阅读说明：本技术 一种抗菌母料的制备方法 (Preparation method of antibacterial master batch ) 是由 许亮 洪江 陶慷 李瑞龙 焦旗 于 2020-12-16 设计创作，主要内容包括：本发明公开了一种抗菌母料的制备方法,包括：S1：将无机抗菌剂按照1：3的比例溶于水中,并加入重量份为0.01份的乳化剂,通过超声进行分散0.5-3h,将其分散成稳定的乳化溶液,得到无机抗菌剂溶液；S2：将重量份为30-90份多孔聚合物载体置于混合机中,开动混合机,在20-300rpm的搅拌速度下,边搅拌边将重量份为10-70份上述步骤中得到的分散好的无机抗菌剂溶液通过喷头加入到混合机中,抗菌溶液的喷洒时间不少于10min,加入完成后,静置至多孔聚合物表面干爽；S3：将吸附抗菌剂溶液的多孔聚合物置于鼓风干燥箱中,80-90℃温度下,干燥2-10h,即得抗菌母粒。本发明制得的母粒母料易于分散于塑料基体中,有利于抗菌剂分布；工艺简单,适合大规模批量生产,且降低使用成本。(The invention discloses a preparation method of an antibacterial master batch, which comprises the following steps: s1: mixing inorganic antibacterial agent according to the ratio of 1: 3, dissolving in water, adding 0.01 part by weight of emulsifier, dispersing for 0.5-3h by ultrasonic to obtain stable emulsified solution, and obtaining inorganic antibacterial agent solution; s2: placing 30-90 parts by weight of porous polymer carrier into a mixer, starting the mixer, adding 10-70 parts by weight of the dispersed inorganic antibacterial agent solution obtained in the step into the mixer through a spray head while stirring at a stirring speed of 20-300rpm, wherein the spraying time of the antibacterial solution is not less than 10min, and standing the mixture until the surface of the porous polymer is dry and comfortable after the addition is finished; s3: and (3) placing the porous polymer adsorbing the antibacterial agent solution in a forced air drying oven, and drying at the temperature of 80-90 ℃ for 2-10h to obtain the antibacterial master batch. The master batch prepared by the invention is easy to disperse in a plastic matrix, and is beneficial to the distribution of the antibacterial agent; the process is simple, is suitable for large-scale batch production, and reduces the use cost.)

1. A preparation method of an antibacterial master batch is characterized by comprising the following steps: the method comprises the following steps in sequence:

s1: mixing inorganic antibacterial agent according to the ratio of 1: 3, dissolving in water, adding 0.01 part by weight of emulsifier, dispersing for 0.5-3h by ultrasonic to obtain stable emulsified solution, and obtaining inorganic antibacterial agent solution;

s2: placing 30-90 parts by weight of porous polymer carrier into a mixer, starting the mixer, adding 10-70 parts by weight of the dispersed inorganic antibacterial agent solution obtained in the step into the mixer through a spray head while stirring at a stirring speed of 20-300rpm, wherein the spraying time of the antibacterial solution is not less than 10min, and standing the mixture until the surface of the porous polymer is dry and comfortable after the addition is finished;

s3: and (3) placing the porous polymer adsorbing the antibacterial agent solution in a forced air drying oven, and drying at the temperature of 80-90 ℃ for 2-10h to obtain the antibacterial master batch.

2. The method for preparing the antibacterial master batch according to claim 1, characterized by comprising the following steps: the inorganic antibacterial agent is one or the combination of a plurality of metal ion type antibacterial agents and oxide photocatalytic type antibacterial agents.

3. The method for preparing the antibacterial master batch according to claim 1, characterized by comprising the following steps: the emulsifier is one or more of polyoxyethylene ether emulsifier, organosilicon emulsifier and organic quaternary ammonium salt emulsifier.

4. The method for preparing the antibacterial master batch according to claim 1, characterized by comprising the following steps: the porous polymer carrier is one or the combination of a plurality of porous polypropylene, porous polyethylene, porous polystyrene, porous acrylonitrile-butadiene-styrene copolymer, porous polycarbonate, porous nylon and porous polylactic acid.

5. The method for preparing the antibacterial master batch according to claim 1, characterized by comprising the following steps: the particle size of the porous polymer is 0.5-10mm, the porosity is more than or equal to 50 percent, and the bulk density is 30-350kg/m³。

6. The method for preparing the antibacterial master batch according to claim 1, characterized by comprising the following steps: the ultrasonic power is 70-120W.

Technical Field

The invention belongs to the technical field of high-molecular functional additives, and particularly relates to a preparation method of an antibacterial master batch.

Background

In recent years, with the improvement of living standard and the enhancement of health consciousness of people, people have more and more demands on antibacterial materials and antibacterial products, wherein, antibacterial plastics are the antibacterial materials which are most rapidly developed and widely applied, and are applied to a plurality of fields such as household appliances, food packages, cultural goods, kitchen and toilet goods, automobile accessories and the like.

The antibacterial property of the antibacterial plastic is realized by adding a plastic antibacterial auxiliary agent. The antibacterial agent includes four major classes of inorganic antibacterial agents, organic antibacterial agents, natural antibacterial agents and polymeric antibacterial agents. High thermal stability of the antimicrobial agent is required under severe conditions of high temperature, high heat, strong shear, etc. during plastic processing. The inorganic antibacterial agent is an important choice for plastic antibacterial modification due to high thermal stability, but the inorganic antibacterial agent has poor dispersibility in a plastic matrix, so that the inorganic antibacterial agent is unevenly dispersed in a plastic system, and the physical properties and the antibacterial efficiency of the material are greatly influenced. Patents CN107793581A, CN108395679A and CN109627553A all report that the inorganic antibacterial agent is subjected to a surface modification treatment in the early stage, and then is subjected to blending granulation with a polymer matrix to form a master batch to solve the problem of dispersion of the inorganic antibacterial agent in plastics. However, the method adopts a path of preparing the powder master batch by using double screws, and the antibacterial master batch with high effective content cannot be prepared; and the pretreatment process of the antibacterial agent is relatively complex, which is not beneficial to industrial production.

Therefore, it is necessary to develop a method for producing a master batch which can effectively disperse an antibacterial agent in a matrix to effectively exert antibacterial activity, and which has a high effective content and is easy for industrial production.

Disclosure of Invention

The invention aims to provide a preparation method of an antibacterial master batch, which aims to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the antibacterial master batch comprises the following steps in sequence:

s1: mixing inorganic antibacterial agent according to the ratio of 1: 3, dissolving in water, adding 0.01 part by weight of emulsifier, dispersing for 0.5-3h by ultrasonic to obtain stable emulsified solution, and obtaining inorganic antibacterial agent solution;

s2: placing 30-90 parts by weight of porous polymer carrier into a mixer, starting the mixer, adding 10-70 parts by weight of the dispersed inorganic antibacterial agent solution obtained in the step into the mixer through a spray head while stirring at a stirring speed of 20-300rpm, wherein the spraying time of the antibacterial solution is not less than 10min, and standing the mixture until the surface of the porous polymer is dry and comfortable after the addition is finished;

s3: and (3) placing the porous polymer adsorbing the antibacterial agent solution in a forced air drying oven, and drying at the temperature of 80-90 ℃ for 2-10h to obtain the antibacterial master batch.

Preferably, the inorganic antibacterial agent is one or more of a metal ion type antibacterial agent and an oxide photocatalytic type antibacterial agent.

In any of the above embodiments, preferably, the emulsifier is one or a combination of more of polyoxyethylene ether type emulsifiers, silicone type emulsifiers, and organic quaternary ammonium salt type emulsifiers.

In any of the above embodiments, preferably, the porous polymer support is one or a combination of porous polypropylene, porous polyethylene, porous polystyrene, porous acrylonitrile-butadiene-styrene copolymer, porous polycarbonate, porous nylon, and porous polylactic acid.

In any of the above schemes, the particle size of the porous polymer is preferably 0.5-10mm, the porosity is more than or equal to 50%, and the bulk density is preferably 30-350kg/m³。

In any of the above schemes, preferably, the ultrasonic power is 70-120W.

The invention has the technical effects and advantages that:

1. the antibacterial master batch prepared by the preparation method of the antibacterial master batch is loaded with the antibacterial agent through the porous polymer, and the master batch is easy to disperse in a plastic matrix, so that the distribution of the antibacterial agent is facilitated, and no negative influence is generated on a plastic product;

2. the antibacterial master batch prepared by the preparation method of the antibacterial master batch is different from a double-screw blending master batch, the effective content of the antibacterial agent is high, and the use cost is reduced;

3. the preparation method of the antibacterial master batch is simple in process and suitable for large-scale batch production, and the product can be widely applied to the fields of public health, food packaging, biomedical treatment and the like.

Detailed Description

The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1:

the preparation method of the antibacterial master batch comprises the following steps in sequence:

s1: mixing nanometer TiO₂The antibacterial agent is prepared according to the following steps of 1: 3, dissolving in water, adding 0.01 part by weight of emulsifier, dispersing for 0.5-3h by ultrasonic to obtain stable emulsified solution, and obtaining inorganic antibacterial agent solution;

s2: placing 30-90 parts by weight of porous polymer carrier into a mixer, starting the mixer, adding 10-70 parts by weight of the dispersed inorganic antibacterial agent solution obtained in the step into the mixer through a spray head while stirring at a stirring speed of 20-300rpm, wherein the spraying time of the antibacterial solution is not less than 10min, and standing the mixture until the surface of the porous polymer is dry and comfortable after the addition is finished;

s3: and (3) placing the porous polymer adsorbing the antibacterial agent solution in a forced air drying oven, and drying at the temperature of 80-90 ℃ for 2-10h to obtain the antibacterial master batch.

