CN111041828A - Lasting antibacterial polypropylene non-woven fabric and preparation method thereof - Google Patents

Lasting antibacterial polypropylene non-woven fabric and preparation method thereof Download PDF

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CN111041828A
CN111041828A CN201911207640.9A CN201911207640A CN111041828A CN 111041828 A CN111041828 A CN 111041828A CN 201911207640 A CN201911207640 A CN 201911207640A CN 111041828 A CN111041828 A CN 111041828A
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woven fabric
polypropylene non
glucitol
polypropylene
alkylamino
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曾艳清
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    • C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
    • C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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    • D06M13/144—Alcohols; Metal alcoholates
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Abstract

The invention discloses a durable antibacterial polypropylene non-woven fabric and a preparation method thereof. The preparation method of the lasting antibacterial polypropylene non-woven fabric comprises the following steps: (1) graft copolymerization of glycidyl methacrylate or acrylic acid on polypropylene non-woven fabric; (2) fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate or acrylic acid; (3) and (6) dipping and finishing. The polypropylene non-woven fabric has excellent broad-spectrum antibacterial performance, lasting effect, good wettability and blood compatibility.

Description

Lasting antibacterial polypropylene non-woven fabric and preparation method thereof
Technical Field
The invention relates to the technical field of non-woven fabric products, in particular to a durable antibacterial polypropylene non-woven fabric and a preparation method thereof.
Background
The polypropylene non-woven fabric belongs to a composite non-woven fabric, is a new-generation environment-friendly material, has the advantages of high strength, excellent protective performance, ventilation, comfort, environmental protection, no toxicity, no odor and the like, and is widely applied to the field of medical health at present, such as surgical gowns, surgical caps, surgical drape fabrics, surgical cover fabrics, sterilization bandages, protective clothing and the like, so that the market puts higher requirements on the antibacterial performance of the polypropylene non-woven fabric.
Microorganisms occupy a very important position in our lives, being closely related to human life. It can not only decompose organic matters to promote substance circulation, but also cause food deterioration and corrosion of commercial appliances and the like; when the microecological balance of the human body is achieved, the microecological balance can coexist with the human body to help the human body to increase the resistance, and when the balance is broken, the human health can be threatened, so that the disease trouble is brought to people. The microorganisms are friends and enemies of human beings, so the relationship between the microorganisms and the human beings should be reasonably seen, and the microorganisms are antibacterial but are not excessively used, so that the microecological balance is ensured.
The antibacterial type is classified into an antimicrobial adhesion type and a bactericidal type, and the bactericidal type is further classified into a contact bactericidal type and a release bactericidal type. Different antibacterial materials have different characteristics, the adhesion resistance type can prevent the adhesion of microorganisms, and the formation of a biological film is avoided by inhibiting bacteria at the initial stage of the interaction of the microorganisms and the materials; the contact sterilization type material can kill bacteria adhered on the surface of the material and has stable sterilization efficiency; the released sterilization type material can kill bacteria adhered to the material and bacteria around the material, and certain materials can realize controllable release of sterilization, and have long sterilization duration and good effect.
Disclosure of Invention
One of the technical problems to be solved by the invention is to provide a preparation method of a durable antibacterial polypropylene non-woven fabric.
Specifically, the preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of glycidyl methacrylate or acrylic acid on polypropylene nonwoven: carrying out plasma treatment on the surface of the polypropylene non-woven fabric to generate polar groups on the surface, and then initiating glycidyl methacrylate or acrylic acid graft copolymerization on the polypropylene non-woven fabric by utilizing ultraviolet irradiation to obtain the polypropylene non-woven fabric grafted with glycidyl methacrylate or acrylic acid;
(2) fixing alkylamino glucitol on the surface of polypropylene non-woven fabric grafted with glycidyl methacrylate or acrylic acid: fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate or acrylic acid to obtain the polypropylene non-woven fabric with the alkylamino glucitol fixed on the surface;
(3) dipping and finishing: and (3) soaking the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol in the antibacterial finishing liquid, and baking the soaked fabric sample by adopting a one-soaking one-rolling process.
In some technical schemes of the invention, the preparation method of the lasting antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of glycidyl methacrylate on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: (10-30) placing the obtained product in absolute ethyl alcohol for ultrasonic cleaning for 1-2 hours, and drying the product at 50-60 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a chamber of a plasma processor, and setting the power to be 150-300W; setting the oxygen flow rate to be 40-300 sccm, carrying out plasma treatment in an oxygen atmosphere for 60-120 seconds, and placing in the air for 10-20 minutes after the treatment to obtain a polypropylene non-woven fabric subjected to plasma treatment; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: (10-30) g/mL of the solution is put into a glycidyl methacrylate aqueous solution with the mass fraction of 5-10%, and the grafting reaction is performed for 6-15 minutes under the ultraviolet power of 300-500W; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) g/mL of the solution is placed in acetone to be washed for 12-24 hours, and the solution is dried at the temperature of 50-60 ℃ to constant weight, so that the polypropylene non-woven fabric grafted with the glycidyl methacrylate is obtained;
(2) fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate: placing the polypropylene non-woven fabric grafted with glycidyl methacrylate into a container, wherein the solid-liquid ratio is 1: (20-40) g/mL is put into a mixed solvent, and the mixed solvent is prepared from methanol and alkylamino glucitol according to the volume ratio of (15-20): 1, carrying out reflux reaction for 36-72 hours at 70-80 ℃ under stirring at 50-130 r/min; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) washing the obtained product in absolute ethyl alcohol for 12-24 hours at a concentration of g/mL, and drying the washed product at a temperature of 50-60 ℃ to constant weight to obtain a polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: (10-25) g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3-5 minutes, one soaking and one rolling are carried out, and the rolling residue rate is 70-80%; and baking the padded polypropylene non-woven fabric at 130-140 ℃ for 2-10 minutes to obtain the polypropylene non-woven fabric.
