CN117511056B - Polypropylene antibacterial material and preparation method thereof - Google Patents

Polypropylene antibacterial material and preparation method thereof Download PDF

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CN117511056B
CN117511056B CN202311468549.9A CN202311468549A CN117511056B CN 117511056 B CN117511056 B CN 117511056B CN 202311468549 A CN202311468549 A CN 202311468549A CN 117511056 B CN117511056 B CN 117511056B
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agent
parts
graphene
modified
stirring
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CN117511056A (en
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曾舒
张怡
黄晓枭
王聚恒
麻玉龙
杨康
曾化雨
钟安澜
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GUIZHOU INSTITUTE OF METALLURGY AND CHEMICAL ENGINEERING
Guizhou Tianrunda Science And Technology Co ltd
GUIZHOU NANO MATERIAL ENGINEERING CENTER
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GUIZHOU INSTITUTE OF METALLURGY AND CHEMICAL ENGINEERING
Guizhou Tianrunda Science And Technology Co ltd
GUIZHOU NANO MATERIAL ENGINEERING CENTER
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • 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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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/10—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K2003/0806—Silver
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • 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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

The invention relates to the technical field of polypropylene antibiosis, and particularly discloses a polypropylene antibiosis material, which comprises polypropylene resin, a carrier nano silver agent, an effective and double-effect modifying agent and a modifying and blending agent based on glass fibers; wherein the mass ratio of the polypropylene resin to the nano silver agent as the carrier to the modified blending agent based on the glass fiber is (10-13): (4-6): (3-5):2. The polypropylene antibacterial material adopts polypropylene resin to match with a carrier nano silver agent, and the carrier nano silver agent formed by nano silicon dioxide, nano titanium dioxide, a phosphoric acid buffer solution, nano silver and a silane coupling agent can mutually coordinate system raw materials, and the two raw materials are mutually coordinated to jointly coordinate, so that the antibacterial durability and mechanical property of the product are improved, and the water-resistant and acid-resistant stability of the product is optimized.

Description

Polypropylene antibacterial material and preparation method thereof
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to a polypropylene antibacterial material and a preparation method thereof.
Background
Polypropylene (PP) is a semi-crystalline thermoplastic. Has high impact resistance, strong mechanical property and resistance to corrosion of various organic solvents and acid and alkali. The polymer has wide application in industry and is one of common polymer materials.
The antibacterial material of polypropylene adopted in the prior art is prepared by adopting polypropylene resin and antibacterial nano silver components, the interfacial property of nano silver in the polypropylene resin is poor, meanwhile, agglomeration is easy, the antibacterial effect and the mechanical property of plastic are influenced, the antibacterial performance of the product is poor, the antibacterial performance is not durable, the antibacterial performance and the mechanical property are difficult to coordinate and improve, meanwhile, the water-washing resistance and the acid corrosion resistance stability of the product are poor, and the antibacterial efficiency of the product is further limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a polypropylene antibacterial material and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a polypropylene antibacterial material, which comprises polypropylene resin, a carrier nano silver agent, an effective and double-effect modifying agent and a modifying and blending agent based on glass fibers; wherein the mass ratio of the polypropylene resin to the nano silver agent as the carrier to the modified blending agent based on the glass fiber is (10-13): (4-6): (3-5) 2;
The preparation method of the carrier nano silver agent comprises the following steps:
Adding 4-7 parts of nano silicon dioxide and 3-5 parts of nano titanium dioxide into 10-15 parts of deionized water, then adding 2-3 parts of phosphoric acid buffer solution, and stirring thoroughly to obtain a mixed solution of nano silicon dioxide/titanium dioxide;
Adding 10-15 parts by weight of nano silver into 35-40 parts by weight of mixed solution of nano silicon dioxide/titanium dioxide, then adding 1-3 parts of silane coupling agent, and stirring and uniformly mixing to obtain the carrier nano silver agent.
Preferably, the pH value of the phosphate buffer solution is 5.0-5.5; the silane coupling agent is silane coupling agent KH560.
