CN110776867A - Antibacterial silane polyether adhesive and preparation method thereof - Google Patents
Antibacterial silane polyether adhesive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
- C09J171/02—Polyalkylene oxides
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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- C08K3/20—Oxides; Hydroxides
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K3/24—Acids; Salts thereof
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- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention discloses an antibacterial silane polyether adhesive which is mainly prepared from silane modified polyether resin, a filler, a solvent, a reinforcing agent, a light stabilizer, an antioxidant, a water removing agent, a catalyst, a coupling agent and an antibacterial agent; the phosphate double-salt antibacterial agent with good compatibility with the silane polyether adhesive is prepared, and the modified polysiloxane (fatty acid substance) with high surface energy is introduced into the silane polyether adhesive, so that the surface energy of the silane polyether adhesive is effectively improved, and the bonding performance is improved. The invention also discloses a preparation method of the antibacterial silane polyether adhesive, which is simple and suitable for popularization.
Description
Technical Field
The invention belongs to the field of polyether adhesives, and particularly relates to an antibacterial silane polyether adhesive and a preparation method thereof.
Background
The modified silane polyether adhesive is a new generation of building sealant developed after polysulfide adhesive, silicone adhesive and polyurethane adhesive. In the silane terminated polyether molecule, because the contained Si-C bond has hydrophobicity, the silane terminated polyether sealant has lower sensitivity to moisture compared with the common polyurethane sealant system, and the storage stability of the sealant is greatly improved. Because the cured crosslinking structure contains Si-O-Si bonds, the silane-terminated polyether sealant has the characteristics of excellent weather resistance, water resistance, chemical medium resistance, antifreezing solution resistance, fuel oil resistance, mechanical transmission oil resistance, heat resistance and the like. The silane terminated polyether sealant system has no free isocyanate, no pollutant cured exudate escaping and no pollution to the surface and periphery of the stuck substrate. It also has excellent painting properties. The silane terminated polyether sealant has the advantages that the adhesion range of the silane terminated polyether sealant without primer is expanded from the adhesion of common building materials (such as metal, glass, masonry and the like) to the adhesion of substrates such as PVC, ABS, polystyrene, polyacrylate and the like and various paint surfaces (including polyacrylic acid type, epoxy type, polyurethane type and enamel paint type paint surfaces), and good adhesion effect is achieved.
The conventional silane-terminated polyether adhesive has poor antibacterial ability and unstable adhesive property, and needs to be improved.
Disclosure of Invention
The invention aims to solve the technical problem of providing an antibacterial silane polyether adhesive which has good adhesive property and antibacterial property.
The invention also aims to solve the technical problem of providing a preparation method of the antibacterial silane polyether adhesive, which is simple.
In order to solve the technical problems, the invention provides an antibacterial silane polyether adhesive which is mainly prepared from the following raw materials in percentage by weight: 20-30% of silane modified polyether resin, 50-60% of filler, 5-10% of solvent, 5-10% of reinforcing agent, 1-2% of light stabilizer, 1-2% of antioxidant, 1-2% of water removing agent, 1-3% of catalyst, 1-3% of coupling agent and 1-3% of antibacterial agent;
the preparation method of the antibacterial agent comprises the following steps:
(1) adding 5-15 parts of zinc oxide and 5-15 parts of calcium carbonate into 40-60 parts of phosphoric acid solution, and stirring for reaction for 0.5-1 h; obtaining a first mixed solution;
(2) dispersing 0.1-2 parts of silver powder and 0.1-2 parts of cerium oxide powder into water to obtain a second mixed solution;
(3) cooling the first mixed solution to 25-35 ℃ and then mixing the first mixed solution with the second mixed solution; adding 10-15 parts of diatomite and 2-5 parts of bentonite; and ball milling to obtain the finished product of the antibacterial agent.
As an improvement of the technical scheme, the reinforcing agent is modified polysiloxane; the modified polysiloxane is prepared from the following raw materials in parts by weight: 70-80 parts of methyl epoxy silane, 5-10 parts of gamma-aminopropyl methyl diethoxy silane, 1-2 parts of potassium hydroxide, 1-2 parts of acetic acid, 5-15 parts of soybean fatty acid and 1-2 parts of toluene;
the preparation method of the modified polysiloxane comprises the following steps:
(1) mixing methyl epoxy silane, gamma-aminopropyl methyl diethoxy silane and potassium hydroxide, heating to 140 ℃ and 150 ℃, reacting for 20-60 minutes, and adding acetic acid for neutralization to obtain an intermediate product;
(2) mixing the intermediate product with soybean fatty acid and toluene, reacting at the temperature of 150-160 ℃ for 0.5-1h, and distilling to obtain the modified polysiloxane.