Further, the preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of acrylic acid on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: (10-30) placing the obtained product in absolute ethyl alcohol for ultrasonic cleaning for 1-2 hours, and drying the product at 50-60 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a chamber of a plasma processor, and setting the power to be 150-300W; setting the oxygen flow rate to be 40-300 sccm, carrying out plasma treatment in an oxygen atmosphere for 60-120 seconds, and placing in the air for 10-20 minutes after the treatment to obtain a polypropylene non-woven fabric subjected to plasma treatment; butanone is adopted as the raw material: ethanol: the volume ratio of water is (5-10): (5-10): (80-90) preparing an acrylic acid solution with the mass fraction of 5-10% by taking the mixed solution as a solvent; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: (10-30) g/mL of the solution is put into an acrylic acid solution, and the grafting reaction is performed for 6-15 minutes under the ultraviolet power of 300-500W; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) g/mL of the acrylic acid grafted polypropylene non-woven fabric is placed in acetone to be washed for 12-24 hours, and dried at 50-60 ℃ to constant weight to obtain acrylic acid grafted polypropylene non-woven fabric;
(2) fixing alkylamino glucitol on the surface of the acrylic acid grafted polypropylene non-woven fabric: placing the acrylic acid grafted polypropylene non-woven fabric into a container, wherein the solid-liquid ratio is 1: (20-40) g/mL is put into a mixed solvent, and the mixed solvent is prepared from methanol and alkylamino glucitol according to the volume ratio of (15-20): 1, reacting for 8-12 hours at 60-80 ℃ under stirring at 50-130 r/min; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) washing the obtained product in absolute ethyl alcohol for 12-24 hours at a concentration of g/mL, and drying the washed product at a temperature of 50-60 ℃ to constant weight to obtain a polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: (10-25) g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3-5 minutes, one soaking and one rolling are carried out, and the rolling residue rate is 70-80%; and baking the padded polypropylene non-woven fabric at 130-140 ℃ for 2-10 minutes to obtain the polypropylene non-woven fabric.
In the two technical schemes, the principle of fixing the alkylamino glucitol on the surface of the polypropylene non-woven fabric is different: fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate through an epoxy group; and (3) performing amidation reaction on a secondary amine bond of the alkylamino glucitol and a carboxyl group on the acrylic acid on the surface of the acrylic acid grafted polypropylene non-woven fabric to fix the alkylamino glucitol.
In the two technical schemes, the alkylamino glucitol is one or a mixture of more of n-butyl amino glucitol, n-octyl amino glucitol and lauryl amino glucitol.
Among them, n-butylaminoglucitol, n-octylaminoglucitol, and dodecylaminoglucitol can be obtained by a commercially available method or can be prepared by a method described in a patent or literature.
For example, n-butylaminoglucitol can be prepared by: adding 5.40g of D-glucose and 3.67g of n-butylamine into a reaction device containing 100mL of methanol, and stirring at the constant temperature of 33 ℃ for 12 hours to generate n-butylamine glucose; after the reaction is stopped, cooling the reaction mixture in ice-water bath, adding 1.48g of sodium borohydride, reacting at 35 ℃ for 6 hours, and standing for 15 hours to generate n-butylamino glucitol; adjusting pH to 2 with 35% concentrated hydrochloric acid, converting the reaction product into n-butylaminoglucitol hydrochloride, cooling at-15 deg.C for 8 hr to precipitate hydrochloric acid salt, filtering with 200 mesh nylon cloth, and collecting filter cake; and (3) mixing the filter cake with ice water and ice ethanol in a volume ratio of 1: 10, washing with a mixed solvent, drying at 40 ℃ under the absolute pressure of 0.06MPa in vacuum until the weight is constant, and collecting a crude product; stirring the crude product in a sodium methoxide methanol solution with the mass fraction of 30% for 24 hours at room temperature, refluxing at 50 ℃ to decompose hydrochloride, naturally cooling to room temperature, and collecting precipitate; and (3) mixing the precipitate with ice water and ice methanol in a volume ratio of 1: 10, washing the mixture, and drying the mixture at 40 ℃ and the absolute pressure of 0.06MPa to constant weight to obtain the n-butylamino glucitol.
For example, n-octylaminoglucitol can be prepared by: (1) dissolving 9.02g of D-glucose in 30mL of distilled water to obtain a glucose solution; dissolving 3.87g of n-octylamine in 30mL of isopropanol, adding the solution into a glucose solution, stirring and uniformly mixing; reacting the reaction mixture at 40 ℃ for 7 hours to generate n-octylamine glucose; after the reaction is stopped, pouring the mixed solution into 300mL of distilled water, and standing for 6 hours to separate out n-octylamine glucose; filtering with 200 mesh nylon cloth, and collecting filter cake; recrystallizing the filter cake with anhydrous ethanol, filtering, washing with 30mL of glacial ethanol, and vacuum drying at 40 deg.C under 0.06MPa to constant weight to obtain n-octylamino glucose. (2) Mixing 5.82g of n-octylaminoglucose with 120mL of anhydrous methanol, and heating to 50 ℃ to dissolve the n-octylaminoglucose; dissolving 0.99g of sodium borohydride in 10mL of glacial methanol, adding the solution into a methanol solution of n-octylaminoglucose, reacting for 6 hours at 37 ℃, and standing for 15 hours at room temperature to generate n-octylaminoglucose alcohol; adding 200mL of distilled water, standing for 2 hours, performing centrifugal separation, and collecting solids; washing the solid with distilled water, and vacuum freeze-drying at-70 deg.C for 24 hr to obtain n-octylamine glucitol.
For example, lauryl glucosamine can be prepared by: (1) dissolving 9.02g of D-glucose in 30mL of distilled water to obtain a glucose solution; dissolving 5.55g of dodecylamine in 45mL of isopropanol, adding the solution into a glucose solution, stirring and mixing uniformly, and reacting at 40 ℃ for 7 hours to generate dodecylamine glucose; after the reaction is stopped, pouring the reaction mixture into 300mL of distilled water, and standing for 6 hours; filtering with 200 mesh nylon cloth, and collecting filter cake; recrystallizing the filter cake with absolute ethyl alcohol, filtering, washing with 30mL of glacial ethyl alcohol, and vacuum drying at 40 ℃ and absolute pressure of 0.06MPa to constant weight to obtain lauryl glucosamine; (2) mixing 6.94g of lauryl glucosamine and 120mL of anhydrous methanol, and heating to 50 ℃ to dissolve the lauryl glucose; dissolving 0.99g of sodium borohydride in 10mL of ice methanol, adding the solution into a methanol solution of lauryl amino glucose, reacting for 6 hours at 37 ℃, and standing for 15 hours at room temperature to generate lauryl amino glucose; adding 200mL of distilled water, standing for 2 hours, performing centrifugal separation, and collecting solids; washing the solid with distilled water, and vacuum freeze-drying at-70 deg.C for 24 hr to obtain lauryl amino glucitol.