Preferably, the preparation method of the effective and adjustable double-effect modifier comprises the following steps:
s01: preparing a thermally regulated graphene agent:
firstly placing the flaky graphene into a potassium permanganate solution with the total amount of 3-5 times of the flaky graphene, uniformly stirring, and then washing and drying to obtain a flaky graphene agent;
preheating the flaky graphene agent at 150-170 ℃ for 5-10min, then heating to 265-275 ℃ at the speed of 2-5 ℃/min, and preserving heat for 2-5min;
then cooling to 50-55 ℃ at a speed of 1-2 ℃/min to obtain a thermally regulated graphene agent;
S02: immersing the thermally regulated graphene agent into an effect regulating modifying liquid which is 4-7 times of the total amount of the thermally regulated graphene agent, and after the treatment is finished, washing and drying to obtain the effect regulating modified graphene;
S03: preparation of the improved treatment agent:
Mixing 8-12 parts of sodium silicate, 20-25 parts of deionized water and 2-5 parts of glycolic acid uniformly at 65-70 ℃ to obtain sodium silicate solution;
Adding 4-7 parts of silicon carbide whisker into sodium silicate solution, then adding 2-4 parts of yttrium nitrate solution with mass fraction of 2-5%, and continuously stirring thoroughly to obtain an improved treating agent;
s04: mixing and ball milling the modified graphene and the modified treating agent according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 1-2h, and washing and drying are carried out after ball milling, so that the modified graphene and the modified treating agent are obtained.
Preferably, the diameter of the flaky graphene is 25-30um, and the thickness of the flaky graphene is 30-35um; the mass fraction of the potassium permanganate solution is 5-10%.
Preferably, the immersion pressure of the immersion treatment is 10-15MPa, and the immersion time is 30-40min.
Preferably, the effect-modifying liquid is sodium lignin sulfonate solution with the mass fraction of 5-7%.
Preferably, the preparation method of the glass fiber-based modified blending agent comprises the following steps:
s101: adding 3-5 parts of nano silica sol and 1-2 parts of urea into 5-10 parts of deionized water, then adding 2-4 parts of lanthanum chloride solution and 0.35-0.45 part of sodium dodecyl benzene sulfonate, and stirring fully to obtain a modified liquid;
S102: uniformly stirring glass fibers in hydrochloric acid solution with the mass fraction of 2% which is 3-5 times of the total amount of the glass fibers, and then washing and drying to obtain pretreated glass fibers;
S103: and (3) stirring the pretreated glass fiber and the modified liquid of S101 according to the weight ratio of 2:5 for reaction, and washing and drying after stirring is finished to obtain the glass fiber modified blending agent.
Preferably, the mass fraction of the lanthanum chloride solution in the S101 is 3-6%; the temperature of stirring reaction treatment in the step S103 is 48-52 ℃, the stirring time is 25-35min, and the stirring rotating speed is 500-700r/min.
The invention also provides a preparation method of the polypropylene antibacterial material, which comprises the following steps:
adding the effective and adjustable double-effect modifier and the glass fiber-based modifying modifier into the carrier nano silver agent for ultrasonic dispersion treatment, ending ultrasonic treatment, washing with water, drying, then carrying out melt blending treatment on the dried product and the polypropylene resin, and ending the treatment to obtain the polypropylene antibacterial material.
Preferably, the ultrasonic power of the ultrasonic dispersion treatment is 350-400W, and the ultrasonic time is 20-30min; the melt blending temperature is 170-220 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. The polypropylene antibacterial material adopts polypropylene resin to match with a carrier nano silver agent, and the carrier nano silver agent formed by nano silicon dioxide, nano titanium dioxide, a phosphoric acid buffer solution, nano silver and a silane coupling agent can mutually coordinate system raw materials, improve interface compatibility among the raw materials, improve dispersion effect of nano silver, improve dispersion efficiency of an enhanced effect-adjusting double-effect modifier and a glass fiber-based modified modifier in the system, mutually coordinate the raw materials, jointly coordinate, improve antibacterial durability and mechanical property of a product, and optimize water resistance and acid corrosion resistance stability of the product;
2. The effective and adjustable double-effect modifier adopts graphene to be matched with potassium permanganate solution, so that the activity of the graphene is optimized, the graphene is preheated for 5-10min at 150-170 ℃, then the graphene is heated to 265-275 ℃ at the speed of 2-5 ℃/min, and the graphene is kept for 2-5min; then cooling to 50-55 ℃ at a speed of 1-2 ℃/min, optimizing the activity efficiency and flexibility of graphene, inserting and improving the interfacial property of raw materials of the system into the system, enhancing the mechanical property of the product, optimizing the activity interfacial efficiency of the graphene by the graphene treated by the modified solution for the effective adjustment of the sodium lignin sulfonate solution, and then cooperating with the modified treatment agent, thereby enhancing the antibacterial persistence and mechanical property of the system;
3. The glass fiber-based modifying and blending agent is prepared by modifying glass fibers by adopting a modifying solution obtained by processing glass fibers by hydrochloric acid solution to optimize the activity and dispersity of the glass fibers, and modifying the glass fibers by using a modifying solution obtained by matching nano silica sol, urea, lanthanum chloride solution and sodium dodecyl benzene sulfonate, so that the synergistic effect of the glass fiber-based modifying and blending agent and the effective and double-effect modifying agent is further enhanced, the antibacterial durability and mechanical property of the product are improved in a coordinated manner, and the acid corrosion resistance and water washing resistance stability of the product are further improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The polypropylene antibacterial material comprises polypropylene resin, a carrier nano silver agent, an effective and double-effect modifying agent and a modifying and blending agent based on glass fibers; wherein the mass ratio of the polypropylene resin to the nano silver agent as the carrier to the modified blending agent based on the glass fiber is (10-13): (4-6): (3-5) 2;
The preparation method of the carrier nano silver agent comprises the following steps:
Adding 4-7 parts of nano silicon dioxide and 3-5 parts of nano titanium dioxide into 10-15 parts of deionized water, then adding 2-3 parts of phosphoric acid buffer solution, and stirring thoroughly to obtain a mixed solution of nano silicon dioxide/titanium dioxide;
Adding 10-15 parts by weight of nano silver into 35-40 parts by weight of mixed solution of nano silicon dioxide/titanium dioxide, then adding 1-3 parts of silane coupling agent, and stirring and uniformly mixing to obtain the carrier nano silver agent.
