rubber microporous foam material adopting mixed cellular structure and preparation method of silicone rubber microporous foam material |
| CN105348655A (en) * | 2015-11-27 | 2016-02-24 | 中国工程物理研究院核物理与化学研究所 | Ethylene-propylene-diene monomer rubber-based microporous foam material and preparation method thereof |
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