Further, the antibacterial finishing liquid comprises the following components: 30-100 mL/L of aloe juice, 1-3 g/L of penetrant JFC, 5-10 g/L of chitosan or borneol modified chitosan, 2-4 g/L of protein and the balance of water.
Further, the aloe vera juice is obtained by the following method: cleaning fresh aloe, drying in the air until the surface has no moisture, cutting into pieces with the thickness of 0.5-1 cm, wrapping with gauze, and squeezing under a sealed environment for 20-40 minutes to obtain juice; heating the obtained juice to 100-120 ℃, preserving the heat for 50-80 minutes, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
Further, the preparation process of the borneol modified chitosan comprises the following steps:
(1) uniformly mixing 0.2-0.4 g of glycol chitosan and 25-35 mL of water, and carrying out ultrasonic treatment until the glycol chitosan is completely dissolved in the water to obtain a glycol chitosan solution; carrying out vacuum freeze drying on the glycol chitosan solution, and removing water to obtain a glycol chitosan freeze-dried substance;
(2) putting 0.4-0.7 g of p-aldehyde benzoic acid into a reaction device, adding 25-35 mL of tetrahydrofuran, introducing nitrogen for protection, adding 0.05-0.1 g of 4-dimethylaminopyridine and 1.5-2 g of dicyclohexylcarbodiimide as catalysts, finally adding 1-2 g of borneol, carrying out ice bath for 30-40 minutes, stirring at room temperature for 3-5 days, and collecting a reaction product; vacuum drying the reaction mixed product at 50-60 ℃ for 3-6 hours to obtain a crude product; the crude product was purified using petroleum ether: ethyl acetate volume ratio (10-20): 1 as eluent to carry out column chromatography separation, and collecting eluent; drying the eluent in vacuum at 50-60 ℃ to constant weight to obtain the para-aldehyde bornyl benzoate;
(3) dissolving 0.01-0.03 g of para-aldehyde bornyl benzoate in 2-4 mL of absolute ethanol to obtain a para-aldehyde bornyl benzoate solution; adding the p-aldehyde bornyl benzoate solution into the freeze-dried glycol chitosan obtained in the step (1), and standing at room temperature for 10-15 hours; centrifuging at 3000-4000 rpm for 20-30 minutes, and collecting reaction products; and cleaning the reaction product with ethanol, and drying at 50-60 ℃ in vacuum to constant weight to obtain the borneol modified chitosan.
Further, the protein is silk fibroin and/or wool keratin. Preferably, the protein is silk fibroin and wool keratin in a mass ratio of 1: 1, in a mixture of the components.
The polypropylene non-woven fabric has excellent broad-spectrum antibacterial performance, lasting effect, good wettability and blood compatibility.
Detailed Description
The raw materials in the examples are as follows:
polypropylene nonwoven Fabric, manufactured by Pujiang Xintai nonwoven Fabric Co., Ltd., gram weight 100g/m2。
Osmotic agent JFC, manufacturer Guangzhou Hongcheng chemical Co.
Chitosan, manufactured by Jinan Dongxuan bioengineering Co., Ltd., Cat. asfgas.
Silk fibroin, a manufacturer of Xian Jinheng chemical Co., Ltd., has a particle size of 2 μm.
Ethylene glycol chitosan, a product of Haizhu Biotech GmbH.
Wool keratin was prepared as described in example 1 of "a method for extracting wool keratin" of patent application No. 201511004518.3.
In a case not specifically described, the specific power of the ultrasound is 300W.
In the case where no specific explanation is made, the rotation speed of the stirring is 100 rpm.
In the case where no specific description is given, the specific conditions for the vacuum freeze-drying are: pre-freezing at-80 deg.c for 2 hr; the freezing temperature is-70 ℃, the freezing time is 24 hours, and the absolute pressure is 100 Pa.
Examples 1 to 3
The preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of glycidyl methacrylate on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: placing 10g/mL of the mixture in absolute ethyl alcohol, ultrasonically cleaning the mixture for 1 hour, and drying the mixture at 50 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a cavity of a DT-03 type plasma processor, and setting the power to be 150W; setting the oxygen flow rate to be 300sccm, carrying out plasma treatment in an oxygen atmosphere for 90 seconds, and placing in the air for 10 minutes after the treatment to obtain the polypropylene non-woven fabric subjected to plasma treatment; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: 20g/mL of the solution is put into glycidyl methacrylate aqueous solution with the mass fraction of 10 percent, and the grafting reaction is carried out for 8 minutes under the irradiation of 500W of ultraviolet power; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in acetone for 12 hours, and drying at 50 ℃ to constant weight to obtain the polypropylene non-woven fabric grafted with glycidyl methacrylate;
(2) fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate: placing the polypropylene non-woven fabric grafted with glycidyl methacrylate into a container, wherein the solid-liquid ratio is 1: putting 25g/mL of the mixed solvent into a mixed solvent, wherein the mixed solvent is prepared by mixing methanol and alkylamino glucitol according to a volume ratio of 20: 1, stirring at 80 rpm, and carrying out reflux reaction at 70 ℃ for 72 hours; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in absolute ethyl alcohol for 12 hours, and drying at 50 ℃ to constant weight to obtain polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: 20g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3 minutes, and the soaking and rolling are carried out once, wherein the rolling residual rate is 70 percent; and baking the padded polypropylene non-woven fabric at 130 ℃ for 10 minutes to obtain the polypropylene non-woven fabric.
The antibacterial finishing liquid comprises the following components: 40mL/L of aloe juice, 5g/L of chitosan, 4g/L of silk fibroin and the balance of deionized water, wherein the penetrant JFC3g/L is used as a penetrant.
The aloe juice is obtained by the following method: cleaning fresh aloe, air drying until no moisture exists on the surface, cutting into 0.8cm thick slices, wrapping with gauze, squeezing at 2000 rpm for 30 min under sealed environment, and collecting juice; heating the obtained juice to 110 deg.C at 2 deg.C/min, maintaining the temperature for 50 min, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
Examples 1 to 3 differ in that: the types of alkylamino glucitol are different, and n-butylaminoglucitol is used in example 1, n-octylaminoglucitol is used in example 2, and dodecylaminoglucitol is used in example 3.
Examples 4 to 6
The preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of acrylic acid on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: placing 10g/mL of the mixture in absolute ethyl alcohol, ultrasonically cleaning the mixture for 1 hour, and drying the mixture at 50 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a cavity of a DT-03 type plasma processor, and setting the power to be 150W; setting the oxygen flow rate to be 300sccm, carrying out plasma treatment in an oxygen atmosphere for 90 seconds, and placing in the air for 10 minutes after the treatment to obtain the polypropylene non-woven fabric subjected to plasma treatment; butanone is adopted as the raw material: ethanol: the water volume ratio is 5: 5: 90 is used as a solvent, and an acrylic acid solution with the mass fraction of 5% is prepared; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: placing 25g/mL of the solution into an acrylic acid solution, and carrying out irradiation grafting reaction for 8 minutes under the ultraviolet power of 500W; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in acetone for 12 hours, and drying at 50 ℃ to constant weight to obtain the acrylic acid grafted polypropylene non-woven fabric;
(2) fixing alkylamino glucitol on the surface of the acrylic acid grafted polypropylene non-woven fabric: placing the acrylic acid grafted polypropylene non-woven fabric into a container, wherein the solid-liquid ratio is 1: putting 25g/mL of the mixed solvent into a mixed solvent, wherein the mixed solvent is prepared by mixing methanol and alkylamino glucitol according to a volume ratio of 20: 1, reacting for 8 hours at 60 ℃ under the stirring of 80 revolutions per minute; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in absolute ethyl alcohol for 12 hours, and drying at 50 ℃ to constant weight to obtain polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: 20g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3 minutes, and the soaking and rolling are carried out once, wherein the rolling residual rate is 70 percent; and baking the padded polypropylene non-woven fabric at 130 ℃ for 10 minutes to obtain the polypropylene non-woven fabric.
The antibacterial finishing liquid comprises the following components: 40mL/L of aloe juice, 5g/L of chitosan, 4g/L of silk fibroin and the balance of deionized water, wherein the penetrant JFC3g/L is used as a penetrant.
The aloe juice is obtained by the following method: cleaning fresh aloe, air drying until no moisture exists on the surface, cutting into 0.8cm thick slices, wrapping with gauze, squeezing at 2000 rpm for 30 min under sealed environment, and collecting juice; heating the obtained juice to 110 deg.C at 2 deg.C/min, maintaining the temperature for 50 min, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
Examples 4 to 6 differ in that: the types of the alkylamino glucitols are different, namely n-butylaminoglucitol in example 4, n-octylaminoglucitol in example 5 and dodecylaminoglucitol in example 6.
Comparative examples 1 to 3
The preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of glycidyl methacrylate on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: placing 10g/mL of the mixture in absolute ethyl alcohol, ultrasonically cleaning the mixture for 1 hour, and drying the mixture at 50 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a cavity of a DT-03 type plasma processor, and setting the power to be 150W; setting the oxygen flow rate to be 300sccm, carrying out plasma treatment in an oxygen atmosphere for 90 seconds, and placing in the air for 10 minutes after the treatment to obtain the polypropylene non-woven fabric subjected to plasma treatment; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: 20g/mL of the solution is put into glycidyl methacrylate aqueous solution with the mass fraction of 10 percent, and the grafting reaction is carried out for 8 minutes under the irradiation of 500W of ultraviolet power; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in acetone for 12 hours, and drying at 50 ℃ to constant weight to obtain the polypropylene non-woven fabric grafted with glycidyl methacrylate;
(2) fixing alkylamine on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate: placing the polypropylene non-woven fabric grafted with glycidyl methacrylate into a container, wherein the solid-liquid ratio is 1: putting 25g/mL of the mixed solvent into a mixed solvent, wherein the mixed solvent is prepared by mixing methanol and alkylamine according to a volume ratio of 20: 1, stirring at 80 rpm, and carrying out reflux reaction at 70 ℃ for 8 hours; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in absolute ethyl alcohol for 12 hours, and drying at 50 ℃ to constant weight to obtain the polypropylene non-woven fabric with the alkylamine fixed on the surface;
(3) dipping and finishing: and (3) fixing the polypropylene non-woven fabric with alkylamine fixed on the surface in a solid-to-liquid ratio of 1: 20g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3 minutes, and the soaking and rolling are carried out once, wherein the rolling residual rate is 70 percent; and baking the padded polypropylene non-woven fabric at 130 ℃ for 10 minutes to obtain the polypropylene non-woven fabric.
The antibacterial finishing liquid comprises the following components: 40mL/L of aloe juice, 5g/L of chitosan, 4g/L of silk fibroin and the balance of deionized water, wherein the penetrant JFC3g/L is used as a penetrant.
The aloe juice is obtained by the following method: cleaning fresh aloe, air drying until no moisture exists on the surface, cutting into 0.8cm thick slices, wrapping with gauze, squeezing at 2000 rpm for 30 min under sealed environment, and collecting juice; heating the obtained juice to 110 deg.C at 2 deg.C/min, maintaining the temperature for 50 min, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
Comparative examples 1 to 3 differ in that: the kinds of alkylamine were different, and comparative example 1 was n-butylamine, comparative example 2 was n-octylamine, and comparative example 3 was dodecylamine.
Test example 1
The durable antibacterial polypropylene nonwoven fabrics of examples 1 to 6 and comparative examples 1 to 3 were subjected to protein adsorption test, and the smaller the adsorption amount of protein, the better the blood compatibility of the material. The specific method comprises the following steps:
① weighing 1.0g bovine serum albumin into a 100mL volumetric flask, and making the volume constant with phosphate buffer solution of pH 7.4 to obtain bovine serum albumin solution with concentration of 1 mg/mL.
② the standard curve is prepared by sequentially adding 40 μ L, 80 μ L, 120 μ L, 160 μ L and 200 μ L of the above 1mg/mL bovine serum albumin solution into a 10mL volumetric flask, diluting to constant volume with a pH 7.4 phosphate buffer solution to prepare bovine serum albumin solutions with concentrations of 4 μ g/mL, 8 μ g/mL, 12 μ g/mL, 16 μ g/mL and 20 μ g/mL as standard solutions, measuring absorbance values of the pure phosphate buffer solution (i.e. bovine serum albumin concentration is 0) and the above five bovine serum albumin standard solutions at 570nm in a microplate reader, and performing linear simulation with the obtained absorbance as ordinate and the concentration abscissa of the standard solution.
③ cut the sample to 1cm2Sterilizing the mixture with ethanol for 30 minutes, and then vacuum-drying the mixture for 10 hours; putting the sample into a pore plate, and adding a phosphate buffer solution with the pH of 7.4 to soak for 2 hours; removing the phosphate solution, adding 1mL of 1mg/mL bovine serum albumin solution, and dynamically adsorbing for 2 hours at 37 ℃ in a shaking table; removing the bovine serum albumin solution, and washing for 5-6 times by using a PBS solution; adding 1mL of 1% sodium dodecyl sulfate aqueous solution into a new PS pore plate, transferring the membrane into the pore plate by using a clean forceps soaked in the sodium dodecyl sulfate solution, and ultrasonically desorbing for 30 minutes; taking 150 mu L desorption solution, then adding 150 mu LBCA color developing agent, standing for 1 hour at 60 ℃, and developing color; cooling to room temperature, and measuring the light absorption value of 570nm by using an enzyme-labeling instrument; and obtaining the protein adsorption quantity according to the measured light absorption value and the standard curve.
The specific test results are shown in table 1.
TABLE 1 protein adsorption amount test sheet
Figure BDA0002297267150000121
As can be seen from table 1, examples 2 and 3 according to the present invention have good protein adsorption resistance and excellent blood compatibility.
Example 7
The preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of glycidyl methacrylate on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: placing 10g/mL of the mixture in absolute ethyl alcohol, ultrasonically cleaning the mixture for 1 hour, and drying the mixture at 50 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a cavity of a DT-03 type plasma processor, and setting the power to be 150W; setting the oxygen flow rate to be 300sccm, carrying out plasma treatment in an oxygen atmosphere for 90 seconds, and placing in the air for 10 minutes after the treatment to obtain the polypropylene non-woven fabric subjected to plasma treatment; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: 20g/mL of the solution is put into glycidyl methacrylate aqueous solution with the mass fraction of 10 percent, and the grafting reaction is carried out for 8 minutes under the irradiation of 500W of ultraviolet power; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in acetone for 12 hours, and drying at 50 ℃ to constant weight to obtain the polypropylene non-woven fabric grafted with glycidyl methacrylate;
(2) fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate: placing the polypropylene non-woven fabric grafted with glycidyl methacrylate into a container, wherein the solid-liquid ratio is 1: putting 25g/mL of the mixed solvent into a mixed solvent, wherein the mixed solvent is prepared by mixing methanol and n-octylamine glucitol according to a volume ratio of 20: 1, stirring at 80 rpm, and carrying out reflux reaction at 70 ℃ for 72 hours; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in absolute ethyl alcohol for 12 hours, and drying at 50 ℃ to constant weight to obtain polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: 20g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3 minutes, and the soaking and rolling are carried out once, wherein the rolling residual rate is 70 percent; and baking the padded polypropylene non-woven fabric at 130 ℃ for 10 minutes to obtain the polypropylene non-woven fabric.
The antibacterial finishing liquid comprises the following components: 40mL/L of aloe juice, 40mL/L of penetrant JFC3g/L, 5g/L of borneol modified chitosan, 4g/L of silk fibroin and the balance of deionized water.
The aloe juice is obtained by the following method: cleaning fresh aloe, air drying until no moisture exists on the surface, cutting into 0.8cm thick slices, wrapping with gauze, squeezing at 2000 rpm for 30 min under sealed environment, and collecting juice; heating the obtained juice to 110 deg.C at 2 deg.C/min, maintaining the temperature for 50 min, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
The preparation process of the borneol modified chitosan comprises the following steps:
(1) uniformly mixing 0.3g of glycol chitosan and 30mL of distilled water, and performing ultrasonic treatment until the glycol chitosan is completely dissolved in the water to obtain a glycol chitosan solution; carrying out vacuum freeze drying on the glycol chitosan solution, and removing water to obtain a glycol chitosan freeze-dried substance;
(2) putting 0.5g of p-aldehyde benzoic acid into a reaction device, adding 30mL of tetrahydrofuran, introducing nitrogen for protection, adding 0.08g of 4-dimethylaminopyridine and 1.7g of dicyclohexylcarbodiimide as catalysts, finally adding 1.0g of borneol, stirring at room temperature for 3 days after ice bath for 40 minutes, and collecting a reaction product; vacuum drying the reaction mixed product at 50 ℃ and 0.06MPa absolute pressure for 4 hours to obtain a crude product; the crude product was purified using petroleum ether: ethyl acetate volume ratio 10: 1 as eluent to carry out column chromatography separation, and collecting eluent; vacuum drying the eluate at 50 deg.C under 0.06MPa to constant weight to obtain bornyl benzoate p-aldehyde;
(3) dissolving 0.02g of bornyl p-aldehyde benzoate in 2mL of ethanol to obtain a bornyl p-aldehyde benzoate solution; adding the p-aldehyde bornyl benzoate solution into the freeze-dried glycol chitosan obtained in the step (1), and standing at room temperature for reaction for 12 hours; centrifuging at 4000 rpm for 25 minutes, and collecting a reaction product; and (3) cleaning the reaction product with ethanol, and drying the reaction product at 50 ℃ under the absolute pressure of 0.06MPa in vacuum to constant weight to obtain the borneol modified chitosan.
Example 8
The preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of glycidyl methacrylate on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: placing 10g/mL of the mixture in absolute ethyl alcohol, ultrasonically cleaning the mixture for 1 hour, and drying the mixture at 50 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a cavity of a DT-03 type plasma processor, and setting the power to be 150W; setting the oxygen flow rate to be 300sccm, carrying out plasma treatment in an oxygen atmosphere for 90 seconds, and placing in the air for 10 minutes after the treatment to obtain the polypropylene non-woven fabric subjected to plasma treatment; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: 20g/mL of the solution is put into glycidyl methacrylate aqueous solution with the mass fraction of 10 percent, and the grafting reaction is carried out for 8 minutes under the irradiation of 500W of ultraviolet power; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in acetone for 12 hours, and drying at 50 ℃ to constant weight to obtain the polypropylene non-woven fabric grafted with glycidyl methacrylate;
(2) fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate: placing the polypropylene non-woven fabric grafted with glycidyl methacrylate into a container, wherein the solid-liquid ratio is 1: putting 25g/mL of the mixed solvent into a mixed solvent, wherein the mixed solvent is prepared by mixing methanol and n-octylamine glucitol according to a volume ratio of 20: 1, stirring at 80 rpm, and carrying out reflux reaction at 70 ℃ for 72 hours; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in absolute ethyl alcohol for 12 hours, and drying at 50 ℃ to constant weight to obtain polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: 20g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3 minutes, and the soaking and rolling are carried out once, wherein the rolling residual rate is 70 percent; and baking the padded polypropylene non-woven fabric at 130 ℃ for 10 minutes to obtain the polypropylene non-woven fabric.
The antibacterial finishing liquid comprises the following components: 40mL/L of aloe juice, 40mL/L of penetrating agent JFC3g/L, 5g/L of borneol modified chitosan, 4g/L of wool keratin and the balance of deionized water.
The aloe juice is obtained by the following method: cleaning fresh aloe, air drying until no moisture exists on the surface, cutting into 0.8cm thick slices, wrapping with gauze, squeezing at 2000 rpm for 30 min under sealed environment, and collecting juice; heating the obtained juice to 110 deg.C at 2 deg.C/min, maintaining the temperature for 50 min, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
The preparation process of the borneol modified chitosan comprises the following steps:
(1) uniformly mixing 0.3g of glycol chitosan and 30mL of distilled water, and performing ultrasonic treatment until the glycol chitosan is completely dissolved in the water to obtain a glycol chitosan solution; carrying out vacuum freeze drying on the glycol chitosan solution, and removing water to obtain a glycol chitosan freeze-dried substance;
(2) putting 0.5g of p-aldehyde benzoic acid into a reaction device, adding 30mL of tetrahydrofuran, introducing nitrogen for protection, adding 0.08g of 4-dimethylaminopyridine and 1.7g of dicyclohexylcarbodiimide as catalysts, finally adding 1.0g of borneol, stirring at room temperature for 3 days after ice bath for 40 minutes, and collecting a reaction product; vacuum drying the reaction mixed product at 50 ℃ and 0.06MPa absolute pressure for 4 hours to obtain a crude product; the crude product was purified using petroleum ether: ethyl acetate volume ratio 10: 1 as eluent to carry out column chromatography separation, and collecting eluent; vacuum drying the eluate at 50 deg.C under 0.06MPa to constant weight to obtain bornyl benzoate p-aldehyde;
(3) dissolving 0.02g of bornyl p-aldehyde benzoate in 2mL of ethanol to obtain a bornyl p-aldehyde benzoate solution; adding the p-aldehyde bornyl benzoate solution into the freeze-dried glycol chitosan obtained in the step (1), and standing at room temperature for reaction for 12 hours; centrifuging at 4000 rpm for 25 minutes, and collecting a reaction product; and (3) cleaning the reaction product with ethanol, and drying the reaction product at 50 ℃ under the absolute pressure of 0.06MPa in vacuum to constant weight to obtain the borneol modified chitosan.
Example 9
The preparation method of the durable antibacterial polypropylene non-woven fabric comprises the following steps:
(1) graft copolymerization of glycidyl methacrylate on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: placing 10g/mL of the mixture in absolute ethyl alcohol, ultrasonically cleaning the mixture for 1 hour, and drying the mixture at 50 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a cavity of a DT-03 type plasma processor, and setting the power to be 150W; setting the oxygen flow rate to be 300sccm, carrying out plasma treatment in an oxygen atmosphere for 90 seconds, and placing in the air for 10 minutes after the treatment to obtain the polypropylene non-woven fabric subjected to plasma treatment; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: 20g/mL of the solution is put into glycidyl methacrylate aqueous solution with the mass fraction of 10 percent, and the grafting reaction is carried out for 8 minutes under the irradiation of 500W of ultraviolet power; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in acetone for 12 hours, and drying at 50 ℃ to constant weight to obtain the polypropylene non-woven fabric grafted with glycidyl methacrylate;
(2) fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate: placing the polypropylene non-woven fabric grafted with glycidyl methacrylate into a container, wherein the solid-liquid ratio is 1: putting 25g/mL of the mixed solvent into a mixed solvent, wherein the mixed solvent is prepared by mixing methanol and n-octylamine glucitol according to a volume ratio of 20: 1, stirring at 80 rpm, and carrying out reflux reaction at 70 ℃ for 72 hours; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: washing 10g/mL in absolute ethyl alcohol for 12 hours, and drying at 50 ℃ to constant weight to obtain polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: 20g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3 minutes, and the soaking and rolling are carried out once, wherein the rolling residual rate is 70 percent; and baking the padded polypropylene non-woven fabric at 130 ℃ for 10 minutes to obtain the polypropylene non-woven fabric.
The antibacterial finishing liquid comprises the following components: 40mL/L of aloe juice, 40mL/L of penetrant JFC3g/L, 5g/L of borneol modified chitosan, 4g/L of protein and the balance of deionized water.
The protein is silk fibroin and wool keratin in a mass ratio of 1: 1, in a mixture of the components.
The aloe juice is obtained by the following method: cleaning fresh aloe, air drying until no moisture exists on the surface, cutting into 0.8cm thick slices, wrapping with gauze, squeezing at 2000 rpm for 30 min under sealed environment, and collecting juice; heating the obtained juice to 110 deg.C at 2 deg.C/min, maintaining the temperature for 50 min, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
The preparation process of the borneol modified chitosan comprises the following steps:
(1) uniformly mixing 0.3g of glycol chitosan and 30mL of distilled water, and performing ultrasonic treatment until the glycol chitosan is completely dissolved in the water to obtain a glycol chitosan solution; carrying out vacuum freeze drying on the glycol chitosan solution, and removing water to obtain a glycol chitosan freeze-dried substance;
(2) putting 0.5g of p-aldehyde benzoic acid into a reaction device, adding 30mL of tetrahydrofuran, introducing nitrogen for protection, adding 0.08g of 4-dimethylaminopyridine and 1.7g of dicyclohexylcarbodiimide as catalysts, finally adding 1.0g of borneol, stirring at room temperature for 3 days after ice bath for 40 minutes, and collecting a reaction product; vacuum drying the reaction mixed product at 50 ℃ and 0.06MPa absolute pressure for 4 hours to obtain a crude product; the crude product was purified using petroleum ether: ethyl acetate volume ratio 10: 1 as eluent to carry out column chromatography separation, and collecting eluent; vacuum drying the eluate at 50 deg.C under 0.06MPa to constant weight to obtain bornyl benzoate p-aldehyde;
(3) dissolving 0.02g of bornyl p-aldehyde benzoate in 2mL of ethanol to obtain a bornyl p-aldehyde benzoate solution; adding the p-aldehyde bornyl benzoate solution into the freeze-dried glycol chitosan obtained in the step (1), and standing at room temperature for reaction for 12 hours; centrifuging at 4000 rpm for 25 minutes, and collecting a reaction product; and (3) cleaning the reaction product with ethanol, and drying the reaction product at 50 ℃ under the absolute pressure of 0.06MPa in vacuum to constant weight to obtain the borneol modified chitosan.