The pH value of the phosphoric acid buffer solution of the embodiment is 5.0-5.5; the silane coupling agent is silane coupling agent KH560.
The preparation method of the effective and adjustable double-effect improver comprises the following steps:
s01: preparing a thermally regulated graphene agent:
firstly placing the flaky graphene into a potassium permanganate solution with the total amount of 3-5 times of the flaky graphene, uniformly stirring, and then washing and drying to obtain a flaky graphene agent;
preheating the flaky graphene agent at 150-170 ℃ for 5-10min, then heating to 265-275 ℃ at the speed of 2-5 ℃/min, and preserving heat for 2-5min;
then cooling to 50-55 ℃ at a speed of 1-2 ℃/min to obtain a thermally regulated graphene agent;
S02: immersing the thermally regulated graphene agent into an effect regulating modifying liquid which is 4-7 times of the total amount of the thermally regulated graphene agent, and after the treatment is finished, washing and drying to obtain the effect regulating modified graphene;
S03: preparation of the improved treatment agent:
Mixing 8-12 parts of sodium silicate, 20-25 parts of deionized water and 2-5 parts of glycolic acid uniformly at 65-70 ℃ to obtain sodium silicate solution;
Adding 4-7 parts of silicon carbide whisker into sodium silicate solution, then adding 2-4 parts of yttrium nitrate solution with mass fraction of 2-5%, and continuously stirring thoroughly to obtain an improved treating agent;
s04: mixing and ball milling the modified graphene and the modified treating agent according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 1-2h, and washing and drying are carried out after ball milling, so that the modified graphene and the modified treating agent are obtained.
The diameter of the flaky graphene is 25-30um, and the thickness is 30-35um; the mass fraction of the potassium permanganate solution is 5-10%.
The immersion pressure of the immersion treatment of this example was 10-15MPa, and the immersion time was 30-40min.
The effective regulating and modifying liquid of the embodiment is sodium lignin sulfonate solution with the mass fraction of 5-7%.
The preparation method of the glass fiber-based modified blending agent comprises the following steps:
s101: adding 3-5 parts of nano silica sol and 1-2 parts of urea into 5-10 parts of deionized water, then adding 2-4 parts of lanthanum chloride solution and 0.35-0.45 part of sodium dodecyl benzene sulfonate, and stirring fully to obtain a modified liquid;
S102: uniformly stirring glass fibers in hydrochloric acid solution with the mass fraction of 2% which is 3-5 times of the total amount of the glass fibers, and then washing and drying to obtain pretreated glass fibers;
S103: and (3) stirring the pretreated glass fiber and the modified liquid of S101 according to the weight ratio of 2:5 for reaction, and washing and drying after stirring is finished to obtain the glass fiber modified blending agent.
In the S101 of the embodiment, the mass fraction of the lanthanum chloride solution is 3-6%; the temperature of stirring reaction treatment in the step S103 is 48-52 ℃, the stirring time is 25-35min, and the stirring rotating speed is 500-700r/min.
The preparation method of the polypropylene antibacterial material comprises the following steps:
adding the effective and adjustable double-effect modifier and the glass fiber-based modifying modifier into the carrier nano silver agent for ultrasonic dispersion treatment, ending ultrasonic treatment, washing with water, drying, then carrying out melt blending treatment on the dried product and the polypropylene resin, and ending the treatment to obtain the polypropylene antibacterial material.
