CN113337012A - Composite antibacterial agent, antibacterial master batch containing composite antibacterial agent and preparation method of antibacterial master batch - Google Patents
Composite antibacterial agent, antibacterial master batch containing composite antibacterial agent and preparation method of antibacterial master batch Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C08K3/40—Glass
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2204/00—Glasses, glazes or enamels with special properties
- C03C2204/02—Antibacterial glass, glaze or enamel
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
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- C08K3/20—Oxides; Hydroxides
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
The invention provides a composite antibacterial agent, an antibacterial master batch containing the composite antibacterial agent and a preparation method of the antibacterial master batch, and belongs to the technical field of inorganic antibacterial materials. The composite antibacterial agent comprises, by weight, 54-70 parts of clay, 6-10 parts of rare earth compounds, 10-20 parts of nano zinc oxide and 10-20 parts of shell powder. The composite antibacterial agent is an inorganic zinc oxide antibacterial agent, and has permanent broad-spectrum antibacterial and mildew-proof effects by interfering microbial gene expression with zinc ions, and simultaneously, rare earth compounds are introduced to further enhance the antibacterial property of the nano zinc oxide; the composite antibacterial agent has good antibacterial effect, low dosage, simple operation and low cost. On the basis, an antibacterial master batch is further developed, which comprises 20-35% of a composite antibacterial agent, 60-75% of a matrix resin, 2-4% of a coupling agent, 2-3% of a dispersing agent and 0.5-1% of an antioxidant in percentage by weight. The antibacterial master batch is easy to disperse in a plastic matrix, and is beneficial to the distribution of an antibacterial agent; and the process is simple, the method is suitable for large-scale batch production, and the use cost is reduced.
Description
Technical Field
The invention relates to the technical field of inorganic antibacterial materials, in particular to a composite antibacterial agent, an antibacterial master batch containing the composite antibacterial agent and a preparation method of the antibacterial master batch.
Background
The antibacterial master batch is a concentrated body prepared by uniformly dispersing various antibacterial agents in matrix resin. After a certain amount of antibacterial master batch and corresponding resin particles are mixed, plastic products or antibacterial fibers with antibacterial surfaces can be prepared according to the processing and forming method of plastics and fibers. At present, the mass production of antibacterial plastics and antibacterial fibers adopts the master batch technology.
The antibacterial agent mixed in the antibacterial master batch is the key for determining the antibacterial performance of the antibacterial master batch. The ideal antibacterial agent should have the characteristics of wide antibacterial spectrum, low effective dose, long action time, no influence on the performance of plastics and the like. In the prior art, the antibacterial effect of the conventional antibacterial agent needs to be improved, the effective dose is relatively high, and the defects of complex preparation process, high cost and the like exist. In addition, the conventional antibacterial master batch has the problems of poor dispersibility, complex preparation process and the like.
Disclosure of Invention
The invention aims to provide a composite antibacterial agent, an antibacterial master batch containing the composite antibacterial agent and a preparation method thereof aiming at overcoming the technical problem that the antibacterial performance of the conventional antibacterial agent for the antibacterial master batch is to be improved at present.
The invention also aims to solve the technical problems of higher effective dose, complex preparation process and higher cost of the conventional antibacterial agent.
The invention also aims to solve the technical problems that the conventional antibacterial master batch has poor dispersibility in a plastic matrix and a complex preparation process.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the composite antibacterial agent comprises the following components in parts by weight: 54-70 parts of clay, 6-10 parts of rare earth compound, 10-20 parts of nano zinc oxide and 10-20 parts of shell powder.
Preferably, the clay is selected from one or several of the following components: kaolinite and bentonite.
Preferably, the particle size of the clay powder is 3-5 μm.
Preferably, the particle size of the shell powder is 0.5-1 μm.
Preferably, the rare earth compound is a cerium compound.
Preferably, the rare earth compound is cerium nitrate hexahydrate.