Test example 2
2.1 test piece wettability test
The wetting state of a non-woven fabric sample is tested by referring to GB/T22799 and 2009 method for testing the water absorption of towel products, and the wetting state is used for evaluating the surface wetting performance of the sample; the experiment was timed from the sample introduction and the time required for the complete wetting of the sample (the entire sample was covered with water) was recorded.
2.1 testing of the Electrostatic Properties of the samples
The electrostatic performance of the non-woven fabric sample is tested by adopting an FY342E fabric induction type electrostatic instrument under the following test conditions: the pressurizing voltage is 10000V, the pressurizing time is 30s, the attenuation rate is 50%, the time length used when the induction voltage is attenuated to a half is recorded, and the longest attenuation recording time of the device is 99 s. Each sample was tested 3 times and the average was taken.
2.3 testing of breaking Strength of cloth samples
According to GB/T3923.1-2013 part I of tensile property of textile fabrics: determination of breaking strength and breaking elongation (bar method) the breaking strength of different non-woven fabric samples was tested, and the average value was taken 3 times for each sample.
2.4 antimicrobial Property test
Staphylococcus aureus and Escherichia coli are selected as experimental strains, and according to the national standard GB/T20944.1-2007 evaluation part 1 of antibacterial performance of textiles: agar plate diffusion method, to the arrangement of cloth sample antibacterial performance test, using vernier caliper to measure the cloth sample around the diameter of the inhibition zone, all test samples all prepared into diameter 8mm round piece. D ═ D (D)1-d0)/2，
In the formula, D is the width of the bacteriostatic band; d1And d0Respectively, the outer diameter of the zone and the diameter of the test specimen.
The specific test results are shown in table 2.
TABLE 2 wettability, antistatic property, breaking strength and antibacterial property test table
Figure BDA0002297267150000191
From table 2 the following conclusions can be drawn:
1. the examples 2 to 3 further shorten the complete wetting time of the polypropylene nonwoven fabric sample compared with the comparative examples 1 to 3, which shows that the polypropylene nonwoven fabric with the fixed alkylamino glucitol contains a certain proportion of hydrophilic groups, so that the surface of the sample has a certain hydrophilicity, and the surface tension can be reduced, and the wetting time of the cloth sample can be shortened.
2. The shorter the half-life time, the better the antistatic properties. The polypropylene non-woven fabrics obtained in the embodiments 2 to 3 have not only antibacterial performance but also certain antistatic performance, which indicates that the polypropylene non-woven fabrics for fixing the alkylamino glucitol have certain proportion of polar groups and certain hydrophilic performance, so that static electricity on the surfaces of the polypropylene non-woven fabrics can be timely discharged.
3. The polypropylene nonwoven fabric sample has antibacterial properties against escherichia coli. Example 7 the chitosan modified by borneol is endowed with hydrophilicity while the wettability is ensured, and the antibacterial ability of the chitosan can be enhanced by the introduction of the traditional Chinese medicine, namely small molecular borneol.
It should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art will be able to make the description as a whole, and the embodiments may be appropriately combined to form other embodiments as will be appreciated by those skilled in the art.

Claims (9)

1. The preparation method of the lasting antibacterial polypropylene non-woven fabric is characterized by comprising the following steps:
(1) graft copolymerization of glycidyl methacrylate or acrylic acid on polypropylene nonwoven: carrying out plasma treatment on the surface of the polypropylene non-woven fabric to generate polar groups on the surface, and then initiating glycidyl methacrylate or acrylic acid graft copolymerization on the polypropylene non-woven fabric by utilizing ultraviolet irradiation to obtain the polypropylene non-woven fabric grafted with glycidyl methacrylate or acrylic acid;
(2) fixing alkylamino glucitol on the surface of polypropylene non-woven fabric grafted with glycidyl methacrylate or acrylic acid: fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate or acrylic acid to obtain the polypropylene non-woven fabric with the alkylamino glucitol fixed on the surface;
(3) dipping and finishing: and (3) soaking the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol in the antibacterial finishing liquid, and baking the soaked fabric sample by adopting a one-soaking one-rolling process.
2. The method for preparing a durable antibacterial polypropylene non-woven fabric according to claim 1, characterized by comprising the steps of:
(1) graft copolymerization of glycidyl methacrylate on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: (10-30) placing the obtained product in absolute ethyl alcohol for ultrasonic cleaning for 1-2 hours, and drying the product at 50-60 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a chamber of a plasma processor, and setting the power to be 150-300W; setting the oxygen flow rate to be 40-300 sccm, carrying out plasma treatment in an oxygen atmosphere for 60-120 seconds, and placing in the air for 10-20 minutes after the treatment to obtain a polypropylene non-woven fabric subjected to plasma treatment; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: (10-30) g/mL of the solution is put into a glycidyl methacrylate aqueous solution with the mass fraction of 5-10%, and the grafting reaction is performed for 6-15 minutes under the ultraviolet power of 300-500W; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) g/mL of the solution is placed in acetone to be washed for 12-24 hours, and the solution is dried at the temperature of 50-60 ℃ to constant weight, so that the polypropylene non-woven fabric grafted with the glycidyl methacrylate is obtained;
(2) fixing alkylamino glucitol on the surface of the polypropylene non-woven fabric grafted with glycidyl methacrylate: placing the polypropylene non-woven fabric grafted with glycidyl methacrylate into a container, wherein the solid-liquid ratio is 1: (20-40) g/mL is put into a mixed solvent, and the mixed solvent is prepared from methanol and alkylamino glucitol according to the volume ratio of (15-20): 1, carrying out reflux reaction for 36-72 hours at 70-80 ℃ under stirring at 50-130 r/min; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) washing the obtained product in absolute ethyl alcohol for 12-24 hours at a concentration of g/mL, and drying the washed product at a temperature of 50-60 ℃ to constant weight to obtain a polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: (10-25) g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3-5 minutes, one soaking and one rolling are carried out, and the rolling residue rate is 70-80%; and baking the padded polypropylene non-woven fabric at 130-140 ℃ for 2-10 minutes to obtain the polypropylene non-woven fabric.
