CN112063180A - Antibacterial and mildew-proof high-temperature vulcanized silicone rubber and preparation method thereof - Google Patents
Antibacterial and mildew-proof high-temperature vulcanized silicone rubber and preparation method thereof Download PDFInfo
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- CN112063180A CN112063180A CN202010949845.0A CN202010949845A CN112063180A CN 112063180 A CN112063180 A CN 112063180A CN 202010949845 A CN202010949845 A CN 202010949845A CN 112063180 A CN112063180 A CN 112063180A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention belongs to the technical field of high-temperature vulcanized silicone rubber materials, and relates to antibacterial mildew-proof high-temperature vulcanized silicone rubber and a preparation method thereof, wherein the antibacterial mildew-proof high-temperature vulcanized silicone rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 2-10 parts of hydroxyl silicone oil, 2-5 parts of dimethyl silicone oil, 1-5 parts of silane coupling agent, 20-100 parts of white carbon black, 1-2 parts of vulcanizing agent, 10-50 parts of diatomite, 1-5 parts of polydivinyltriamineguanidine, 1-5 parts of aluminate coupling agent and 0.1-0.5 part of release agent. The antibacterial silicone rubber has excellent antibacterial and mildew-proof properties, simple preparation process, good mechanical properties and good application prospect in the engineering field.
Description
Technical Field
The invention belongs to the technical field of high-temperature vulcanized silicone rubber materials, and relates to antibacterial and mildewproof high-temperature vulcanized silicone rubber and a preparation method thereof.
Background
The high-temperature vulcanized silicone rubber material has the characteristics of excellent high and low temperature resistance, weather resistance, water resistance, moisture resistance, good compression deformation performance and the like, and can be widely applied to the field of marine equipment. Because the working environment in the field of marine equipment contains salt mist and water vapor, a large number of microorganisms and bacteria exist and are attached to the surface and holes of the silicon rubber material, the service life of the material is shortened, and the harm is brought to equipment and personnel. Therefore, the development of the antibacterial and mildewproof silicon rubber is of great significance. The performance of the currently used antibacterial mildew-resistant silicone rubber cannot meet the use requirement or the price is too high, so that the development of novel antibacterial mildew-resistant high-temperature vulcanized silicone rubber is urgently needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an antibacterial and mildewproof high-temperature vulcanized silicone rubber and a preparation method thereof. The novel antibacterial and mildew-proof high-temperature vulcanized silicone rubber has the advantages of excellent antibacterial and mildew-proof effects, simple production process, excellent mechanical properties, lower cost and the like.
The invention is realized by the following technical scheme:
the antibacterial mildew-proof high-temperature vulcanized silicone rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 2-10 parts of hydroxyl silicone oil, 20-100 parts of white carbon black, 10-50 parts of diatomite, 1-2 parts of vulcanizing agent, 1-5 parts of poly (diethylenetriamine guanidine), 1-5 parts of aluminate coupling agent, 1-2 parts of silane coupling agent, 2-5 parts of dimethyl silicone oil and 0.1-0.5 part of mold release agent.
The molecular weight of the methyl vinyl silicone rubber is between 600000 and 700000.
The vinyl content of the methyl vinyl silicone rubber is 0.1-0.3 mol%.
The white carbon black is treated by silazane, and the particle size is 10-1000 nm.
The coupling agent is aluminate and silane coupling agent.
The antibacterial agent is poly-diethylenetriamine guanidine.
The diatomite is treated by stearic acid, and the particle size is 10-1000 mu m.
The vulcanizing agent is 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane.
The preparation method specifically comprises the following steps:
1) and adding the methyl vinyl silicone rubber, polydivinyltriamineguanidine, aluminate coupling agent and silane coupling agent into a kneading machine, and stirring for 0.5-1 hour without heating.
2) Heating the materials, stirring, heating to 80-120 ℃, vacuumizing, preserving heat and stirring for 0.5-1 hour.
3) Adding white carbon black, hydroxyl silicone oil, diatomite, dimethyl silicone oil and a release agent into the materials, heating to 140-160 ℃, preserving heat and stirring for 0.5-1 hour to obtain a silicone rubber material;
4) and (3) preserving the heat of the materials, vacuumizing and stirring for 0.5-1 hour.
5) And adding the silicon rubber material and a vulcanizing agent 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane into an open rubber mixing mill, uniformly mixing, and then placing the mixture into a flat vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to prepare the antibacterial silicon rubber.
The invention has the beneficial effects that: the invention provides antibacterial silicone rubber and a preparation method thereof, and the antibacterial silicone rubber has good mechanical properties and antibacterial properties by adding polydivinyltriamineguanidine, an aluminate coupling agent and a silane coupling agent.