The ultrasonic power of the ultrasonic dispersion treatment of the embodiment is 350-400W, and the ultrasonic time is 20-30min; the melt blending temperature is 170-220 ℃.
Example 1.
The polypropylene antibacterial material comprises polypropylene resin, a carrier nano silver agent, an effective and double-effect modifying agent and a modifying and blending agent based on glass fibers; wherein the mass ratio of the polypropylene resin to the nano silver agent to the modified additive based on glass fiber is 10:4:3:2;
The preparation method of the carrier nano silver agent comprises the following steps:
adding 4 parts of nano silicon dioxide and 3 parts of nano titanium dioxide into 10 parts of deionized water, and then adding 2 parts of phosphoric acid buffer solution, and stirring thoroughly to obtain a mixed solution of nano silicon dioxide/titanium dioxide;
Adding 10 parts by weight of nano silver into 35 parts by weight of mixed solution of nano silicon dioxide/titanium dioxide, then adding 1 part of silane coupling agent, and stirring and mixing uniformly to obtain the carrier nano silver agent.
The pH of the phosphate buffer solution of this example was 5.0; the silane coupling agent is silane coupling agent KH560.
The preparation method of the effective and adjustable double-effect improver comprises the following steps:
s01: preparing a thermally regulated graphene agent:
firstly placing the flaky graphene into a potassium permanganate solution with the total amount of 3 times of the flaky graphene, uniformly stirring, and then washing and drying to obtain a flaky graphene agent;
preheating the flaky graphene agent at 150 ℃ for 5min, then heating to 265 ℃ at a speed of 2 ℃/min, and preserving heat for 2min;
Then cooling to 50 ℃ at a speed of 1 ℃/min to obtain a thermally regulated graphene agent;
S02: immersing the thermally regulated graphene agent into an effect regulating modifying liquid which is 4 times of the total amount of the thermally regulated graphene agent, and after the treatment is finished, washing and drying to obtain the effect regulating modified graphene;
S03: preparation of the improved treatment agent:
Mixing 8 parts of sodium silicate, 20 parts of deionized water and 2 parts of glycolic acid uniformly at 65 ℃ to obtain sodium silicate solution;
Adding 4 parts of silicon carbide whisker into sodium silicate solution, then adding 2 parts of yttrium nitrate solution with the mass fraction of 2%, and continuously and fully stirring to obtain an improved treating agent;
s04: mixing and ball milling the modified graphene and the modified treating agent according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000r/min, the ball milling time is 1h, and washing and drying are carried out after ball milling is finished to obtain the modified graphene and modified treating agent.
The diameter of the flake graphene in the embodiment is 25um, and the thickness is 30um; the mass fraction of the potassium permanganate solution is 5%.
The immersion pressure of the immersion treatment of this example was 10MPa, and the immersion time was 30min.
The effect-adjusting modifying liquid of the embodiment is sodium lignin sulfonate solution with the mass fraction of 5%.
The preparation method of the glass fiber-based modified blending agent comprises the following steps:
S101: adding 3 parts of nano silica sol and 1 part of urea into 5 parts of deionized water, then adding 2 parts of lanthanum chloride solution and 0.35 part of sodium dodecyl benzene sulfonate, and stirring fully to obtain a modified liquid;
s102: uniformly stirring glass fibers in hydrochloric acid solution with the mass fraction of 2% which is 3 times that of the total glass fibers, and then washing and drying to obtain pretreated glass fibers;
S103: and (3) stirring the pretreated glass fiber and the modified liquid of S101 according to the weight ratio of 2:5 for reaction, and washing and drying after stirring is finished to obtain the glass fiber modified blending agent.
In the S101 of the embodiment, the mass fraction of the lanthanum chloride solution is 3%; the temperature of the stirring reaction treatment in the step S103 is 48 ℃, the stirring time is 25min, and the stirring rotating speed is 500r/min.
The preparation method of the polypropylene antibacterial material comprises the following steps:
adding the effective and adjustable double-effect modifier and the glass fiber-based modifying modifier into the carrier nano silver agent for ultrasonic dispersion treatment, ending ultrasonic treatment, washing with water, drying, then carrying out melt blending treatment on the dried product and the polypropylene resin, and ending the treatment to obtain the polypropylene antibacterial material.
The ultrasonic power of the ultrasonic dispersion treatment of the embodiment is 350W, and the ultrasonic time is 20min; the melt blending temperature is 170-220 ℃.
