阅读说明：本技术 纳米抗菌型毛刷材料及其制备方法 (Nano antibacterial hairbrush material and preparation method thereof ) 是由 熊静静 于 2020-12-07 设计创作，主要内容包括：本发明提供了纳米抗菌型毛刷材料及其制备方法。制备步骤如下：制备蚕砂生物炭；纳米抗菌剂接枝蚕砂生物炭：1)将十六烷基三甲基氯化胺和去离子水混合超声,加热搅拌；2)加入NaCl溶液高速搅拌,逐滴加入AgNO-3溶液反应；3)加入HCl溶液调pH；4)再缓慢加入蚕砂生物炭反应；5)离心洗涤,真空干燥；6)加入到戊二醛溶液中,磁力搅拌,离心洗涤,干燥过夜；将纳米抗菌剂接枝蚕砂生物炭、尼龙66切片和辅助助剂在捏合机中搅匀,经双螺杆挤出机挤出造粒；真空干燥后,采用喷丝板进行喷丝即得。本发明所制备的纳米抗菌型毛刷材料具有很好的抗菌性能,对大肠杆菌的抑制率、金黄色葡萄球菌和枯草杆菌都具有很好的抑制效果。(The invention provides a nano antibacterial hairbrush material and a preparation method thereof. The preparation steps are as follows: preparing silkworm excrement biochar; grafting silkworm excrement biochar by using a nano antibacterial agent: 1) mixing hexadecyl trimethyl ammonium chloride and deionized water, and carrying out ultrasonic treatment, heating and stirring; 2) adding NaCl solution, stirring at high speed, and adding AgNO dropwise 3 Carrying out solution reaction; 3) adding HCl solution to adjust the pH value; 4) slowly adding silkworm excrement biochar for reaction; 5) centrifugally washing and vacuum drying; 6) adding into glutaraldehyde solution, magnetically stirring, centrifuging, washing, and drying overnight; uniformly stirring the nano antibacterial agent grafted silkworm excrement biochar, the nylon 66 slices and the auxiliary agent in a kneading machine, and extruding and granulating by a double-screw extruder; and (4) after vacuum drying, spinning by using a spinneret plate to obtain the yarn. The nano antibacterial hairbrush material prepared by the invention has good antibacterial performance and is suitable for escherichia coliThe inhibition rate, staphylococcus aureus and bacillus subtilis all have good inhibition effect.)

1. the nanometer antibacterial hairbrush material and the preparation method thereof are characterized by comprising the following steps:

(1) preparing silkworm excrement biochar: washing faeces Bombycis with distilled water, drying at 105 deg.C for 2 hr; putting the mixture into a heating zone of a tube furnace, and introducing N₂Charring for 2h at the temperature of 700 ℃ in 5 ℃/min; mixing KOH powder and carbonized silkworm excrement at a mass ratio of 4:1, placing the mixture into a porcelain ark, and introducing N₂Carrying out secondary activation; reacting the activated sample with 1mol/L hydrochloric acid, and then cleaning with distilled water until the pH value is neutral to obtain silkworm excrement biochar;

(2) grafting silkworm excrement biochar by using a nano antibacterial agent: 1) mixing 0.18mmol of hexadecyl trimethyl ammonium chloride and 100mL of deionized water, performing ultrasonic treatment for 10min, and heating and stirring for 30 min; 2) adding 1mL of 0.5mol/L NaCl solution, stirring at high speed for 30min, and dropwise adding 1mL of 0.5mol/L AgNO₃Reacting the solution at 40 ℃ for 1 h; 3) adding 1mL of 0.1mol/L HCl solution, and adjusting the pH value of the solution to 5; 4) slowly adding 3-5g of silkworm excrement biochar for reaction for 2-3 h; 5) centrifuging, washing, and vacuum drying at 30 deg.C for 24 hr; 6) adding into 25% glutaraldehyde solution, magnetically stirring for 3 hr, centrifuging, washing, and drying in a vacuum drying oven at 40 deg.C overnight to obtain nanometer antibacterial agent grafted faeces Bombycis biochar;

(3) uniformly stirring the nano antibacterial agent grafted silkworm excrement biochar, the nylon 66 slices and the auxiliary agent in a kneading machine, and extruding and granulating by a double-screw extruder;

(4) and after vacuum drying, spinning by using a spinneret plate to obtain the nano antibacterial hairbrush material.

