CN112063177A - 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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- CN112063177A CN112063177A CN202010949090.4A CN202010949090A CN112063177A CN 112063177 A CN112063177 A CN 112063177A CN 202010949090 A CN202010949090 A CN 202010949090A CN 112063177 A CN112063177 A CN 112063177A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/0806—Silver
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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Abstract
The invention discloses an antibacterial mildew-proof high-temperature vulcanized silicone rubber and a preparation method thereof. The antibacterial mildew-proof high-temperature vulcanized silicone rubber has good physical and mechanical properties and processability, meets various characteristics of the traditional high-temperature vulcanized silicone rubber, has good killing and inhibiting effects on fungi, bacteria, mildew and enzyme bacteria, is long in duration, good in broad-spectrum property, safe and environment-friendly, does not generate drug resistance, and is wider in application range.
Description
Technical Field
The invention relates to the manufacture of silicon rubber compound, in particular to antibacterial mildew-proof high-temperature vulcanized silicon rubber and a preparation method thereof, belonging to the field of rubber material manufacture.
Background
The silicon rubber products are widely applied, and with the continuous improvement of living standard, the market demand of functional silicon rubber products is more and more increased, wherein the antibacterial property of the silicon rubber products in the fields of industrial production, medical treatment and health care, civil health care and the like has higher requirements, such as machine tool equipment, surgical instruments, medical supplies, artificial organs, using vessels and the like. The silicon rubber is divided into a heat vulcanization type (high temperature vulcanized silicon rubber HTV) and a room temperature vulcanization type (RTV) according to a vulcanization mode and a vulcanization temperature. The room temperature vulcanized silicone rubber can be crosslinked and cured at normal temperature, is fluid or viscous paste in a physical normal state, and is often used for adhesives, sealants, protective coatings, potting materials, low temperature mold manufacturing and the like. The high-temperature vulcanized silicone rubber has excellent mechanical and physical properties and high temperature resistance, can obtain corresponding different characteristics by adding different additives, has wide application compared with the room-temperature silicone rubber, and is suitable for the preparation of silicone rubber products in various industries.
The continuous development of economic society, people's antibiotic mould proof requirement to production, life is increasing day by day. The antibacterial material is used as a novel functional material, and can effectively inhibit microorganisms harmful to human bodies, such as bacteria, germs and the like in the surrounding environment; therefore, the antibacterial mildew-proof silicone rubber material obtained by combining the antibacterial effect with the silicone rubber, which has the advantages of obvious long-acting effect, wide application range, safety and environmental protection, becomes a hot spot in the field at present. At present, most of the produced antibacterial and mildewproof silicon rubber has the defects of short antibacterial duration, single antibacterial property, easy generation of drug resistance and the like; meanwhile, the defects of insufficient mechanical and physical properties, narrow application range and the like of the antibacterial and mildewproof room-temperature silicone rubber limit the operation environment and cannot meet the requirements of large-scale production and living.
Aiming at the problems in the preparation of the antibacterial and mildewproof silicon rubber, the invention adopts fumed silica with large specific surface area and good reinforcing property and a mixed antibacterial agent with the characteristics of high sterilization rate, large broad spectrum, safety, environmental protection, no drug resistance and the like, and the antibacterial and mildewproof high-temperature vulcanized silicon rubber is obtained by fully mixing the raw rubber with the methyl vinyl silicon rubber. The silver-loaded antibacterial agent in the mixed antibacterial agent integrates two characteristics of silver ion sterilization and titanium dioxide photocatalytic sterilization, the guanidine salt antibacterial agent has the characteristics of long duration time of the organic antibacterial agent and difficulty in generating drug-resistant bacteria, the high sterilization rate of the silicone rubber is ensured, the antibacterial broad-spectrum property is enhanced, the drug resistance is avoided, the mechanical and physical properties of the silicone rubber are improved, and the use is wide.