On the basis of the technical scheme, the invention further provides a preparation method of the composite antibacterial agent, which comprises the following steps:
1) taking the clay with the formula amount, mixing the clay with water with the mass of 8-12 times, and stirring for 4-6 min;
2) mixing the rare earth compound and the nano zinc oxide in the formula amount with water in an amount which is 8-12 times the mass of the mixture, stirring for 4-6 min, adding the shell powder in the formula amount, and performing ultrasonic dispersion for 4-6 min;
3) mixing the product obtained in the step 1) with the product obtained in the step 2), and keeping for 25-35 min under the conditions of ultrasonic dispersion and stirring;
4) evaporating the product obtained in the step 3) to dryness;
5) heating the product obtained in the step 4) to 1000-1400 ℃ to form a glass body;
6) taking out the glass body obtained in the step 5), and rapidly cooling with ice water when the temperature is reduced to 80-120 ℃;
7) drying the product quenched in the step 6), and ball-milling the product until the particle size is 0.5-1 mu m to obtain the composite antibacterial agent.
The antibacterial master batch containing the composite antibacterial agent comprises the following components in percentage by weight: 20 to 35 percent of composite antibacterial agent, 60 to 75 percent of matrix resin, 2 to 4 percent of coupling agent, 2 to 3 percent of dispersant and 0.5 to 1 percent of antioxidant.
Preferably, the matrix resin is selected from one or several of the following components: polyethylene, polypropylene, polyvinyl chloride, polystyrene, acrylonitrile-butadiene-styrene copolymer; the coupling agent is selected from one or more of the following components: KH550, KH560, KH 570; the dispersing agent is selected from one or more of the following components: stearic acid, dioctyl phthalate; the antioxidant is selected from one or more of the following components: antioxidant 1010, antioxidant 1076, and antioxidant 164.
On the basis of the technical scheme, the invention further provides a preparation method of the antibacterial master batch, which comprises the following steps: premixing the compound antibacterial agent with the formula amount in a high-speed mixer, adding the coupling agent with the formula amount, uniformly mixing, taking out, drying, grinding, adding the ground product, the dispersing agent, the antioxidant and the matrix resin with the formula amount in the high-speed mixer, uniformly mixing, extruding by using a double-screw extruder, and granulating to obtain the antibacterial master batch.
The invention provides a composite antibacterial agent, an antibacterial master batch containing the composite antibacterial agent and a preparation method thereof. The composite antibacterial agent is an inorganic zinc oxide antibacterial agent, and has permanent broad-spectrum antibacterial and mildew-proof effects by interfering microbial gene expression with zinc ions, and simultaneously, rare earth compounds are introduced to further enhance the antibacterial property of the nano zinc oxide; the composite antibacterial agent has good antibacterial effect, low dosage, simple operation and low cost. On the basis, an antibacterial master batch is further developed, and is easy to disperse in a plastic matrix, so that the distribution of an antibacterial agent is facilitated; and the process is simple, the method is suitable for large-scale batch production, and the use cost is reduced.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A composite antibacterial agent takes clay as an inorganic carrier material, and rare earth doped nano zinc oxide and shell powder as antibacterial components, and comprises the following components in parts by weight: 54-70 parts of clay, 6-10 parts of rare earth compound, 10-20 parts of nano zinc oxide and 10-20 parts of shell powder.
Wherein the clay is one or a mixture of kaolinite and bentonite in any proportion, and the particle size of the powder is 3-5 μm.
The particle size of the shell powder is 0.5-1 mu m.
The rare earth compound is cerium nitrate hexahydrate or other cerium compounds.
The preparation method of the composite antibacterial agent comprises the following steps:
1) adding clay into 10 times of water, and stirring for 5 min;
2) adding a rare earth compound and nano zinc oxide into water with the mass of 10 times, stirring for 5min, adding shell powder, and performing ultrasonic dispersion for 5 min;
3) adding the mixed solution of the rare earth compound, the nano zinc oxide and the shell powder after ultrasonic dispersion into the clay solution, and continuing ultrasonic stirring for 30 min;
4) evaporating the solution to dryness;
5) putting the dried solid into a muffle furnace, and heating to 1000-1400 ℃ to form a glass body;
6) taking out the glass body, and cooling with ice water after the temperature is reduced to 100 ℃;
7) and drying and quenching the product, and ball-milling the product until the particle size is 0.5-1 mu m.
The antibacterial master batch containing the composite antibacterial agent comprises the components of the composite antibacterial agent, matrix resin, a coupling agent, a dispersing agent and an antioxidant in percentage by weight: 20 to 35 percent of composite antibacterial agent, 60 to 75 percent of matrix resin, 2 to 4 percent of coupling agent, 2 to 3 percent of dispersant and 0.5 to 1 percent of antioxidant.