The antibacterial silicone rubber has good antibacterial property, and retains the excellent mechanical properties of the silicone rubber; tensile strength of the novel high-temperature silicone rubber>9.0MPa, elongation at break>500% hardness (Shore A)>50, density<1.25g/cm3The invention has high strength, good elasticity and low density; the bacteriostasis rate of the invention exceeds 90 percent, which shows that the invention has good antibacterial performance.
Detailed Description
For a further understanding of the invention, reference will now be made to the following description of embodiments, but it will be understood that the description is intended to illustrate further features and advantages of the invention, and not to limit the scope of the claims.
Example 1
The antibacterial silicone rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 3 parts of hydroxyl silicone oil, 2 parts of aluminate coupling agent, 50 parts of white carbon black, 10 parts of diatomite, 1 part of vulcanizing agent, 5 parts of polydivinyltriamineguanidine, 1 part of silane coupling agent, 2 parts of methyl silicone oil and 0.1 part of release agent.
The preparation method comprises the following steps:
1) adding methyl vinyl silicone rubber, polydivinyltriamineguanidine, an aluminate coupling agent and a silane coupling agent into a kneading machine, and stirring for 40 minutes without heating to obtain a molding material;
2) heating and stirring the formed material to 80 ℃, vacuumizing, preserving heat and stirring for 1 hour.
3) Adding white carbon black, hydroxyl silicone oil, diatomite, methyl silicone oil and a release agent into the materials, heating to 140 ℃, preserving heat and stirring for 0.5 hour to obtain a silicone rubber material;
4) the material was held at temperature and evacuated for 40 minutes.
5) And adding the obtained silicon rubber material and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane into an open rubber mixing mill, uniformly mixing, and then placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the antibacterial silicon rubber.
Example 2
The antibacterial silicone rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 4 parts of hydroxyl silicone oil, 3 parts of aluminate coupling agent, 45 parts of white carbon black, 15 parts of diatomite, 1 part of vulcanizing agent, 5 parts of polydivinyltriamineguanidine, 2 parts of silane coupling agent, 5 parts of methyl silicone oil and 0.2 part of release agent.
The preparation method comprises the following steps:
1) adding methyl vinyl silicone rubber, polydivinyltriamineguanidine, aluminate coupling agent and silane coupling agent into a kneading machine, and stirring for 30 minutes without heating to obtain a molding material.
2) Heating and stirring the formed material to 110 ℃, vacuumizing, preserving heat and stirring for 1 hour.
3) Adding white carbon black, hydroxyl silicone oil, diatomite, methyl silicone oil and a release agent into the materials, heating to 150 ℃, preserving heat and stirring for 40 minutes to obtain the silicone rubber material.
4) The materials are vacuumized, kept warm and stirred for 1 hour.
5) And adding the obtained silicon rubber material and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane into an open rubber mixing mill, uniformly mixing, and then placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the antibacterial silicon rubber.
Example 3
The antibacterial silicone rubber is prepared from the following raw materials in parts by weight: 100 parts of methyl vinyl silicone rubber, 5 parts of hydroxyl silicone oil, 3 parts of aluminate coupling agent, 40 parts of white carbon black, 20 parts of diatomite, 1 part of vulcanizing agent, 4 parts of polydivinyltriamineguanidine, 1 part of silane coupling agent, 5 parts of methyl silicone oil and 0.1 part of release agent.
The preparation method comprises the following steps:
1) adding methyl vinyl silicone rubber, polydivinyltriamineguanidine, aluminate coupling agent and silane coupling agent into a kneading machine, and stirring for 1 hour without heating to obtain a molding material.
2) Heating and stirring the molding material to 120 ℃, vacuumizing, preserving heat and stirring for 40 minutes.
3) Adding white carbon black, hydroxyl silicone oil and a release agent into the materials, heating to 160 ℃, preserving heat and stirring for 30 minutes to prepare the silicone rubber material.
4) The materials are vacuumized, kept warm and stirred for 60 minutes.
5) And adding the obtained silicon rubber material and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane into an open rubber mixing mill, uniformly mixing, and then placing the mixture into a flat plate vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to obtain the antibacterial silicon rubber.
Performance detection
The hardness (Shore A) is tested according to the GB/T531-1999 standard; the tensile strength and the elongation at break are tested according to the GB/T528-1998 standard; and (3) testing antibacterial performance:
(1) cutting the rubber sheet into 1cm × 11cm pieces, and cleaning with ethanol.
(2) The staphylococcus aureus strain is activated to prepare bacterial suspension with the concentration of 1 × 104 cfu/ml-5 × 104 cfu/ml. And then putting the cut rubber sheet into the container.
(3) The Erlenmeyer flask containing the bacterial suspension and the rubber sheet is fixed on a shaking table and shaken for 2min at the temperature of 20-25 ℃ and at the speed of 300 r/min. Then 1.0ml of the bacterial suspension was diluted to 100-fold.
(4) Sucking l.0ml of the shaken sample solution, inoculating on agar medium, and culturing at 37 deg.C for 48h under natural light. Colony counts were then performed as described in GB 15979-2003.
(5) Both blank and negative controls of the experiment were run as described above.
(6) The test is repeated for 3 times, and the bacteriostasis rate is calculated according to a formula.
The mildewproof antibacterial silicone rubbers prepared in examples 1 to 3 were subjected to performance tests and compared with antibacterial silicone rubbers manufactured by a company of Guangdong, and the comparison results are shown in Table 1.
Table 1 shows a comparison of the performance indexes of the mildewproof antibacterial silicone rubber prepared in examples 1 to 3 and a comparative antibacterial silicone rubber.
As can be seen from Table 1, the tensile strength of the novel high-temperature silicone rubber is more than 9MPa, and the elongation at break is more than 500 percent, which is superior to that of the comparative example. The Shore hardness is lower than that of the comparative example, which shows that the invention has good softness and elasticity. The bacteriostasis rate of the invention is over 90 percent, which is superior to that of the comparative example, and shows that the invention has good antibacterial performance. The density of the invention is lower than 1.30g/cm3Wide raw material source, simple process, and effective reductionAnd (4) cost.
It should be understood that the detailed description of the present invention is only for illustrating the present invention and is not limited by the technical solutions described in the embodiments of the present invention, and those skilled in the art should understand that the present invention can be modified or substituted equally to achieve the same technical effects; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (9)
1. The antibacterial and mildewproof high-temperature vulcanized silicone rubber is characterized by being prepared from the following raw materials in parts by weight:
2. the antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the molecular weight of the methyl vinyl silicone rubber is between 600000 and 700000.
3. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the vinyl content of the methyl vinyl silicone rubber is 0.1-0.3 mol%.
4. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the white carbon black is treated by silazane, and the particle size is 10-1000 nm.
5. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the coupling agent is aluminate and silane coupling agent.
6. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the antibacterial agent polydiethylene triamine guanidine is a reactant of diethylenetriamine and guanidine hydrochloride.
7. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the vulcanizing agent is 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane.
8. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the diatomite is treated by stearic acid, and the particle size is 10-1000 μm.
9. The preparation method of the antibacterial and mildewproof high-temperature vulcanized silicone rubber according to claim 1, which is characterized by comprising the following steps of:
1) adding the methyl vinyl silicone rubber, polydivinyltriamineguanidine, aluminate coupling agent and silane coupling agent into a kneading machine, and stirring for 0.5-1 hour without heating;
2) heating, stirring and heating the materials to 80-120 ℃, vacuumizing, preserving heat and stirring for 0.5-1 hour;
3) adding white carbon black, hydroxyl silicone oil, diatomite, dimethyl silicone oil and a release agent into the materials, heating to 140-160 ℃, preserving heat and stirring for 0.5-1 hour to obtain a silicone rubber material;
4) keeping the temperature of the materials, vacuumizing and stirring for 0.5-1 hour;
5) and adding the silicon rubber material and a vulcanizing agent 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane into an open rubber mixing mill, uniformly mixing, and then placing the mixture into a flat vulcanizing machine to vulcanize for 5 minutes at 175 ℃ to prepare the antibacterial silicon rubber.
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| CN202010949845.0A CN112063180A (en) | 2020-09-10 | 2020-09-10 | Antibacterial and mildew-proof high-temperature vulcanized silicone rubber and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114316604A (en) * | 2021-12-29 | 2022-04-12 | 广东天跃新材料股份有限公司 | Mildew-proof antibacterial silicone rubber fabric and production process thereof |
| CN115895276A (en) * | 2022-12-10 | 2023-04-04 | 宁波韩太硅胶制品有限公司 | Food-grade antibacterial mildew-proof synthetic high-temperature vulcanized silicone rubber and preparation method thereof |
| CN117534962A (en) * | 2023-09-27 | 2024-02-09 | 广东阿普邦新材料科技股份有限公司 | Wear-resistant antibacterial silica gel and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114316604A (en) * | 2021-12-29 | 2022-04-12 | 广东天跃新材料股份有限公司 | Mildew-proof antibacterial silicone rubber fabric and production process thereof |
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| CN117534962A (en) * | 2023-09-27 | 2024-02-09 | 广东阿普邦新材料科技股份有限公司 | Wear-resistant antibacterial silica gel and preparation method thereof |
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