2. The nano antibacterial hairbrush material and the preparation method thereof according to claim 1, wherein the auxiliary agent in the step (3) comprises epoxidized soybean oil, polytetrafluoroethylene and montmorillonite.

3. The nano antibacterial hairbrush material and the preparation method thereof according to claim 1, wherein the extrusion temperature of the twin-screw extruder in the step (3) is 240 ℃ to 270 ℃, and the screw rotation speed is 150 r/min.

4. The nano antibacterial brush material and the preparation method thereof according to claim 1, wherein the diameter of the spinneret in the step (4) is 160mm, the diameter of the spinneret is 90 holes, and the diameter of the spinneret is 0.8 mm.

5. The nano antibacterial brush material and the preparation method thereof according to claim 2, wherein the montmorillonite is sodium-based or calcium-based montmorillonite, and C is used before use₁₆-C₁₈The quaternary ammonium salt is treated, and the interlayer distance after treatment is between 2nm and 3.5 nm.

Technical Field

The invention relates to the field of new materials, in particular to a nano antibacterial hairbrush material and a preparation method thereof.

Background

Since the new century, the market potential of antibacterial brush materials draws wide attention of the brush industry, and particularly, the diversity of performances and the processability of synthetic fibers enable the synthetic fibers to start to comprehensively replace animal hair in the aspect of application of the brush industry, so that the rapid development of brush production is greatly promoted. Meanwhile, because the synthetic fiber has strong processability, the performance requirement on the brush wire is higher and higher, and the antibacterial property is one of the requirements, and as a material used for a long time, how to achieve effective and long-acting antibacterial effect has important significance in the aspects of widening the field, reducing the cost and the like.

Disclosure of Invention

The technical problem to be solved is as follows: the invention aims to provide a nano antibacterial hairbrush material and a preparation method thereof, wherein the nano antibacterial hairbrush material has good antibacterial performance and good inhibition effect on the inhibition rate of escherichia coli, staphylococcus aureus and bacillus subtilis.

The technical scheme is as follows: the nanometer antibacterial hairbrush material and the preparation method thereof comprise the following steps:

(1) preparing silkworm excrement biochar: washing faeces Bombycis with distilled water, drying at 105 deg.C for 2 hr; putting the mixture into a heating zone of a tube furnace, and introducing N₂Charring for 2h at the temperature of 700 ℃ in 5 ℃/min; mixing KOH powder and carbonized silkworm excrement at a mass ratio of 4:1, placing the mixture into a porcelain ark, and introducing N₂Carrying out secondary activation; reacting the activated sample with 1mol/L hydrochloric acid, and then cleaning with distilled water until the pH value is neutral to obtain silkworm excrement biochar;

(2) grafting silkworm excrement biochar by using a nano antibacterial agent: 1) mixing 0.18mmol of hexadecyl trimethyl ammonium chloride and 100mL of deionized water, performing ultrasonic treatment for 10min, and heating and stirring for 30 min; 2) adding 1mL of 0.5mol/L NaCl solution, stirring at high speed for 30min, and dropwise adding 1mL of 0.5mol/L AgNO₃Reacting the solution at 40 ℃ for 1 h; 3) adding 1mL of 0.1mol/L HCl solution, and adjusting the pH value of the solution to 5; 4) slowly adding 3-5g of silkworm excrement biochar for reaction for 2-3 h; 5) centrifuging, washing, and vacuum drying at 30 deg.C for 24 hr; 6) adding into 25% glutaraldehyde solution, magnetically stirring for 3 hr, centrifuging, washing, and drying in a vacuum drying oven at 40 deg.C overnight to obtain nanometer antibacterial agent grafted faeces Bombycis biochar;

(3) uniformly stirring the nano antibacterial agent grafted silkworm excrement biochar, the nylon 66 slices and the auxiliary agent in a kneading machine, and extruding and granulating by a double-screw extruder;

(4) and after vacuum drying, spinning by using a spinneret plate to obtain the nano antibacterial hairbrush material.

Further, the auxiliary agent in the step (3) comprises epoxidized soybean oil, polytetrafluoroethylene and montmorillonite.