Disclosure of Invention
The invention provides a preparation method of antibacterial and mildewproof high-temperature vulcanized silicone rubber, aiming at the problems that the antibacterial duration is short, the antibacterial property is single, the drug resistance is easy to generate and the like in the preparation of the antibacterial and mildewproof silicone rubber, and the defects that the antibacterial and mildewproof room-temperature silicone rubber is insufficient in mechanical and physical properties, narrow in application range and the like.
The invention is carried out by the following technical scheme:
the antibacterial and mildewproof high-temperature vulcanized silicone rubber comprises the following components in parts by weight:
the antibacterial and mildewproof high-temperature vulcanized silicone rubber comprises the following preparation steps:
adding methyl vinyl polysiloxane and zinc stearate into a kneader, and stirring for 5 min; adding fumed silica and structure control agent 4-6 times, and stirring thoroughly after each addition; and then mixing and stirring the silver-loaded nano titanium dioxide and the polyhexamethylene biguanide hydrochloride with KH-151 and KH-560 silane coupling agents uniformly, adding the mixture, kneading the mixture for molding, heating the mixture to 140-165 ℃, kneading the mixture for 1-2h, keeping the temperature, vacuumizing the mixture for 15-45min, introducing cooling water to reduce the temperature to below 80 ℃, discharging the material, cooling the material to room temperature, and filtering the material to obtain the silicon rubber compound.
The antibacterial and mildewproof high-temperature vulcanized silicone rubber has the advantages that the vinyl content in the methyl vinyl polysiloxane is 0.03-3.0%, and the molecular weight of raw rubber is 50-70 ten thousand.
According to the antibacterial mildew-proof high-temperature vulcanized silicone rubber, the fumed silica is added according to the sequence of 40%, 20%, 10% and 10% of the total amount respectively, and the BET specific surface area of the fumed silica is 200 +/-20 m2/g。
The antibacterial mildew-proof high-temperature vulcanized silicone rubber comprises one or two of dimethyl organo silane, hexamethyldisilazane and hydroxyl silicone oil as a structural control agent. The structure control agent and the fumed silica according to a mass ratio of 4: adding in the ratio of 100-10: 100.
The antibacterial and mildewproof high-temperature vulcanized silicone rubber has the advantages that the content of silver-loaded nano titanium dioxide nano silver is 2.0 percent, and the average particle size is 30 +/-10 nm; the effective content of the polyhexamethylene biguanide hydrochloride is more than 98 percent; the adding proportion of the silver-loaded nano titanium dioxide and the polyhexamethylene biguanide hydrochloride PHMB is 3:2 by mass.
The antibacterial mildew-proof high-temperature vulcanized silicone rubber comprises the silane coupling agents KH-151 and KH-560 which are added according to the mass ratio of 1:1, wherein the KH-151 is vinyl triethoxysilane, and the KH-560 is gamma-glycidyl ether oxypropyl trimethoxysilane.
Compared with the prior art, the method has the following advantages and technical effects: aiming at the defects of short antibacterial duration time, single antibacterial property, easy generation of drug resistance and the like of most of the existing antibacterial silicone rubber and insufficient mechanical and physical properties of the antibacterial and mildewproof room-temperature silicone rubber, the antibacterial and mildewproof high-temperature vulcanized silicone rubber adopts an antibacterial agent which combines a silver-loaded nano titanium dioxide antibacterial agent and a polyhexamethylene biguanide hydrochloride antibacterial agent. The silver-loaded nano titanium dioxide integrates the advantages of silver ion type and titanium dioxide photocatalysis antibacterial agents, avoids the influence of the color of a common silver-loaded antibacterial material, and does not need to be limited under the ultraviolet irradiation condition as the traditional titanium antibacterial agent; the polyhexamethylene biguanide hydrochloride belongs to an organic polymer, can form a bonding effect with silicon rubber, is not easy to separate out, has a long sterilization lasting effect, and is safe and environment-friendly; meanwhile, the antibacterial and mildewproof high-temperature vulcanized silicone rubber keeps the mechanical and physical performance advantages of the high-temperature vulcanized silicone rubber, meets the requirements of production and life in various aspects, and is wide in usability.