Specifically, the emulsifier is one or more of polyoxyethylene ether emulsifier, organosilicon emulsifier, and organic quaternary ammonium salt emulsifier.

Specifically, the porous polymer carrier is one or more of porous polypropylene, porous polyethylene, porous polystyrene, porous acrylonitrile-butadiene-styrene copolymer, porous polycarbonate, porous nylon and porous polylactic acid.

Specifically, the particle size of the porous polymer is 0.5-10mm, the porosity is more than or equal to 50%, and the bulk density is 30-350kg/m³。

Specifically, the ultrasonic power is 70-120W.

Example 2:

the preparation method of the antibacterial master batch comprises the following steps in sequence:

s1: mixing AgNO₃The antibacterial agent is prepared according to the following steps of 1: 3 in proportion in water, adding 0.01 part by weight of emulsifier, dispersing for 0.5-3h by ultrasonic to obtain stable emulsified solutionAn antimicrobial solution;

s2: placing 30-90 parts by weight of porous polymer carrier into a mixer, starting the mixer, adding 10-70 parts by weight of the dispersed inorganic antibacterial agent solution obtained in the step into the mixer through a spray head while stirring at a stirring speed of 20-300rpm, wherein the spraying time of the antibacterial solution is not less than 10min, and standing the mixture until the surface of the porous polymer is dry and comfortable after the addition is finished;

s3: and (3) placing the porous polymer adsorbing the antibacterial agent solution in a forced air drying oven, and drying at the temperature of 80-90 ℃ for 2-10h to obtain the antibacterial master batch.

Specifically, the emulsifier is one or more of polyoxyethylene ether emulsifier, organosilicon emulsifier, and organic quaternary ammonium salt emulsifier.

Specifically, the porous polymer carrier is one or more of porous polypropylene, porous polyethylene, porous polystyrene, porous acrylonitrile-butadiene-styrene copolymer, porous polycarbonate, porous nylon and porous polylactic acid.

Specifically, the particle size of the porous polymer is 0.5-10mm, the porosity is more than or equal to 50%, and the bulk density is 30-350kg/m³。

Specifically, the ultrasonic power is 70-120W.

Example 3:

the preparation method of the antibacterial master batch comprises the following steps in sequence:

s1: the phosphate type antibacterial agent was prepared according to the following ratio of 1: 3, dissolving in water, adding 0.01 part by weight of emulsifier, dispersing for 0.5-3h by ultrasonic to obtain stable emulsified solution, and obtaining inorganic antibacterial agent solution;

s2: placing 30-90 parts by weight of porous polymer carrier into a mixer, starting the mixer, adding 10-70 parts by weight of the dispersed inorganic antibacterial agent solution obtained in the step into the mixer through a spray head while stirring at a stirring speed of 20-300rpm, wherein the spraying time of the antibacterial solution is not less than 10min, and standing the mixture until the surface of the porous polymer is dry and comfortable after the addition is finished;

s3: and (3) placing the porous polymer adsorbing the antibacterial agent solution in a forced air drying oven, and drying at the temperature of 80-90 ℃ for 2-10h to obtain the antibacterial master batch.

Specifically, the emulsifier is one or more of polyoxyethylene ether emulsifier, organosilicon emulsifier, and organic quaternary ammonium salt emulsifier.

Specifically, the porous polymer carrier is one or more of porous polypropylene, porous polyethylene, porous polystyrene, porous acrylonitrile-butadiene-styrene copolymer, porous polycarbonate, porous nylon and porous polylactic acid.

Specifically, the particle size of the porous polymer is 0.5-10mm, the porosity is more than or equal to 50%, and the bulk density is 30-350kg/m³。

Specifically, the ultrasonic power is 70-120W.

The antibacterial resin obtained by blending, extruding and granulating the antibacterial master batch prepared in the embodiments 1-3 of the invention and the matrix resin thereof is tested according to the QB/T2591-. The bacteriostasis rate of the sample for 24h was examined, as shown in table 1:

TABLE 1

From the above table 1, it can be seen that the antibacterial master batch prepared by the invention has very high escherichia coli sterilization rate and staphylococcus aureus sterilization rate% after being mixed with the matrix resin, which indicates that the antibacterial master batch has very high bacteriostasis rate.

Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.