Example 2.
The polypropylene antibacterial material comprises polypropylene resin, a carrier nano silver agent, an effective and double-effect modifying agent and a modifying and blending agent based on glass fibers; wherein the mass ratio of the polypropylene resin to the nano silver agent to the modified additive based on glass fiber is 13:6:5:2;
The preparation method of the carrier nano silver agent comprises the following steps:
adding 7 parts of nano silicon dioxide and 5 parts of nano titanium dioxide into 15 parts of deionized water, and then adding 3 parts of phosphoric acid buffer solution, and stirring thoroughly to obtain a mixed solution of nano silicon dioxide/titanium dioxide;
15 parts by weight of nano silver is added into 40 parts by weight of mixed solution of nano silicon dioxide/titanium dioxide, then 3 parts of silane coupling agent is added, and the mixture is stirred and mixed uniformly to obtain the carrier nano silver agent.
The pH of the phosphate buffer solution of this example was 5.5; the silane coupling agent is silane coupling agent KH560.
The preparation method of the effective and adjustable double-effect improver comprises the following steps:
s01: preparing a thermally regulated graphene agent:
firstly placing the flaky graphene into a potassium permanganate solution with the total amount of 5 times of the flaky graphene, uniformly stirring, and then washing and drying to obtain a flaky graphene agent;
preheating the flaky graphene agent at 170 ℃ for 10min, then heating to 275 ℃ at a speed of 5 ℃/min, and preserving heat for 5min;
then cooling to 55 ℃ at a speed of 2 ℃/min to obtain a thermally regulated graphene agent;
s02: immersing the thermally regulated graphene agent into an effect regulating modifying liquid which is 7 times of the total amount of the thermally regulated graphene agent, and after the treatment is finished, washing and drying to obtain the effect regulating modified graphene;
S03: preparation of the improved treatment agent:
mixing 12 parts of sodium silicate, 25 parts of deionized water and 5 parts of glycolic acid uniformly at 70 ℃ to obtain sodium silicate solution;
adding 7 parts of silicon carbide whisker into sodium silicate solution, then adding 4 parts of yttrium nitrate solution with mass fraction of 5%, and continuously stirring thoroughly to obtain an improved treating agent;
s04: mixing and ball milling the modified graphene and the modified treating agent according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1500r/min, the ball milling time is 2h, and washing and drying are carried out after ball milling is finished to obtain the modified graphene and modified treating agent.
The diameter of the flaky graphene in the embodiment is 30um, and the thickness is 35um; the mass fraction of the potassium permanganate solution is 10%.
The immersion pressure of the immersion treatment of this example was 15MPa, and the immersion time was 40min.
The effect-adjusting modifying liquid of the embodiment is sodium lignin sulfonate solution with the mass fraction of 7%.
The preparation method of the glass fiber-based modified blending agent comprises the following steps:
S101: adding 5 parts of nano silica sol and 2 parts of urea into 10 parts of deionized water, then adding 4 parts of lanthanum chloride solution and 0.45 part of sodium dodecyl benzene sulfonate, and stirring fully to obtain a modified liquid;
S102: uniformly stirring glass fibers in hydrochloric acid solution with the mass fraction of 2% which is 5 times that of the total glass fibers, and then washing and drying to obtain pretreated glass fibers;
S103: and (3) stirring the pretreated glass fiber and the modified liquid of S101 according to the weight ratio of 2:5 for reaction, and washing and drying after stirring is finished to obtain the glass fiber modified blending agent.
In the S101 of the embodiment, the mass fraction of the lanthanum chloride solution is 6%; the temperature of the stirring reaction treatment in the step S103 is 52 ℃, the stirring time is 35min, and the stirring rotating speed is 700r/min.
The preparation method of the polypropylene antibacterial material comprises the following steps:
adding the effective and adjustable double-effect modifier and the glass fiber-based modifying modifier into the carrier nano silver agent for ultrasonic dispersion treatment, ending ultrasonic treatment, washing with water, drying, then carrying out melt blending treatment on the dried product and the polypropylene resin, and ending the treatment to obtain the polypropylene antibacterial material.
The ultrasonic power of the ultrasonic dispersion treatment of the embodiment is 400W, and the ultrasonic time is 30min; the melt blending temperature is 170-220 ℃.
Example 3.