Wherein the matrix resin is one of Polyethylene (PE), polypropylene (PP), polyvinyl chloride (PVC), Polystyrene (PS) or acrylonitrile-butadiene-styrene copolymer (ABS).
The coupling agent is a silane coupling agent; the coupling agent is one of KH550, KH560 or KH 570.
The dispersant is one or two of stearic acid and dioctyl phthalate.
The antioxidant is one or two of antioxidant 1010, antioxidant 1076 and antioxidant 164.
The preparation method of the antibacterial master batch comprises the following steps: preparing antibacterial master batch by adopting a double-screw extrusion method; before extrusion, premixing the antibacterial agent powder in a high-speed mixer for 10min, adding a coupling agent according to a ratio, uniformly mixing, taking out, drying, grinding, adding the powder, a dispersing agent, an antioxidant and matrix resin into the high-speed mixer according to the ratio, uniformly mixing, extruding the uniformly mixed material through a double-screw extruder, and granulating to obtain the antibacterial master batch.
Example 1
An antibacterial master batch comprises the following raw materials: 25% of composite antibacterial agent, 70% of polypropylene matrix resin, 2% of KH550 coupling agent, 2% of dioctyl phthalate dispersing agent and 1% of 1010 antioxidant.
The preparation process of the antibacterial master batch comprises the following steps: weighing the raw materials of the components in percentage, premixing composite antibacterial agent powder in a high-speed mixer for 10min, adding a coupling agent in proportion, uniformly mixing, taking out, drying, grinding, adding the powder, a dispersing agent, an antioxidant and matrix resin in the high-speed mixer, uniformly mixing, extruding the uniformly mixed material by a double-screw extruder, and granulating to obtain the antibacterial master batch. The specific parameters of the twin-screw extruder in this example were set as follows: the temperatures of the zones from the feed port to the head outlet were 172 deg.C, 193 deg.C, 195 deg.C, 186 deg.C, and 202 deg.C, respectively.
The preparation process of the composite antibacterial agent is as follows: the components by weight portion are as follows: 60 parts of kaolin, 8 parts of cerium nitrate hexahydrate, 20 parts of nano zinc oxide and 12 parts of shell powder, and weighing raw materials of the components respectively.
1) Adding kaolin into water with the mass of 10 times, and stirring for 5 min;
2) adding cerium nitrate hexahydrate and nano zinc oxide into water with the mass being 10 times that of the raw materials, stirring for 5min, adding shell powder, and performing ultrasonic dispersion for 5 min;
3) adding the mixed solution of cerium nitrate hexahydrate, nano zinc oxide and shell powder after ultrasonic dispersion into a clay solution, and continuing ultrasonic stirring for 30 min;
4) evaporating the solution to dryness;
5) putting the dried solid into a muffle furnace, and heating to 1000-1400 ℃ to form a glass body;
6) taking out the glass body, and cooling with ice water after the temperature is reduced to 100 ℃;
7) and drying and quenching the product, and ball-milling the product until the particle size is 0.5-1 mu m.
Example 2
An antibacterial master batch comprises the following raw materials: 30% of composite antibacterial agent, 65% of polypropylene matrix resin, 3% of KH560 coupling agent, 1.5% of stearic acid dispersant and 10760.5% of antioxidant.
The preparation process of the antibacterial master batch comprises the following steps: weighing the raw materials of the components in percentage, premixing composite antibacterial agent powder in a high-speed mixer for 10min, adding a coupling agent in proportion, uniformly mixing, taking out, drying, grinding, adding the powder, a dispersing agent, an antioxidant and matrix resin in the high-speed mixer, uniformly mixing, extruding the uniformly mixed material by a double-screw extruder, and granulating to obtain the antibacterial master batch. The specific parameters of the twin-screw extruder in this example were set as follows: the temperature of each region from the feed inlet to the outlet of the machine head is 176 ℃, 190 ℃, 192 ℃, 185 ℃ and 200 ℃.
The preparation process of the composite antibacterial agent is as follows: the components by weight portion are as follows: 55 parts of bentonite, 7 parts of high-cerium sodium sulfate, 18 parts of nano zinc oxide and 20 parts of shell powder. The raw materials of each component are respectively weighed.
1) Adding kaolin into water with the mass of 10 times, and stirring for 5 min;
2) adding cerium nitrate hexahydrate and nano zinc oxide into water with the mass being 10 times that of the raw materials, stirring for 5min, adding shell powder, and performing ultrasonic dispersion for 5 min;
3) adding the mixed solution of cerium nitrate hexahydrate, nano zinc oxide and shell powder after ultrasonic dispersion into a clay solution, and continuing ultrasonic stirring for 30 min;
4) evaporating the solution to dryness;
5) putting the dried solid into a muffle furnace, and heating to 1000-1400 ℃ to form a glass body;
6) taking out the glass body, and cooling with ice water after the temperature is reduced to 100 ℃;
7) and drying and quenching the product, and ball-milling the product until the particle size is 0.5-1 mu m.
Experimental example 1
The antibacterial performance of the plastic surface is tested in examples 1 and 2 by referring to the test method of the antibacterial performance of GB/T31402-2015 plastic surface. The test results are shown in table 1.
TABLE 1 antibacterial Property test results
The experimental results show that the antibacterial master batch prepared by the invention can fully inhibit the growth of staphylococcus aureus and escherichia coli, and shows excellent antibacterial performance.
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the application of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The composite antibacterial agent is characterized by comprising the following components in parts by weight: 54-70 parts of clay, 6-10 parts of rare earth compound, 10-20 parts of nano zinc oxide and 10-20 parts of shell powder.
2. The composite antimicrobial agent of claim 1, wherein the clay is selected from one or more of the following: kaolinite and bentonite.
3. The composite antibacterial agent according to claim 1, wherein the clay has a powder particle size of 3-5 μm.
4. The composite antibacterial agent according to claim 1, wherein the shell powder has a particle size of 0.5-1 μm.
5. The composite antimicrobial agent of claim 1, wherein said rare earth compound is a cerium compound.
6. The composite antimicrobial agent of claim 1, wherein said rare earth compound is cerium nitrate hexahydrate.
7. The method for preparing the composite antibacterial agent of any one of claims 1 to 6, characterized by comprising the following steps:
1) taking the clay with the formula amount, mixing the clay with water with the mass of 8-12 times, and stirring for 4-6 min;
2) mixing the rare earth compound and the nano zinc oxide in the formula amount with water in an amount which is 8-12 times the mass of the mixture, stirring for 4-6 min, adding the shell powder in the formula amount, and performing ultrasonic dispersion for 4-6 min;
3) mixing the product obtained in the step 1) with the product obtained in the step 2), and keeping for 25-35 min under the conditions of ultrasonic dispersion and stirring;
4) evaporating the product obtained in the step 3) to dryness;
5) heating the product obtained in the step 4) to 1000-1400 ℃ to form a glass body;
6) taking out the glass body obtained in the step 5), and rapidly cooling with ice water when the temperature is reduced to 80-120 ℃;
7) drying the product quenched in the step 6), and ball-milling the product until the particle size is 0.5-1 mu m to obtain the composite antibacterial agent.
8. The antibacterial master batch containing the composite antibacterial agent of any one of claims 1 to 6 is characterized by comprising the following components in percentage by weight: 20 to 35 percent of composite antibacterial agent, 60 to 75 percent of matrix resin, 2 to 4 percent of coupling agent, 2 to 3 percent of dispersant and 0.5 to 1 percent of antioxidant.
9. The antimicrobial masterbatch according to claim 8, wherein the matrix resin is selected from one or more of the following components: polyethylene, polypropylene, polyvinyl chloride, polystyrene, acrylonitrile-butadiene-styrene copolymer; the coupling agent is selected from one or more of the following components: KH550, KH560, KH 570; the dispersing agent is selected from one or more of the following components: stearic acid, dioctyl phthalate; the antioxidant is selected from one or more of the following components: antioxidant 1010, antioxidant 1076, and antioxidant 164.
10. The method for preparing the antibacterial masterbatch of claim 8, which is characterized by comprising the following steps: premixing the compound antibacterial agent with the formula amount in a high-speed mixer, adding the coupling agent with the formula amount, uniformly mixing, taking out, drying, grinding, adding the ground product, the dispersing agent, the antioxidant and the matrix resin with the formula amount in the high-speed mixer, uniformly mixing, extruding by using a double-screw extruder, and granulating to obtain the antibacterial master batch.
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| CN115387024A (en) * | 2022-08-29 | 2022-11-25 | 上海水梵科技集团有限公司 | Antibacterial melt-blown fabric |
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