As an improvement of the technical scheme, the coupling agent is a mixture of gamma-aminopropyltriethoxysilane, N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane and gamma-mercaptopropyltriethoxysilane, and the weight ratio of the gamma-aminopropyltriethoxysilane to the N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane to the gamma-mercaptopropyltriethoxysilane is (1-2): 0.5-1): 0.8-1);
as an improvement of the technical scheme, the filler is one or a combination of light calcium carbonate, heavy calcium carbonate, kaolin, talcum powder and wollastonite powder.
As an improvement of the technical scheme, the filler is a combination of light calcium carbonate, kaolin and talcum powder, and the weight ratio of the light calcium carbonate to the kaolin to the talcum powder is as follows: kaolin: talcum powder (2-5): (1-2): (0.1-0.5).
As an improvement of the technical scheme, the silane modified polyether resin is one or a combination of dimethoxy silyl terminated polyether and triethoxy silyl terminated polyether.
As an improvement of the technical scheme, the solvent is one or a combination of polybasic alcohol acid esters and polyoxypropylene glycol.
As an improvement of the technical scheme, the light stabilizer is at least one of salicylate, benzophenone, benzotriazole, triazine, substituted acrylonitrile and hindered amine light stabilizer.
As an improvement of the technical scheme, the antioxidant is at least one of hindered phenol antioxidant, phosphite antioxidant, thioester antioxidant and composite antioxidant.
Correspondingly, the invention also discloses a method for preparing the antibacterial silane polyether adhesive, which specifically comprises the following steps:
(1) preparing modified polysiloxane and antibacterial agent;
(2) adding the silane modified polyether resin, the filler, the solvent, the light stabilizer, the antioxidant and the antibacterial agent into a stirring cylinder, and vacuumizing and stirring for 4-6 hours at 80-120 ℃ to obtain a mixture; wherein the vacuum degree is 0.085-0.09 MPa;
(3) cooling the mixture to 20-40 ℃, adding a reinforcing agent, a dehydrating agent and a coupling agent, vacuumizing and stirring for 0.2-2h to obtain a finished product; wherein the vacuum degree is 0.085-0.09 MPa.
The invention provides an antibacterial silane polyether adhesive, which greatly improves the bonding and antibacterial properties of the silane polyether adhesive through the prepared antibacterial agent and reinforcing agent; the technical scheme of the invention has the following beneficial effects:
1. the polysiloxane (fatty acid substance) with high surface energy is prepared and introduced into the silane polyether adhesive, so that the surface energy of the silane polyether adhesive can be effectively improved, and the bonding performance of the silane polyether adhesive is improved; meanwhile, the fatty acid substance has good compatibility with the phosphate double salt, and is beneficial to the full dispersion of the sterilizing agent.
2. The silver and cerium sterilizing agent loaded with calcium magnesium phosphate is prepared, has strong sterilizing capability and strong compatibility with the silane polyether adhesive.
3. According to the invention, through the matching of the coupling agent, the surface tension is effectively improved, the wettability of an adherend is improved, and the bonding performance of the silane polyether adhesive is improved.
4. The preparation method is simple, and the range of the raw materials can be selected widely.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below.
The invention provides an antibacterial silane polyether adhesive which is mainly prepared from the following raw materials in percentage by weight: 20-30% of silane modified polyether resin, 50-60% of filler, 5-10% of solvent, 5-10% of reinforcing agent, 1-2% of light stabilizer, 1-2% of antioxidant, 1-2% of water removing agent, 1-3% of catalyst, 1-3% of coupling agent and 1-3% of antibacterial agent;
wherein, the reinforcing agent is selected from modified polysiloxane; the modified polysiloxane is prepared from the following raw materials in parts by weight: 70-80 parts of methyl epoxy silane, 5-10 parts of gamma-aminopropyl methyl diethoxy silane, 1-2 parts of potassium hydroxide, 1-2 parts of acetic acid, 5-15 parts of soybean fatty acid and 1-2 parts of toluene;
the preparation method of the modified polysiloxane comprises the following steps:
(1) mixing methyl epoxy silane, gamma-aminopropyl methyl diethoxy silane and potassium hydroxide, heating to 140 ℃ and 150 ℃, reacting for 20-60 minutes, and adding acetic acid for neutralization to obtain an intermediate product;
(2) mixing the intermediate product with soybean fatty acid and toluene, reacting at the temperature of 150-160 ℃ for 0.5-1h, and distilling to obtain the modified polysiloxane.