The polypropylene antibacterial material comprises polypropylene resin, a carrier nano silver agent, an effective and double-effect modifying agent and a modifying and blending agent based on glass fibers; wherein the mass ratio of the polypropylene resin to the nano silver agent to the modified additive based on glass fiber is 12:5:4:2;
The preparation method of the carrier nano silver agent comprises the following steps:
Adding 5.5 parts of nano silicon dioxide and 4 parts of nano titanium dioxide into 12.5 parts of deionized water, and then adding 2.5 parts of phosphoric acid buffer solution, and stirring thoroughly to obtain a mixed solution of nano silicon dioxide/titanium dioxide;
Adding 12.5 parts by weight of nano silver into 37.5 parts by weight of mixed solution of nano silicon dioxide/titanium dioxide, then adding 2 parts of silane coupling agent, and stirring and mixing uniformly to obtain the carrier nano silver agent.
The pH of the phosphate buffer solution of this example was 5.2; the silane coupling agent is silane coupling agent KH560.
The preparation method of the effective and adjustable double-effect improver comprises the following steps:
s01: preparing a thermally regulated graphene agent:
Firstly placing the flaky graphene into a potassium permanganate solution with the total amount of 4 times of the flaky graphene, uniformly stirring, and then washing and drying to obtain a flaky graphene agent;
Preheating the flaky graphene agent at 160 ℃ for 7.5min, then heating to 270 ℃ at the speed of 3.5 ℃/min, and preserving heat for 3.5min;
Then cooling to 52 ℃ at a speed of 1.5 ℃/min to obtain a thermally regulated graphene agent;
S02: immersing the thermally regulated graphene agent into an effect regulating modifying liquid which is 5.5 times of the total amount of the thermally regulated graphene agent, and after the treatment is finished, washing and drying to obtain the effect regulating modified graphene;
S03: preparation of the improved treatment agent:
mixing 10 parts of sodium silicate, 22.5 parts of deionized water and 3.5 parts of glycolic acid uniformly at 68 ℃ to obtain sodium silicate solution;
Adding 5.5 parts of silicon carbide whisker into sodium silicate solution, then adding 3 parts of yttrium nitrate solution with mass fraction of 3.5%, and continuously stirring fully to obtain an improved treating agent;
S04: mixing and ball milling the modified graphene and the modified treating agent according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1250r/min, the ball milling time is 1.5h, and washing and drying are carried out after ball milling, so that the modified graphene and the modified treating agent are obtained.
The diameter of the flake graphene of the embodiment is 28um, and the thickness is 32.5um; the mass fraction of the potassium permanganate solution is 7.5%.
The immersion pressure of the immersion treatment of this example was 12.5MPa, and the immersion time was 35min.
The effective modification liquid of the embodiment is sodium lignin sulfonate solution with the mass fraction of 6%.
The preparation method of the glass fiber-based modified blending agent comprises the following steps:
S101: adding 4 parts of nano silica sol and 1.5 parts of urea into 7.5 parts of deionized water, then adding 3 parts of lanthanum chloride solution and 0.40 part of sodium dodecyl benzene sulfonate, and stirring fully to obtain a modified liquid;
s102: uniformly stirring glass fibers in hydrochloric acid solution with the mass fraction of 2% which is 4 times that of the total glass fibers, and then washing and drying to obtain pretreated glass fibers;
S103: and (3) stirring the pretreated glass fiber and the modified liquid of S101 according to the weight ratio of 2:5 for reaction, and washing and drying after stirring is finished to obtain the glass fiber modified blending agent.
In the S101 of the embodiment, the mass fraction of the lanthanum chloride solution is 4.5%; the temperature of the stirring reaction treatment in the step S103 is 50 ℃, the stirring time is 30min, and the stirring rotating speed is 600r/min.
The preparation method of the polypropylene antibacterial material comprises the following steps:
adding the effective and adjustable double-effect modifier and the glass fiber-based modifying modifier into the carrier nano silver agent for ultrasonic dispersion treatment, ending ultrasonic treatment, washing with water, drying, then carrying out melt blending treatment on the dried product and the polypropylene resin, and ending the treatment to obtain the polypropylene antibacterial material.
The ultrasonic power of the ultrasonic dispersion treatment of the embodiment is 370W, and the ultrasonic time is 25min; the melt blending temperature is 170-220 ℃.
Comparative example 1.
The difference from example 3 is that the carrier nanosilver agent is replaced with nanosilver.
Comparative example 2.
The difference from example 3 is that no nano titanium dioxide or silane coupling agent is added in the preparation of the carrier nano silver agent.
Comparative example 3.
The difference from example 3 is that no dual effect modifier is added.
Comparative example 4.
The difference from example 3 is that the preparation method of the dual effect modifier is not treated by the step S01.
Comparative example 5.
The difference from example 3 is that no temperature rise to 270℃at a rate of 3.5℃per minute was employed in the S01 step treatment, and the incubation was carried out for 3.5 minutes.
Comparative example 6.
The difference from example 3 is that no dip treatment in the effect-modifying liquid is used in the preparation of the effect-modifying double-effect modifier.
Comparative example 7.
The difference from example 3 is that no treatment with the modifying treatment agent is used in the preparation of the dual effect modifier.
Comparative example 8.
The difference from example 3 is that the silicon carbide whisker and yttrium nitrate solution are not added in the preparation of the improved treating agent.
Comparative example 9.
Unlike example 3, the modified treatment agent was prepared by replacing the sodium silicate solution with deionized water.
Comparative example 10.
The difference from example 3 is that no modifying tempering agent based on glass fibers was added.
Comparative example 11.
The difference from example 3 is that no modification liquid treatment is used in the preparation of the glass fiber-based modification moderator.
Comparative example 12.
The difference from example 3 is that the lanthanum chloride solution and sodium dodecylbenzenesulfonate were not added to the modified liquid.
Comparative example 13.
The difference from example 3 is that no nano silica sol or urea was added to the modified liquid.
The products prepared in examples 1 to 3 and comparative examples 1 to 13 were tested for their antibacterial durability, mechanical properties, acid corrosion resistance (measured after the products were placed under 2% hydrochloric acid mist for 24 hours), water wash resistance (measured after the products were washed with water 100 times), and the test results were as follows;
The invention also places the product under 2% hydrochloric acid mist for 24 hours, and then measures the product, and the measurement result is as follows;
the invention also adopts the water washing for 100 times for measurement, and the measurement results are as follows:
It can be seen from comparative examples 1 to 13 and examples 1 to 3 that the product was washed with water 100 times and placed in 2% hydrochloric acid mist under conventional conditions;
the product of the embodiment 3 has excellent tensile strength, meanwhile, the escherichia coli antibacterial rate of the product can realize durable antibacterial performance, the antibacterial durability and the tensile strength performance can be improved in a coordinated manner, and meanwhile, the product has excellent performance stability under the conditions of 100 times of water washing and acid corrosion resistance;
As shown in comparative examples 1 to 9 and example 3, the nano silver agent is replaced by nano silver, no nano titanium dioxide and no silane coupling agent are added in the preparation of the nano silver agent, the performance of the product is prone to be deteriorated, no effective adjustment double-effect modifier is added, the performance deterioration effect of the product is obvious, the acid corrosion resistance and the washing stability are obvious, the preparation method of the effective adjustment double-effect modifier does not adopt S01 step treatment, the S01 step treatment does not adopt to raise the temperature to 270 ℃ at the speed of 3.5 ℃/min, the heat preservation is carried out for 3.5min, the preparation of the effective adjustment double-effect modifier does not adopt to be immersed in the effective adjustment modifying liquid, the preparation of the effective adjustment double-effect modifier does not adopt to be treated by the modifying treating agent, the silicon carbide whisker, the yttrium nitrate solution and the sodium silicate liquid are not added in the preparation of the modifying treating agent, and the performance of the product is prone to be deteriorated;
The product performance is obviously deteriorated without adopting the modified treatment agent in the preparation of the modified liquid and the modified double-effect modifier, and meanwhile, the modified treatment agent prepared by different methods and the S01 concrete step treatment are different, the product performance is in different degree deterioration trend, and only the modified liquid and the modified treatment agent prepared by the method are matched with the S01 concrete step of the invention, the product performance effect is most obvious, and other methods are adopted to replace the modified liquid and the modified treatment agent, which are not as obvious as the effect of the invention;
As shown in comparative example 1, comparative example 10 and example 3, the glass fiber-based modifying and blending agents and the effective and blending double-effect improving agents are not added, the performances of the products are obviously deteriorated, only the two agents are adopted to cooperate together, and the performance effect of the products is most obvious;
As can be seen from comparative examples 10 to 13 and example 3, the modified blending agent based on glass fiber is prepared without modifying liquid treatment, lanthanum chloride solution, sodium dodecyl benzene sulfonate and nano silica sol and urea are not added in the modified liquid, and the modified liquid prepared by different methods has a tendency of deterioration in performance effect, and the modified blending agent based on glass fiber obtained by the modified liquid prepared by the specific method only has the most remarkable performance effect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (5)

1. The polypropylene antibacterial material is characterized by comprising polypropylene resin, a carrier nano silver agent, an effective and double-effect modifying agent and a glass fiber-based modifying and blending agent; wherein the mass ratio of the polypropylene resin to the nano silver agent as the carrier to the modified blending agent based on the glass fiber is (10-13): (4-6): (3-5) 2;
The preparation method of the carrier nano silver agent comprises the following steps:
Adding 4-7 parts of nano silicon dioxide and 3-5 parts of nano titanium dioxide into 10-15 parts of deionized water, then adding 2-3 parts of phosphoric acid buffer solution, and stirring thoroughly to obtain a mixed solution of nano silicon dioxide/titanium dioxide;
Adding 10-15 parts by weight of nano silver into 35-40 parts by weight of mixed solution of nano silicon dioxide/titanium dioxide, then adding 1-3 parts of silane coupling agent, and stirring and mixing uniformly to obtain a carrier nano silver agent;
The preparation method of the effective and adjustable double-effect modifier comprises the following steps:
s01: preparing a thermally regulated graphene agent:
firstly placing the flaky graphene into a potassium permanganate solution with the total amount of 3-5 times of the flaky graphene, uniformly stirring, and then washing and drying to obtain a flaky graphene agent;
preheating the flaky graphene agent at 150-170 ℃ for 5-10min, then heating to 265-275 ℃ at the speed of 2-5 ℃/min, and preserving heat for 2-5min;
then cooling to 50-55 ℃ at a speed of 1-2 ℃/min to obtain a thermally regulated graphene agent;
S02: immersing the thermally regulated graphene agent into an effect regulating modifying liquid which is 4-7 times of the total amount of the thermally regulated graphene agent, and after the treatment is finished, washing and drying to obtain the effect regulating modified graphene;
S03: preparation of the improved treatment agent:
Mixing 8-12 parts of sodium silicate, 20-25 parts of deionized water and 2-5 parts of glycolic acid uniformly at 65-70 ℃ to obtain sodium silicate solution;
Adding 4-7 parts of silicon carbide whisker into sodium silicate solution, then adding 2-4 parts of yttrium nitrate solution with mass fraction of 2-5%, and continuously stirring thoroughly to obtain an improved treating agent;
S04: mixing and ball milling the modified graphene and the modified treating agent according to a weight ratio of 5:2, wherein the ball milling rotating speed is 1000-1500r/min, the ball milling time is 1-2h, and washing and drying are carried out after ball milling to obtain the modified graphene and modified treating agent; the preparation method of the glass fiber-based modified blending agent comprises the following steps:
s101: adding 3-5 parts of nano silica sol and 1-2 parts of urea into 5-10 parts of deionized water, then adding 2-4 parts of lanthanum chloride solution and 0.35-0.45 part of sodium dodecyl benzene sulfonate, and stirring fully to obtain a modified liquid;
S102: uniformly stirring glass fibers in hydrochloric acid solution with the mass fraction of 2% which is 3-5 times of the total amount of the glass fibers, and then washing and drying to obtain pretreated glass fibers;
s103: stirring the pretreated glass fiber and the modified liquid of S101 according to the weight ratio of 2:5 for reaction, and washing and drying after stirring is finished to obtain a modified blending agent of the glass fiber;
The immersing pressure of the immersing treatment is 10-15MPa, and the immersing time is 30-40min; the effect-regulating modifying liquid is sodium lignin sulfonate solution with the mass fraction of 5-7%; the mass fraction of the lanthanum chloride solution in the S101 is 3-6%; the temperature of stirring reaction treatment in the step S103 is 48-52 ℃, the stirring time is 25-35min, and the stirring rotating speed is 500-700r/min.
2. The polypropylene antimicrobial material according to claim 1, wherein the pH of the phosphate buffer solution is 5.0-5.5; the silane coupling agent is silane coupling agent KH560.
3. The polypropylene antibacterial material according to claim 1, wherein the diameter of the flaky graphene is 25-30um and the thickness is 30-35um; the mass fraction of the potassium permanganate solution is 5-10%.
4. A method for preparing the polypropylene antibacterial material according to any one of claims 1 to 3, comprising the steps of:
Adding the effective and adjustable double-effect modifier and the glass fiber-based modifying modifier into the carrier nano silver agent for ultrasonic dispersion treatment, ending ultrasonic treatment, washing with water, drying, then carrying out melt blending treatment on the dried product and the polypropylene resin, and ending the treatment to obtain the polypropylene antibacterial material.
5. The method for preparing a polypropylene antibacterial material according to claim 4, wherein the ultrasonic power of the ultrasonic dispersion treatment is 350-400W, and the ultrasonic time is 20-30min; the melt blending temperature is 170-220 ℃.
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