Detailed Description
The following is a more detailed description of the embodiments of the present invention with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
100 parts of methyl vinyl polysiloxane with 0.10 mol percent of vinyl and 60 ten thousand of molecular weight and 0.3 part of zinc stearate are added into a kneader and stirred for 5 minutes; then adding 40 parts of fumed silica and 2 parts of hydroxyl silicone oil for 4 times, and fully stirring after each addition; then adding 1.2 parts of silver-loaded nano titanium dioxide, 0.8 part of polyhexamethylene biguanide hydrochloride, 0.25 part of KH-151 and 0.25 part of KH-560 respectively, kneading and forming, heating to 150 ℃, kneading for 1 hour, keeping the temperature, vacuumizing and heating for 0.5 hour, introducing cooling water to reduce the temperature to below 80 ℃, discharging, cooling to room temperature, and filtering to obtain the silicon rubber compound.
1.5 percent of dipenta-vulcanizing agent is uniformly added into the rubber compound by an open mill, weighed and then placed into a mold for vulcanization, and the vulcanization is carried out for 5 minutes at 175 ℃.
Example 2
100 parts of methyl vinyl polysiloxane with 0.12 percent of vinyl mole percentage content and 60 ten thousand of molecular weight and 0.3 part of zinc stearate are added into a kneader and stirred for 5 minutes; adding 50 parts of fumed silica and 3 parts of hydroxyl silicone oil for 5 times, and fully stirring after each addition; then adding 2.4 parts of silver-loaded nano titanium dioxide, 1.6 parts of polyhexamethylene biguanide hydrochloride, KH-151 and KH-560 which are mixed well into the mixture, kneading and forming, heating to 150 ℃, kneading for 1.5 hours, keeping the temperature, vacuumizing and cooking for 40 minutes, cooling to below 80 ℃ by cooling water, discharging, cooling to room temperature and filtering to obtain the silicon rubber compound.
1.5 percent of dipenta-vulcanizing agent is uniformly added into the rubber compound by an open mill, weighed and then placed into a mold for vulcanization, and the vulcanization is carried out for 5 minutes at 175 ℃.
Example 3
100 parts of methyl vinyl polysiloxane with 0.16 mol percent of vinyl and 65 ten thousand of molecular weight and 0.3 part of zinc stearate are added into a kneader and stirred for 5 minutes; adding 70 parts of fumed silica and 5 parts of hydroxy silicone oil for 6 times, and fully stirring after each addition; then adding 3 parts of silver-loaded nano titanium dioxide, 2 parts of polyhexamethylene biguanide hydrochloride, KH-151 and KH-560 which are respectively 0.5 part of mixed paste, kneading and forming, heating to 150 ℃, kneading for 1 hour, keeping the temperature, vacuumizing and cooking for 15 minutes, introducing cooling water to reduce the temperature to below 80 ℃, discharging, cooling to room temperature and filtering to obtain the silicon rubber compound.
Uniformly adding 1.2% of DCP vulcanizing agent into the rubber compound by using an open mill, weighing, placing the mixture into a mould for vulcanization, and vulcanizing for 5 minutes at 160 ℃.
The mechanical and physical properties and bacteriostatic effect data of the antibacterial and mildewproof high-temperature vulcanized silicone rubber prepared by the invention are as follows:
| test items | Unit of | Example 1 | Example 2 | Example 3 |
| Hardness of | Shore A +/-2 | 45 | 55 | 70 |
| Tensile strength | MPa | 8.5 | 9.0 | 8.8 |
| Elongation at break | ％ | 630 | 500 | 420 |
| Tear strength | kN/m | 28 | 30 | 25 |
| Rate of inhibition of bacteria | 88％ | 95％ | 100％ |
Claims (10)
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 raw silicon rubber is 110-2 methyl vinyl silicon rubber, the vinyl content is 0.03-3.0%, and the molecular weight is 50-70 ten thousand.
3. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the release agent is zinc stearate.
4. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the structural control agent is one or two of dimethyl organic silicane, hexamethyl disilazane and hydroxyl silicone oil.
5. The antibacterial and mildewproof high-temperature vulcanized silicone rubber as set forth in claim 1, wherein: the release agent is zinc stearate.