Further, the extrusion temperature of the double-screw extruder in the step (3) is 240-270 ℃, and the screw rotating speed is 150 r/min. Further, the diameter of the spinneret plate in the step (4) is 160mm, the diameter of the spinneret plate is 90 holes, and the diameter of the holes is 0.8 mm.

Further, the montmorillonite is sodium-based or calcium-based montmorillonite, and is treated with C before use₁₆-C₁₈The quaternary ammonium salt is treated, and the interlayer distance after treatment is between 2nm and 3.5 nm.

Has the advantages that:

1. according to the invention, the silkworm excrement is carbonized and activated to obtain the medium-micro double-channel biochar material with a high specific surface, and the antibacterial agent has a good adsorption effect and can be firmly fixed in the medium-micro double-channel biochar material.

2. The invention adopts the matching of inorganic/organic antibacterial agents, so that the antibacterial agent has the synergistic effect of quick sterilization and long-term antibiosis.

3. The nano antibacterial hairbrush material prepared by the invention has good antibacterial performance, and the inhibition rate of the nano antibacterial hairbrush material on escherichia coli can reach 100% and the inhibition rates on staphylococcus aureus and bacillus subtilis can respectively reach 99.6% and 99.7% at most.

Detailed Description

Example 1

The nanometer antibacterial hairbrush material and the preparation method thereof comprise the following steps:

(1) preparing silkworm excrement biochar: washing faeces Bombycis with distilled water, drying at 105 deg.C for 2 hr; putting the mixture into a heating zone of a tube furnace, and introducing N₂Charring for 2h at the temperature of 700 ℃ in 5 ℃/min; mixing KOH powder and carbonized silkworm excrement at a mass ratio of 4:1, placing the mixture into a porcelain ark, and introducing N₂Carrying out secondary activation; reacting the activated sample with 1mol/L hydrochloric acid, and then cleaning with distilled water until the pH value is neutral to obtain silkworm excrement biochar;

(2) grafting silkworm excrement biochar by using a nano antibacterial agent: 1) mixing 0.18mmol of hexadecyl trimethyl ammonium chloride and 100mL of deionized water, performing ultrasonic treatment for 10min, and heating and stirring for 30 min; 2) adding 1mL of 0.5mol/L NaCl solution, stirring at high speed for 30min, and dropwise adding 1mL of 0.5mol/L AgNO₃Reacting the solution at 40 ℃ for 1 h; 3) adding 1mL of 0.1mol/L HCl solution, and adjusting the pH value of the solution to 5; 4) slowly adding 3g of silkworm excrement biochar for reaction for 2 hours; 5) centrifuging, washing, and vacuum drying at 30 deg.C for 24 hr; 6) adding to 25 percentMagnetically stirring the solution in glutaraldehyde solution for 3h, centrifuging, washing, and drying in a vacuum drying oven at 40 ℃ overnight to obtain nano antibacterial agent grafted silkworm excrement biochar;

(3) uniformly stirring nano antibacterial agent grafted silkworm excrement biochar, nylon 66 slices, epoxidized soybean oil, polytetrafluoroethylene and sodium montmorillonite in a kneading machine, and extruding and granulating by using a double-screw extruder, wherein the extrusion temperature is 240 ℃, and the screw rotating speed is 150 r/min; (4) and (3) after vacuum drying, spinning by using a spinneret plate to obtain the nano antibacterial hairbrush material, wherein the diameter of the spinneret plate is 160mm, the number of the holes is 90, and the aperture is 0.8 mm.

Example 2

The nanometer antibacterial hairbrush material and the preparation method thereof comprise the following steps:

(1) preparing silkworm excrement biochar: washing faeces Bombycis with distilled water, drying at 105 deg.C for 2 hr; putting the mixture into a heating zone of a tube furnace, and introducing N₂Charring for 2h at the temperature of 700 ℃ in 5 ℃/min; mixing KOH powder and carbonized silkworm excrement at a mass ratio of 4:1, placing the mixture into a porcelain ark, and introducing N₂Carrying out secondary activation; reacting the activated sample with 1mol/L hydrochloric acid, and then cleaning with distilled water until the pH value is neutral to obtain silkworm excrement biochar;