According to the invention, methyl epoxy silane is selected as a matrix, and under the action of a coupling agent gamma-aminopropyl methyl diethoxy silane, a fatty acid substance is grafted to the structure of the methyl epoxy silane, so that a modified polysiloxane substance is obtained; the silane polyether adhesive has higher surface energy, and after a silane polyether adhesive system is added, the system surface energy of the silane polyether adhesive can be effectively improved, and the bonding performance of the silane polyether adhesive is improved; it should be noted that, although fatty acids have high surface energy, because they are incompatible with silane polyether colloid system, the present invention grafts fatty acid group to methyl epoxy silane structure; preferably, the methyl alkylene oxide in the present invention is octamethylcyclotetrasiloxane. In addition, the modified polysiloxane substance prepared by the method has good compatibility with the antimicrobial agent phosphate double salt, and can promote good dispersion of the antimicrobial agent and improve the antimicrobial effect.
Wherein the preparation method of the antibacterial agent comprises the following steps:
(1) adding 5-15 parts of zinc oxide and 5-15 parts of calcium carbonate into 40-60 parts of phosphoric acid solution, and stirring for reaction for 0.5-1 h; obtaining a first mixed solution;
(2) dispersing 0.1-2 parts of silver powder and 0.1-2 parts of cerium oxide powder into water to obtain a second mixed solution;
(3) cooling the first mixed solution to 25-35 ℃ and then mixing the first mixed solution with the second mixed solution; adding 10-15 parts of diatomite and 2-5 parts of bentonite; and ball milling to obtain the finished product of the antibacterial agent.
The calcium carbonate, the zinc oxide and the phosphoric acid solution react to form a double-phosphate base body with a supporting function, so that the silver powder, the cerium oxide powder and the diatomite are uniformly loaded on the double-phosphate base body to fully play a role in disinfection, and meanwhile, the double-phosphate and the silane polyether adhesive have good compatibility and can be uniformly dispersed in the silane polyether. The silver-phosphate composite system antibacterial agent adopted by the invention mainly has the effects of killing viruses by the silver powder and the cerium oxide, the silver powder can kill most common bacteria, the generation content of hydroxyl free radicals can be effectively increased by adding the transition metal cerium oxide, the antibacterial effect of the antibacterial agent is enhanced, and meanwhile, the using amount of the silver powder which is a more expensive raw material can be reduced.
The curing agent is one or a mixture of gamma-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, N- (β -aminoethyl) -gamma-aminopropyl trimethoxysilane, N- (β -aminoethyl) -gamma-aminopropyl methyl dimethoxysilane and gamma-mercaptopropyl triethoxysilane, preferably, the mixture of gamma-aminopropyl triethoxysilane, N- (β -aminoethyl) -gamma-aminopropyl trimethoxysilane and gamma-mercaptopropyl triethoxysilane is used as the coupling agent, the mixture of monoamino gamma-aminopropyl triethoxysilane and diamino N- (β -aminoethyl) -gamma-aminopropyl trimethoxysilane can effectively accelerate the reaction speed of the silane polyether adhesive, the thiosilane coupling agent and gamma-mercaptopropyl triethoxysilane can effectively accelerate the elongation and the tensile strength of the silane polyether adhesive, the combination of the three can effectively accelerate the various properties of the silane polyether adhesive, preferably, the gamma-aminopropyl triethoxysilane and N- (β -aminoethyl) -gamma-aminopropyl triethoxysilane can effectively accelerate the elongation and the tensile strength of the silane adhesive, the preferable mechanical strength of the silane adhesive is still more than 0.1.1.1.1.0.1-0.2.1.1.1.1.0.0.2-mercaptopropyl triethoxysilane (1.1.1.1.1.1.0.1.1.0.0.0.0.1 MPa) and the preferable mechanical strength of the adhesive can be improved by one month by one by three by one by three.
Wherein, the filler is one or a combination of nano calcium carbonate, light calcium carbonate, heavy calcium carbonate, kaolin, talcum powder, wollastonite powder and fly ash; preferably, light calcium carbonate, heavy calcium carbonate, kaolin and talcum powder are selected; preferably, the filler is a combination of light calcium carbonate, kaolin and talcum powder, and the weight ratio of the light calcium carbonate to the kaolin to the talcum powder is (2-5) to (1-2) to (0.1-0.5).
Wherein, the silane modified polyether resin is one or the combination of dimethoxy silyl terminated polyether and triethoxy silyl terminated polyether; the solvent is one or a combination of polybasic alcohol acid esters and polyoxypropylene glycol; the solvent can improve the viscosity of the silane polyether adhesive and also has a certain effect of increasing plasticity.
Wherein the light stabilizer is at least one of salicylate, benzophenone, benzotriazole, triazine, substituted acrylonitrile and hindered amine light stabilizer. The antioxidant is at least one of hindered phenol antioxidant, phosphite antioxidant, thioester antioxidant and composite antioxidant. The water removing agent is oxazolidine cross-linking agent; the catalyst is one or a mixture of dibutyltin diacetate and dibutyltin dilaurate.
Correspondingly, the invention also discloses a preparation method of the antibacterial silane polyether adhesive, which comprises the following steps:
(1) preparing modified polysiloxane and antibacterial agent;
(2) adding the silane modified polyether resin, the filler, the solvent, the light stabilizer and the antioxidant into a stirring cylinder, and vacuumizing and stirring for 4-6 hours at 80-120 ℃ to obtain a mixture; wherein the vacuum degree is 0.085-0.09 MPa;
(3) cooling the mixture to 20-40 ℃, adding a reinforcing agent, a dehydrating agent and a coupling agent, vacuumizing and stirring for 0.2-2h to obtain a finished product; wherein the vacuum degree is 0.085-0.09 MPa.
The following description is given by way of specific examples:
example 1
The formula of the silane polyether adhesive comprises:
the formula of the modified polysiloxane comprises the following components:
| raw materials | Dosage (parts) |
| Methyl epoxy silane | 72 |
| Gamma-aminopropylmethyldiethoxysilane | 6 |
| Potassium hydroxide | 1 |
| Acetic acid | 1 |
| Soybean fatty acid | 12 |
| Toluene | 1 |
The formula of the antibacterial agent is as follows:
the preparation method comprises the following steps:
(1) preparation of modified polysiloxane:
A. mixing methyl epoxy silane, gamma-aminopropyl methyl diethoxy silane and potassium hydroxide, heating to 145 ℃ for reaction for 26 minutes, and adding acetic acid for neutralization to obtain an intermediate product;
B. and mixing the intermediate product with soybean fatty acid and toluene, reacting at 155 ℃ for 0.5h, and distilling to obtain the modified polysiloxane.
(2) Preparation of antibacterial agent
C. Adding zinc oxide and calcium carbonate into a phosphoric acid solution, and stirring for reaction for 0.5 h; obtaining a first mixed solution;
D. dispersing silver powder and cerium oxide powder into water to obtain a second mixed solution;
E. cooling the first mixed solution to 25 ℃ and then mixing the first mixed solution with the second mixed solution; adding diatomite and bentonite; and ball milling to obtain the finished product of the antibacterial agent.
(3) Adding the silane modified polyether resin, the filler, the solvent, the light stabilizer and the antioxidant into a stirring cylinder, and vacuumizing and stirring for 4 hours at 80 ℃ to obtain a mixture; wherein the vacuum degree is 0.085 MPa;
(4) cooling the mixture to 20 ℃, adding a reinforcing agent, a dehydrating agent and a coupling agent, and vacuumizing and stirring for 0.2h to obtain a finished product; wherein the vacuum degree is 0.085 MPa.
Example 2
The formula of the silane polyether adhesive comprises:
the formula of the modified polysiloxane comprises the following components:
| raw materials | Dosage (parts) |
| Methyl epoxy silane | 78 |
| Gamma-aminopropylmethyldiethoxysilane | 7 |
| Potassium hydroxide | 1.5 |
| Acetic acid | 2 |
| Soybean fatty acid | 13 |
| Toluene | 1 |
The formula of the antibacterial agent is as follows:
| raw materials | Dosage (parts) |
| Zinc oxide | 15 |
| Calcium carbonate | 15 |
| Phosphoric acid | 60 |
| Silver (Ag) | 2 |
| Cerium oxide | 2 |
| Diatomite | 15 |
The preparation method comprises the following steps:
(1) preparation of modified polysiloxane:
A. mixing methyl epoxy silane, gamma-aminopropyl methyl diethoxy silane and potassium hydroxide, heating to 145 ℃ for reacting for 40 minutes, and adding acetic acid for neutralizing to obtain an intermediate product;
B. and mixing the intermediate product with soybean fatty acid and toluene, reacting at 150 ℃ for 0.8h, and distilling to obtain the modified polysiloxane.
(2) Preparation of antibacterial agent
C. Adding zinc oxide and calcium carbonate into a phosphoric acid solution, and stirring for reaction for 0.8 h; obtaining a first mixed solution;
D. dispersing silver powder and cerium oxide powder into water to obtain a second mixed solution;
E. cooling the first mixed solution to 30 ℃ and then mixing the first mixed solution with the second mixed solution; adding diatomite and bentonite; and ball milling to obtain the finished product of the antibacterial agent.
(3) Adding the silane modified polyether resin, the filler, the solvent, the light stabilizer and the antioxidant into a stirring cylinder, and vacuumizing and stirring for 6 hours at 120 ℃ to obtain a mixture; wherein the vacuum degree is 0.09 MPa;
(4) cooling the mixture to 40 ℃, adding a reinforcing agent, a dehydrating agent and a coupling agent, and vacuumizing and stirring for 2 hours to obtain a finished product; wherein the vacuum degree is 0.09 MPa.
Example 3
The formula of the silane polyether adhesive comprises:
the formula of the modified polysiloxane comprises the following components:
| raw materials | Dosage (parts) |
| Methyl epoxy silane | 75 |
| Gamma-aminopropylmethyldiethoxysilane | 8 |
| Potassium hydroxide | 1 |
| Acetic acid | 1 |
| Soybean fatty acid | 10 |
| Toluene | 1 |
The formula of the antibacterial agent is as follows:
the preparation method comprises the following steps:
(1) preparation of modified polysiloxane:
A. mixing methyl epoxy silane, gamma-aminopropyl methyl diethoxy silane and potassium hydroxide, heating to 145 ℃ for reaction for 30 minutes, and adding acetic acid for neutralization to obtain an intermediate product;
B. and mixing the intermediate product with soybean fatty acid and toluene, reacting at 155 ℃ for 0.5h, and distilling to obtain the modified polysiloxane.
(2) Preparation of antibacterial agent
C. Adding zinc oxide and calcium carbonate into a phosphoric acid solution, and stirring for reaction for 0.6 h; obtaining a first mixed solution;
D. dispersing silver powder and cerium oxide powder into water to obtain a second mixed solution;
E. cooling the first mixed solution to 30 ℃ and then mixing the first mixed solution with the second mixed solution; adding diatomite and bentonite; and ball milling to obtain the finished product of the antibacterial agent.
(3) Adding the silane modified polyether resin, the filler, the solvent, the light stabilizer and the antioxidant into a stirring cylinder, and vacuumizing and stirring for 5 hours at 100 ℃ to obtain a mixture; wherein the vacuum degree is 0.09 MPa;
(4) cooling the mixture to 35 ℃, adding a reinforcing agent, a dehydrating agent and a coupling agent, and vacuumizing and stirring for 0.5h to obtain a finished product; wherein the vacuum degree is 0.09 MPa.
Comparative example 1
The formula of the silane polyether adhesive does not contain modified polysiloxane and an antibacterial agent, the preparation method does not comprise the step of preparing the modified polysiloxane, and the rest is the same as that of the silane polyether adhesive in the embodiment 3.
Comparative example 2
The coupling agent in the formula of the silane polyether adhesive adopts gamma-aminopropyltriethoxysilane, namely N- (β -aminoethyl) -gamma-aminopropyltrimethoxysilane, namely 1: 1, and the formula does not contain an antibacterial agent, and the rest is the same as that in the example 3.
The antibacterial silane polyether adhesives in examples 1-3 and comparative examples 1-2 were tested according to the method of GB 16776-:
TABLE 1 results of adhesion Properties test
The antibacterial silane polyether adhesives of examples 1-3 and comparative examples 1-2 were tested according to the method of QB/T2591-2003, wherein a plastic sheet was used as a substrate, and the results are shown in Table 2:
TABLE 2 results of antibacterial and antifungal tests
As can be seen from tables 1 and 2, the silane polyether adhesive has good adhesive property and antibacterial property, and other indexes of the silane polyether adhesive meet the relevant requirements of national standards.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (10)
1. The antibacterial silane polyether adhesive is characterized by mainly comprising the following raw materials in percentage by weight: 20-30% of silane modified polyether resin, 50-60% of filler, 5-10% of solvent, 5-10% of reinforcing agent, 1-2% of light stabilizer, 1-2% of antioxidant, 1-2% of water removing agent, 1-3% of catalyst, 1-3% of coupling agent and 1-3% of antibacterial agent;
the preparation method of the antibacterial agent comprises the following steps:
(1) adding 5-15 parts of zinc oxide and 5-15 parts of calcium carbonate into 40-60 parts of phosphoric acid solution, and stirring for reaction for 0.5-1 h; obtaining a first mixed solution;
(2) dispersing 0.1-2 parts of silver powder and 0.1-2 parts of cerium oxide powder into water to obtain a second mixed solution;
(3) cooling the first mixed solution to 25-35 ℃ and then mixing the first mixed solution with the second mixed solution; adding 10-15 parts of diatomite and 2-5 parts of bentonite; and ball milling to obtain the finished product of the antibacterial agent.
2. The antibacterial silane polyether gum of claim 1, wherein the reinforcing agent is selected from modified polysiloxane; the modified polysiloxane is prepared from the following raw materials in parts by weight: 70-80 parts of methyl epoxy silane, 5-10 parts of gamma-aminopropyl methyl diethoxy silane, 1-2 parts of potassium hydroxide, 1-2 parts of acetic acid, 5-15 parts of soybean fatty acid and 1-2 parts of toluene;
the preparation method of the modified polysiloxane comprises the following steps:
(1) mixing methyl epoxy silane, gamma-aminopropyl methyl diethoxy silane and potassium hydroxide, heating to 140 ℃ and 150 ℃, reacting for 20-60 minutes, and adding acetic acid for neutralization to obtain an intermediate product;
(2) mixing the intermediate product with soybean fatty acid and toluene, reacting at the temperature of 150-160 ℃ for 0.5-1h, and distilling to obtain the modified polysiloxane.
3. The antibacterial silane polyether gum of claim 2, wherein the coupling agent is a mixture of γ -aminopropyltriethoxysilane, N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane and γ -mercaptopropyltriethoxysilane, and the weight ratio of γ -aminopropyltriethoxysilane to N- (β -aminoethyl) - γ -aminopropyltrimethoxysilane to γ -mercaptopropyltriethoxysilane is (1-2): 0.5-1): 0.8-1.
4. The antibacterial silane polyether adhesive of claim 1, wherein the filler is one or a combination of light calcium carbonate, heavy calcium carbonate, kaolin, talcum powder and wollastonite powder.
5. The antibacterial silane polyether adhesive of claim 4, wherein the filler is a combination of light calcium carbonate, kaolin and talc, and the weight ratio of the light calcium carbonate to the kaolin to the talc is light calcium carbonate: kaolin: talcum powder (2-5): (1-2): (0.1-0.5).
6. The antimicrobial silane polyether gum of claim 1, wherein the silane modified polyether resin is one or a combination of dimethoxysilyl terminated polyether and triethoxysilyl terminated polyether.
7. The antibacterial silane polyether gum of claim 1, wherein the solvent is selected from one or a combination of a polyol acid ester and a polyoxypropylene glycol.
8. The antibacterial silane polyether gum of claim 1, wherein the light stabilizer is at least one of salicylates, benzophenones, benzotriazoles, triazines, substituted acrylonitriles, hindered amine light stabilizers.
9. The antimicrobial silane polyether gum of claim 1, wherein the antioxidant is at least one of a hindered phenol antioxidant, a phosphite antioxidant, a thioester antioxidant, and a complex antioxidant.
10. A method of preparing the antimicrobial silane polyether gum of any one of claims 1-9, comprising:
(1) preparing modified polysiloxane and antibacterial agent;
(2) adding the silane modified polyether resin, the filler, the solvent, the light stabilizer, the antioxidant and the antibacterial agent into a stirring cylinder, and vacuumizing and stirring for 4-6 hours at 80-120 ℃ to obtain a mixture; wherein the vacuum degree is 0.085-0.09 MPa;
(3) cooling the mixture to 20-40 ℃, adding a reinforcing agent, a dehydrating agent and a coupling agent, vacuumizing and stirring for 0.2-2h to obtain a finished product; wherein the vacuum degree is 0.085-0.09 MPa.
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| CN201811352648.XA CN109628047A (en) | 2018-11-14 | 2018-11-14 | A kind of antibacterial silylated polyether glue and preparation method thereof |
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| CN111269691A (en) * | 2020-04-13 | 2020-06-12 | 江西省科学院应用化学研究所 | Single-component composite modified polyether sealant and preparation method thereof |
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