6. A preparation method of antibacterial mildew-proof high-temperature vulcanized silicone rubber is characterized by adding 100 parts of raw silicone rubber and 0.3-1.2 parts of a release agent into a kneader under normal temperature conditions, stirring for 5 minutes, adding 40-70 parts of fumed silica, stirring and mixing, adding 2-8 parts of a structural control agent after 4-6 times of addition of the fumed silica, adding 2-10 parts of a mixed antibacterial agent and 0.5-2 parts of a silane coupling agent, kneading and forming at the temperature of below 90 ℃, heating to 140 ℃ and 165 ℃ for treatment for 1-2 hours, vacuumizing for 15-45 minutes, cooling to the temperature of below 80 ℃, discharging, cooling to room temperature, and filtering to obtain a silicone rubber compound.
7. 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: the white carbon black is added according to the sequence of 40%, 30%, 20% and 10% of the total amount respectively by the gas phase method, and the BET specific surface area of the white carbon black is 200 +/-20 m2/g。
8. 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: the structure control agent and the white carbon black are mixed according to the mass ratio of 4: adding in the ratio of 100-10: 100.
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: the antibacterial agent is silver-loaded nano titanium dioxide and polyhexamethylene biguanide hydrochloride PHMB, and the addition proportion is 3: 2. The content of the silver-loaded nano titanium dioxide nano silver is 2.0 percent, and the average grain diameter is 30 +/-10 nm; the effective content of the polyhexamethylene biguanide hydrochloride is more than 98 percent.
10. 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: the silane coupling agent is KH-151 and KH-560, the adding proportion is 1:1 by mass, the KH-151 is vinyl triethoxysilane, and the KH-560 is gamma-glycidoxypropyltrimethoxysilane.
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Cited By (8)
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| CN112795195A (en) * | 2021-02-02 | 2021-05-14 | 深圳深凯硅胶制品有限公司 | Wear-resistant antibacterial silica gel and preparation method thereof |
| CN112876851A (en) * | 2021-02-02 | 2021-06-01 | 深圳深凯硅胶制品有限公司 | Medical antibacterial sealing element and preparation method thereof |
| CN113308033A (en) * | 2021-06-11 | 2021-08-27 | 厦门鑫鹭耀橡塑有限公司 | Antibacterial rubber gasket and preparation method thereof |
| 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 |
| CN115725184A (en) * | 2022-11-28 | 2023-03-03 | 东莞市贝特利新材料有限公司 | Antibacterial self-adhesive addition type organic silicon rubber composition and preparation method 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 |
| CN116023784A (en) * | 2021-10-25 | 2023-04-28 | Oppo广东移动通信有限公司 | Antibacterial silicone rubber, silicone rubber product and method thereof, wearing product and antibacterial material |
| CN116162355A (en) * | 2023-02-03 | 2023-05-26 | 昆山力普电子橡胶有限公司 | Antibacterial silica gel and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795195A (en) * | 2021-02-02 | 2021-05-14 | 深圳深凯硅胶制品有限公司 | Wear-resistant antibacterial silica gel and preparation method thereof |
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| CN113308033A (en) * | 2021-06-11 | 2021-08-27 | 厦门鑫鹭耀橡塑有限公司 | Antibacterial rubber gasket and preparation method thereof |
| CN116023784A (en) * | 2021-10-25 | 2023-04-28 | Oppo广东移动通信有限公司 | Antibacterial silicone rubber, silicone rubber product and method thereof, wearing product and antibacterial material |
| 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 |
| CN115725184A (en) * | 2022-11-28 | 2023-03-03 | 东莞市贝特利新材料有限公司 | Antibacterial self-adhesive addition type organic silicon rubber composition and preparation method 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 |
| CN116162355A (en) * | 2023-02-03 | 2023-05-26 | 昆山力普电子橡胶有限公司 | Antibacterial silica gel and preparation method thereof |
| CN116162355B (en) * | 2023-02-03 | 2023-12-05 | 昆山力普电子橡胶有限公司 | Antibacterial silica gel and preparation method thereof |
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Application publication date: 20201211 |