3. The method for preparing a durable antibacterial polypropylene non-woven fabric according to claim 1, characterized by comprising the steps of:
(1) graft copolymerization of acrylic acid on polypropylene nonwoven: firstly, polypropylene non-woven fabric is mixed according to the solid-liquid ratio of 1: (10-30) placing the obtained product in absolute ethyl alcohol for ultrasonic cleaning for 1-2 hours, and drying the product at 50-60 ℃ to constant weight to obtain a clean polypropylene non-woven fabric; putting the cleaned polypropylene non-woven fabric into a chamber of a plasma processor, and setting the power to be 150-300W; setting the oxygen flow rate to be 40-300 sccm, carrying out plasma treatment in an oxygen atmosphere for 60-120 seconds, and placing in the air for 10-20 minutes after the treatment to obtain a polypropylene non-woven fabric subjected to plasma treatment; butanone is adopted as the raw material: ethanol: the volume ratio of water is (5-10): (5-10): (80-90) preparing an acrylic acid solution with the mass fraction of 5-10% by taking the mixed solution as a solvent; and (3) treating the polypropylene non-woven fabric subjected to plasma treatment in a solid-to-liquid ratio of 1: (10-30) g/mL of the solution is put into an acrylic acid solution, and the grafting reaction is performed for 6-15 minutes under the ultraviolet power of 300-500W; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) g/mL of the acrylic acid grafted polypropylene non-woven fabric is placed in acetone to be washed for 12-24 hours, and dried at 50-60 ℃ to constant weight to obtain acrylic acid grafted polypropylene non-woven fabric;
(2) fixing alkylamino glucitol on the surface of the acrylic acid grafted polypropylene non-woven fabric: placing the acrylic acid grafted polypropylene non-woven fabric into a container, wherein the solid-liquid ratio is 1: (20-40) g/mL is put into a mixed solvent, and the mixed solvent is prepared from methanol and alkylamino glucitol according to the volume ratio of (15-20): 1, reacting for 8-12 hours at 60-80 ℃ under stirring at 50-130 r/min; after the reaction is finished, taking out the polypropylene non-woven fabric, and mixing the polypropylene non-woven fabric according to a solid-liquid ratio of 1: (10-20) washing the obtained product in absolute ethyl alcohol for 12-24 hours at a concentration of g/mL, and drying the washed product at a temperature of 50-60 ℃ to constant weight to obtain a polypropylene non-woven fabric with the surface fixed with alkylamino glucitol;
(3) dipping and finishing: and (2) fixing the polypropylene non-woven fabric with the surface fixed with the alkylamino glucitol by a solid-liquid ratio of 1: (10-25) g/mL of the antibacterial finishing liquid is soaked in the antibacterial finishing liquid for 3-5 minutes, one soaking and one rolling are carried out, and the rolling residue rate is 70-80%; and baking the padded polypropylene non-woven fabric at 130-140 ℃ for 2-10 minutes to obtain the polypropylene non-woven fabric.
4. The preparation method of the lasting antibacterial polypropylene non-woven fabric according to any one of claims 1 to 3, wherein the alkylamino glucitol is one or a mixture of n-butyl amino glucitol, n-octyl amino glucitol and dodecyl amino glucitol.
5. The method for preparing a durable antibacterial polypropylene non-woven fabric according to claim 2 or 3, wherein the antibacterial finishing liquid comprises the following components: 30-100 mL/L of aloe juice, 1-3 g/L of penetrant JFC, 5-10 g/L of chitosan or borneol modified chitosan, 2-4 g/L of protein and the balance of water.
6. The method for preparing a long-lasting antibacterial polypropylene nonwoven fabric according to claim 5, wherein the aloe vera juice is obtained by: cleaning fresh aloe, drying in the air until the surface has no moisture, cutting into pieces with the thickness of 0.5-1 cm, wrapping with gauze, and squeezing under a sealed environment for 20-40 minutes to obtain juice; heating the obtained juice to 100-120 ℃, preserving the heat for 50-80 minutes, removing surface ash juice, and naturally cooling to room temperature to obtain the aloe juice.
7. The method for preparing the durable antibacterial polypropylene non-woven fabric according to claim 5, wherein the preparation process of the borneol modified chitosan is as follows:
(1) uniformly mixing 0.2-0.4 g of glycol chitosan and 25-35 mL of water, and carrying out ultrasonic treatment until the glycol chitosan is completely dissolved in the water to obtain a glycol chitosan solution; carrying out vacuum freeze drying on the glycol chitosan solution, and removing water to obtain a glycol chitosan freeze-dried substance;
(2) putting 0.4-0.7 g of p-aldehyde benzoic acid into a reaction device, adding 25-35 mL of tetrahydrofuran, introducing nitrogen for protection, adding 0.05-0.1 g of 4-dimethylaminopyridine and 1.5-2 g of dicyclohexylcarbodiimide as catalysts, finally adding 1-2 g of borneol, carrying out ice bath for 30-40 minutes, stirring at room temperature for 3-5 days, and collecting a reaction product; vacuum drying the reaction mixed product at 50-60 ℃ for 3-6 hours to obtain a crude product; the crude product was purified using petroleum ether: ethyl acetate volume ratio (10-20): 1 as eluent to carry out column chromatography separation, and collecting eluent; drying the eluent in vacuum at 50-60 ℃ to constant weight to obtain the para-aldehyde bornyl benzoate;
(3) dissolving 0.01-0.03 g of para-aldehyde bornyl benzoate in 2-4 mL of absolute ethanol to obtain a para-aldehyde bornyl benzoate solution; adding the p-aldehyde bornyl benzoate solution into the freeze-dried glycol chitosan obtained in the step (1), and standing at room temperature for 10-15 hours; centrifuging at 3000-4000 rpm for 20-30 minutes, and collecting reaction products; and cleaning the reaction product with ethanol, and drying at 50-60 ℃ in vacuum to constant weight to obtain the borneol modified chitosan.
8. The method for preparing a durable antibacterial polypropylene non-woven fabric according to claim 5, wherein the protein is silk fibroin and/or wool keratin.
9. The durable antibacterial polypropylene non-woven fabric is characterized by being processed by the preparation method of the durable antibacterial polypropylene non-woven fabric according to any one of claims 1 to 8.
CN201911207640.9A 2019-11-29 2019-11-29 Lasting antibacterial polypropylene non-woven fabric and preparation method thereof Pending CN111041828A (en)

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