(2) grafting silkworm excrement biochar by using a nano antibacterial agent: 1) mixing 0.18mmol of hexadecyl trimethyl ammonium chloride and 100mL of deionized water, performing ultrasonic treatment for 10min, and heating and stirring for 30 min; 2) adding 1mL of 0.5mol/L NaCl solution, stirring at high speed for 30min, and dropwise adding 1mL of 0.5mol/L AgNO₃Reacting the solution at 40 ℃ for 1 h; 3) adding 1mL of 0.1mol/L HCl solution, and adjusting the pH value of the solution to 5; 4) slowly adding 4g of silkworm excrement biochar for reaction for 2.5 hours; 5) centrifuging, washing, and vacuum drying at 30 deg.C for 24 hr; 6) adding into 25% glutaraldehyde solution, magnetically stirring for 3 hr, centrifuging, washing, and drying in a vacuum drying oven at 40 deg.C overnight to obtain nanometer antibacterial agent grafted faeces Bombycis biochar;

(3) uniformly stirring nano antibacterial agent grafted silkworm excrement biochar, nylon 66 slices, epoxidized soybean oil, polytetrafluoroethylene and sodium-based or calcium-based montmorillonite in a kneading machine, and extruding and granulating by using a double-screw extruder, wherein the extrusion temperature is 265 ℃, and the screw rotating speed is 150 r/min;

(4) and (3) after vacuum drying, spinning by using a spinneret plate to obtain the nano antibacterial hairbrush material, wherein the diameter of the spinneret plate is 160mm, the number of the holes is 90, and the aperture is 0.8 mm.

Example 3

The nanometer antibacterial hairbrush material and the preparation method thereof comprise the following steps:

(1) preparing silkworm excrement biochar: washing faeces Bombycis with distilled water, drying at 105 deg.C for 2 hr; putting the mixture into a heating zone of a tube furnace, and introducing N₂Charring for 2h at the temperature of 700 ℃ in 5 ℃/min; mixing KOH powder and carbonized silkworm excrement at a mass ratio of 4:1, placing the mixture into a porcelain ark, and introducing N₂Carrying out secondary activation; reacting the activated sample with 1mol/L hydrochloric acid, and then cleaning with distilled water until the pH value is neutral to obtain silkworm excrement biochar;

(2) grafting silkworm excrement biochar by using a nano antibacterial agent: 1) mixing 0.18mmol of hexadecyl trimethyl ammonium chloride and 100mL of deionized water, performing ultrasonic treatment for 10min, and heating and stirring for 30 min; 2) adding 1mL of 0.5mol/L NaCl solution, stirring at high speed for 30min, and dropwise adding 1mL of 0.5mol/L AgNO₃Reacting the solution at 40 ℃ for 1 h; 3) adding 1mL of 0.1mol/L HCl solution, and adjusting the pH value of the solution to 5; 4) slowly adding 5g of silkworm excrement biochar for reaction for 3 hours; 5) centrifuging, washing, and vacuum drying at 30 deg.C for 24 hr; 6) adding into 25% glutaraldehyde solution, magnetically stirring for 3 hr, centrifuging, washing, and drying in a vacuum drying oven at 40 deg.C overnight to obtain nanometer antibacterial agent grafted faeces Bombycis biochar;

(3) uniformly stirring nano antibacterial agent grafted silkworm excrement biochar, nylon 66 slices, epoxidized soybean oil, polytetrafluoroethylene and sodium-based or calcium-based montmorillonite in a kneading machine, and extruding and granulating by using a double-screw extruder, wherein the extrusion temperature is 270 ℃, and the screw rotating speed is 150 r/min;

(4) and (3) after vacuum drying, spinning by using a spinneret plate to obtain the nano antibacterial hairbrush material, wherein the diameter of the spinneret plate is 160mm, the number of the holes is 90, and the aperture is 0.8 mm.

The nano antibacterial hairbrush material prepared by the invention has good antibacterial performance, and the inhibition rate of the nano antibacterial hairbrush material on escherichia coli can reach 100% and the inhibition rates on staphylococcus aureus and bacillus subtilis can respectively reach 99.6% and 99.7% at most.

The properties of the examples are as follows: