CN114133623B - Plastic antibacterial agent, preparation method and application thereof - Google Patents
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Abstract
The invention relates to the technical field of antibiosis, in particular to a plastic antibiosis agent, a preparation method and application thereof. The nano silver antibacterial agent is prepared by loading silver ions on zirconium phosphate exchange, and is compounded with nano zinc oxide, and has broad-spectrum antibacterial property. The powder is fine powder with uniform granularity, has extremely low hygroscopicity and high heat resistance, and can be easily mixed and processed in fiber, film and plastic resin molded products. The physical and chemical properties are very stable, and the product has excellent dyeing resistance and color change resistance both in the processing process and the using process. The product has high safety and passes a plurality of environmental protection safety tests.
Description
Technical Field
The invention relates to the technical field of antibiosis, in particular to a plastic antibiosis agent, a preparation method and application thereof.
Background
The antibacterial agent is used for preventing and curing plant diseases caused by various pathogenic microorganisms. Agents which kill or inhibit the growth of pathogenic microorganisms but which do not interfere with the normal growth of the plant. The bactericides can be classified according to the mode of action, the source of the raw materials and the chemical composition. Internationally, it is generally known as a drug for controlling various pathogenic microorganisms. With the development of bactericides, subclasses such as bactericides, virucides, algicides and the like are also distinguished.
Antibacterial agents are generally classified into inorganic antibacterial agents, organic antibacterial agents and natural antibacterial agents. The inorganic antibacterial agent is prepared by fixing metals (or ions thereof) such as silver, copper, zinc and the like on the surface of porous materials such as fluorite, silica gel and the like by utilizing the antibacterial capability of the metals such as silver, copper, zinc and the like through physical adsorption ion exchange and other methods, and then adding the antibacterial agent into corresponding products to obtain the material with antibacterial capability. Metals such as mercury, cadmium, lead and the like also have antibacterial capability, but are harmful to human bodies; the color of copper, nickel, lead and other ions will affect the beautiful appearance of the product, and zinc has certain antibacterial property, but the antibacterial strength is only 1/1000 of that of silver ions. Therefore, silver ion antibacterial agents are dominant among inorganic antibacterial agents.
However, the existing nano silver antibacterial agent is too complex to manufacture, is unfavorable for industrial production, and limits the development of the nano silver antibacterial agent.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a plastic antibacterial agent, a preparation method and application thereof.
The aim of the invention is achieved by the following technical scheme:
the plastic antibacterial agent consists of a nano silver antibacterial agent and nano zinc oxide, wherein the nano silver antibacterial agent is prepared by the following steps: adding 20-30 parts by weight of zirconium phosphate and 1-10 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, then adding 0.3-1.3 parts by weight of silver nitrate, stirring for 2-24 hours, and then filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
The nano silver antibacterial agent is prepared by the following steps: adding 25-30 parts by weight of zirconium phosphate and 5-10 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.8-1.3 parts by weight of silver nitrate, stirring for 12-24 hours, and then filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
The nano silver antibacterial agent is prepared by the following steps: adding 20-25 parts by weight of zirconium phosphate and 1-5 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.3-0.8 part by weight of silver nitrate, stirring for 2-12 hours, and then filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
The nano silver antibacterial agent is prepared by the following steps: adding 25 parts by weight of zirconium phosphate and 5 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.8 part by weight of silver nitrate, stirring for 12 hours, and filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
Wherein the calcining temperature is 700-900 ℃ and the calcining time is 2-3h.
Wherein the nano silver antibacterial agent and the nano zinc oxide are mixed according to the weight ratio of 1:1-5.
Wherein the particle size of the nano silver is 10-30nm.
The plastic antibacterial agent is prepared by physically dispersing and mixing the nano silver antibacterial agent and the nano zinc oxide.
The application of the plastic antibacterial agent is used for preparing antibacterial rubber or antibacterial plastic, and particularly can be used for preparing antibacterial degradable plastic resin.
The antibacterial degradable plastic resin is antibacterial degradable polylactic acid resin, and the antibacterial degradable polylactic acid resin is prepared by the following steps:
(1) Adding 12-22 parts by weight of polyvinyl chloride, 6-12 parts by weight of tributyl citrate and 30-50 parts by weight of micron-sized silicon dioxide into 100 parts by weight of organic solvent, heating to 50-60 ℃ and performing ultrasonic oscillation for 10-30min, gradually dropwise adding 60-80 parts by weight of deionized water after ultrasonic oscillation, and filtering, washing and drying after complete precipitation to obtain polyvinyl chloride modified silicon dioxide;
(2) Taking 100 parts by weight of polylactic acid, 50-70 parts by weight of polyvinyl chloride modified silicon dioxide, 8-12 parts by weight of flame retardant, 1-2.5 parts by weight of antioxidant and 0.01-0.5 part by weight of plastic antibacterial agent, putting into a high-speed mixer for mixing, and then putting into a double-screw extruder for melt granulation to obtain the antibacterial degradable polylactic acid resin.
The antibacterial degradable polylactic acid resin disclosed by the invention takes the polylactic acid as a matrix, and a large amount of micron-sized silicon dioxide is added as a filler, so that the antibacterial degradable polylactic acid resin has excellent biodegradability, can also have yellowing resistance and mildew resistance when being matched with the antibacterial agent disclosed by the invention, and has good safety and environmental friendliness when being used as a civil product. However, polylactic acid is brittle, and the brittleness of the polylactic acid is further increased by adding a large amount of inorganic filler, so that the toughness of the polylactic acid is extremely poor. Although the prior art has an example of blending modification by adopting nano-filler, the comprehensive performance of polylactic acid can be obviously improved by utilizing the nano-size effect, the nano-filler has large specific surface area and has practical value only by modifying with a coupling agent, and the cost of the nano-filler is high, so that the nano-filler is not beneficial to industrial application.
In order to reduce the cost of the antibacterial degradable polylactic acid resin, micron-sized silicon dioxide is selected as a filler, and in order to improve the dispersibility of the silicon dioxide and improve the toughness of the resin, a polyvinyl chloride coating modification mode is adopted. Specifically, a polyvinyl chloride coating is formed on the surface of micron-sized silicon dioxide by a precipitation method, tributyl citrate is adopted to plasticize polyvinyl chloride in order to improve the coating rate and the film forming continuity, in addition, an ultrasonic technology is combined in the precipitation method, the suspension property of the micron-sized silicon dioxide is improved by ultrasonic action, and the silicon dioxide and the polyvinyl chloride are activated by the action of high temperature generated by bubble collapse, so that a stable coating structure is formed, and the modification efficiency of the silicon dioxide is improved. The polyvinyl chloride modified silicon dioxide prepared by the method is a core-shell structure modified body, has the dual properties of a rigid body and an elastic body, can obviously improve the mechanical properties of degradable glue, particularly has different elasticity and plasticity, and can cause the phenomenon that stress concentration is easier to occur between phases due to inconsistent deformation degree under the action of external force, thereby causing silver streak phenomenon, absorbing energy and achieving the effect of obviously improving toughness.
The invention has the beneficial effects that: the nano silver antibacterial agent is prepared by loading silver ions on zirconium phosphate exchange, and is compounded with nano zinc oxide, and has broad-spectrum antibacterial property. The powder is fine powder with uniform granularity, has extremely low hygroscopicity and high heat resistance, and can be easily mixed and processed in fiber, film and plastic resin molded products. The physical and chemical properties are very stable, and the product has excellent dyeing resistance and color change resistance both in the processing process and the using process. The product has high safety and passes a plurality of environmental protection safety tests.
Detailed Description
The invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention, in order to facilitate the understanding of those skilled in the art.
Example 1
The plastic antibacterial agent consists of a nano silver antibacterial agent and nano zinc oxide, wherein the nano silver antibacterial agent is prepared by the following steps: adding 25 parts by weight of zirconium phosphate and 5 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.8 part by weight of silver nitrate, stirring for 12 hours, and filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
Wherein the calcination temperature is 800 ℃ and the calcination time is 2.5h.
Wherein the nano silver antibacterial agent and the nano zinc oxide are mixed according to the weight ratio of 1:3.
Wherein the particle size of the nano silver is 20nm.
The plastic antibacterial agent is prepared by physically dispersing and mixing the nano silver antibacterial agent and the nano zinc oxide.
The application of the plastic antibacterial agent is used for preparing antibacterial rubber or antibacterial plastic, and particularly can be used for preparing antibacterial degradable plastic resin.
The antibacterial degradable plastic resin is antibacterial degradable polylactic acid resin, and the antibacterial degradable polylactic acid resin is prepared by the following steps:
(1) Adding 17 parts by weight of polyvinyl chloride, 9 parts by weight of tributyl citrate and 40 parts by weight of micron-sized silicon dioxide into 100 parts by weight of organic solvent, heating to 55 ℃, carrying out ultrasonic oscillation for 20min, gradually dropwise adding 70 parts by weight of deionized water after ultrasonic oscillation, and filtering, washing and drying after complete precipitation to obtain polyvinyl chloride modified silicon dioxide;
(2) And (3) taking 100 parts by weight of polylactic acid, 60 parts by weight of polyvinyl chloride modified silicon dioxide, 10 parts by weight of flame retardant, 1.5 parts by weight of antioxidant and 0.2 part by weight of plastic antibacterial agent, putting into a high-speed mixer for mixing, and then putting into a double-screw extruder for melt granulation to obtain the antibacterial degradable polylactic acid resin.
Example 2
The plastic antibacterial agent consists of a nano silver antibacterial agent and nano zinc oxide, wherein the nano silver antibacterial agent is prepared by the following steps: adding 20 parts by weight of zirconium phosphate and 1 part by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.3 part by weight of silver nitrate, stirring for 2-24 hours, and filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
Wherein the calcination temperature is 700 ℃ and the calcination time is 2h.
Wherein the nano silver antibacterial agent and the nano zinc oxide are mixed according to the weight ratio of 1:1.
Wherein the particle size of the nano silver is 10nm.
The plastic antibacterial agent is prepared by physically dispersing and mixing the nano silver antibacterial agent and the nano zinc oxide.
The application of the plastic antibacterial agent is used for preparing antibacterial rubber or antibacterial plastic, and particularly can be used for preparing antibacterial degradable plastic resin.
The antibacterial degradable plastic resin is antibacterial degradable polylactic acid resin, and the antibacterial degradable polylactic acid resin is prepared by the following steps:
(1) Adding 12 parts by weight of polyvinyl chloride, 6 parts by weight of tributyl citrate and 30 parts by weight of micron-sized silicon dioxide into 100 parts by weight of organic solvent, heating to 50 ℃, carrying out ultrasonic oscillation for 10min, gradually dropwise adding 60 parts by weight of deionized water after ultrasonic oscillation, and filtering, washing and drying after complete precipitation to obtain polyvinyl chloride modified silicon dioxide;
(2) 100 parts by weight of polylactic acid, 50 parts by weight of polyvinyl chloride modified silicon dioxide, 8 parts by weight of flame retardant, 1 part by weight of antioxidant and 0.01 part by weight of plastic antibacterial agent are put into a high-speed mixer to be mixed, and then are put into a double-screw extruder to be melted and granulated, so that the antibacterial degradable polylactic acid resin is obtained.
Example 3
The plastic antibacterial agent consists of a nano silver antibacterial agent and nano zinc oxide, wherein the nano silver antibacterial agent is prepared by the following steps: adding 30 parts by weight of zirconium phosphate and 10 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 1.3 parts by weight of silver nitrate, stirring for 2-24 hours, and filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
Wherein the calcining temperature is 900 ℃ and the calcining time is 2-3h.
Wherein the nano silver antibacterial agent and the nano zinc oxide are mixed according to the weight ratio of 1:5.
Wherein the particle size of the nano silver is 30nm.
The plastic antibacterial agent is prepared by physically dispersing and mixing the nano silver antibacterial agent and the nano zinc oxide.
The application of the plastic antibacterial agent is used for preparing antibacterial rubber or antibacterial plastic, and particularly can be used for preparing antibacterial degradable plastic resin.
The antibacterial degradable plastic resin is antibacterial degradable polylactic acid resin, and the antibacterial degradable polylactic acid resin is prepared by the following steps:
(1) Adding 22 parts by weight of polyvinyl chloride, 12 parts by weight of tributyl citrate and 50 parts by weight of micron-sized silicon dioxide into 100 parts by weight of organic solvent, heating to 60 ℃, carrying out ultrasonic oscillation for 30min, gradually dropwise adding 80 parts by weight of deionized water after ultrasonic oscillation, and filtering, washing and drying after complete precipitation to obtain polyvinyl chloride modified silicon dioxide;
(2) And (3) taking 100 parts by weight of polylactic acid, 70 parts by weight of polyvinyl chloride modified silicon dioxide, 12 parts by weight of flame retardant, 2.5 parts by weight of antioxidant and 0.5 part by weight of plastic antibacterial agent, putting into a high-speed mixer for mixing, and then putting into a double-screw extruder for melt granulation to obtain the antibacterial degradable polylactic acid resin.
Comparative example 1
The antibacterial degradable polylactic acid resin of the comparative example is prepared by the following method:
100 parts by weight of polylactic acid, 42 parts by weight of micron-sized silicon dioxide, 18 parts by weight of polyvinyl chloride, 10 parts by weight of flame retardant, 1.5 parts by weight of antioxidant and 0.2 part by weight of plastic antibacterial agent are taken to be put into a high-speed mixer for mixing, and then are put into a double-screw extruder for melt granulation, so that the antibacterial degradable polylactic acid resin is obtained.
Comparative example 2
The antibacterial degradable polylactic acid resin of the comparative example is prepared by the following method:
(1) Adding 17 parts by weight of polyvinyl chloride, 9 parts by weight of tributyl citrate and 40 parts by weight of micron-sized silicon dioxide into 100 parts by weight of organic solvent, heating to 55 ℃ and stirring, gradually dropwise adding 70 parts by weight of deionized water in the stirring process, and filtering, washing and drying after complete precipitation to obtain polyvinyl chloride modified silicon dioxide;
(2) And (3) taking 100 parts by weight of polylactic acid, 60 parts by weight of polyvinyl chloride modified silicon dioxide, 10 parts by weight of flame retardant, 1.5 parts by weight of antioxidant and 0.2 part by weight of plastic antibacterial agent, putting into a high-speed mixer for mixing, and then putting into a double-screw extruder for melt granulation to obtain the antibacterial degradable polylactic acid resin.
The antibacterial degradable polylactic acid resins of example 1 and comparative examples 1 to 2 were subjected to performance tests of tensile strength, flexural strength and impact strength according to the test standards of GB/T1040, GB/T9341 and GB/T1043, and the test results are as follows:
from the above test, it is difficult to ensure the dispersibility of the micron-sized silica by directly adopting a physical blending mode in comparative example 1, the reinforcing effect of the silica is greatly reduced, and the toughness of the material is obviously reduced; although the precipitation method is also used for modifying the silica in comparative example 2, the lack of the ultrasonic action leads to a low modification degree, and thus the mechanical properties are also lowered to some extent.
The above embodiments are preferred embodiments of the present invention, and besides, the present invention may be implemented in other ways, and any obvious substitution is within the scope of the present invention without departing from the concept of the present invention.
Claims (8)
1. A plastic antibacterial agent, which is characterized in that: the nano silver antibacterial agent consists of a nano silver antibacterial agent and nano zinc oxide, and is prepared by the following method: adding 20-30 parts by weight of zirconium phosphate and 1-10 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, then adding 0.3-1.3 parts by weight of silver nitrate, stirring for 2-24 hours, and then filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent; the application of the plastic antibacterial agent comprises the following steps: the preparation method is used for preparing the antibacterial degradable plastic resin, wherein the antibacterial degradable plastic resin is antibacterial degradable polylactic acid resin, and the antibacterial degradable polylactic acid resin is prepared by the following steps: (1) Adding 12-22 parts by weight of polyvinyl chloride, 6-12 parts by weight of tributyl citrate and 30-50 parts by weight of micron-sized silicon dioxide into 100 parts by weight of organic solvent, heating to 50-60 ℃ and performing ultrasonic oscillation for 10-30min, gradually dropwise adding 60-80 parts by weight of deionized water after ultrasonic oscillation, and filtering, washing and drying after complete precipitation to obtain polyvinyl chloride modified silicon dioxide; (2) Taking 100 parts by weight of polylactic acid, 50-70 parts by weight of polyvinyl chloride modified silicon dioxide, 8-12 parts by weight of flame retardant, 1-2.5 parts by weight of antioxidant and 0.01-0.5 part by weight of plastic antibacterial agent, putting into a high-speed mixer for mixing, and then putting into a double-screw extruder for melt granulation to obtain the antibacterial degradable polylactic acid resin.
2. A plastic antibacterial agent according to claim 1, wherein: the nano silver antibacterial agent is prepared by the following steps: adding 25-30 parts by weight of zirconium phosphate and 5-10 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.8-1.3 parts by weight of silver nitrate, stirring for 12-24 hours, and then filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
3. A plastic antibacterial agent according to claim 1, wherein: the nano silver antibacterial agent is prepared by the following steps: adding 20-25 parts by weight of zirconium phosphate and 1-5 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.3-0.8 part by weight of silver nitrate, stirring for 2-12 hours, and then filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
4. A plastic antibacterial agent according to claim 1, wherein: the nano silver antibacterial agent is prepared by the following steps: adding 25 parts by weight of zirconium phosphate and 5 parts by weight of citric acid into 100 parts by weight of deionized water to prepare suspension, adding 0.8 part by weight of silver nitrate, stirring for 12 hours, and filtering, drying, calcining and crushing to obtain the nano silver antibacterial agent.
5. A plastic antibacterial agent according to claim 1, wherein: the calcining temperature is 700-900 ℃ and the calcining time is 2-3h.
6. A plastic antibacterial agent according to claim 1, wherein: consists of nano silver antibacterial agent and nano zinc oxide in the weight ratio of 1:1-5.
7. A plastic antibacterial agent according to claim 1, wherein: the grain diameter of the nano silver is 10-30nm.
8. A method for preparing a plastic antibacterial agent according to any one of claims 1 to 7, characterized in that: is prepared from nano silver antibacterial agent and nano zinc oxide through physical dispersing and mixing.
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|---|---|---|---|---|
| CN101744002A (en) * | 2009-12-29 | 2010-06-23 | 浙江理工大学 | Silicon-zinc mesoporous material silver-carrying antibacterial agent and preparation method thereof |
| CN103011276A (en) * | 2012-12-13 | 2013-04-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing silver-loaded titanium oxide-zirconium phosphate composite nanometer material |
| CN112142027A (en) * | 2020-09-17 | 2020-12-29 | 赣州瑞德化工有限公司 | Preparation method of nano layered zirconium phosphate and silver-loaded zirconium phosphate thereof |
| CN112574510A (en) * | 2020-12-14 | 2021-03-30 | 东莞市三至新材料技术有限公司 | Antibacterial ultraviolet aging resistant modified PP composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101744002A (en) * | 2009-12-29 | 2010-06-23 | 浙江理工大学 | Silicon-zinc mesoporous material silver-carrying antibacterial agent and preparation method thereof |
| CN103011276A (en) * | 2012-12-13 | 2013-04-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing silver-loaded titanium oxide-zirconium phosphate composite nanometer material |
| CN112142027A (en) * | 2020-09-17 | 2020-12-29 | 赣州瑞德化工有限公司 | Preparation method of nano layered zirconium phosphate and silver-loaded zirconium phosphate thereof |
| CN112574510A (en) * | 2020-12-14 | 2021-03-30 | 东莞市三至新材料技术有限公司 | Antibacterial ultraviolet aging resistant modified PP composite material and preparation method thereof |
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