CN114032625B - Antibacterial material and application thereof in preparing adult menstrual period pants - Google Patents

Antibacterial material and application thereof in preparing adult menstrual period pants Download PDF

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CN114032625B
CN114032625B CN202111280808.6A CN202111280808A CN114032625B CN 114032625 B CN114032625 B CN 114032625B CN 202111280808 A CN202111280808 A CN 202111280808A CN 114032625 B CN114032625 B CN 114032625B
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antibacterial material
polyamide fiber
drying
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antibacterial
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CN114032625A (en
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吴跃
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Qianzhiya Hubei Sanitary Products Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/90Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A01N25/10Macromolecular compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00Bandages or dressings; Absorbent pads
    • A61F13/15Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F13/45Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the shape
    • A61F13/49Absorbent articles specially adapted to be worn around the waist, e.g. diapers
    • A61F13/496Absorbent articles specially adapted to be worn around the waist, e.g. diapers in the form of pants or briefs
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides

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Abstract

The invention discloses an antibacterial material and application thereof in preparing adult menstrual pants; belonging to the field of sanitary materials; an antibacterial material which is a modified polyamide fiber; the modified polyamide fiber is grafted with apiose isoliquiritin; the air permeability of the antibacterial material is higher than 550mm/s; the method comprises the following steps: washing polyamide fiber with water, and drying to obtain a pretreated fiber raw material; dissolving an initiator in a solvent, crystallizing, filtering, washing and drying to obtain a purified initiator; dissolving the purified initiator, and then adding apiose isoliquiritin to obtain a mixed solution; and soaking the pretreated fiber raw material in the mixed solution, taking out, drying, carrying out heat treatment, then soaking in an ethanol solution, washing and drying to obtain the modified polyamide fiber. The obtained antibacterial material has excellent antibacterial property, hygroscopicity and air permeability, is safe and nontoxic to human bodies, and has wide application in adult menstrual pants.

Description

Antibacterial material and application thereof in preparing adult menstrual pants
Technical Field
The invention belongs to the field of sanitary materials, and particularly relates to an antibacterial material and application thereof in preparing adult menstrual pants.
Background
Women are most vulnerable to bacterial attack during menstruation. During the period, the weak acid environment in the vagina is changed by the elimination of menstrual blood, so that conditions are created for the growth and the propagation of bacteria; due to the unique physiological structure of women, the sanitary towel can shift during the use process, and bacteria or other harmful substances in the waste discharged by excretory organs are easily transmitted to reproductive organs; meanwhile, after bacteria in human bodies are discharged out of the human bodies, if a warm and humid environment rich in nutrition is met, a large amount of bacteria can propagate, and the sanitary towel in the use state just meets the conditions and becomes a hotbed for the bacteria. The research shows that after the common sanitary towel is continuously used for two hours, the surface layer bacteria are always
Infant's panty-shape diapers of selling on the existing market, the pull-up diaper, disposable hygienic products such as sanitary towel for women adopt multilayer structure such as top layer non-woven fabrics combines inside absorbent resin layer, bottom leak protection layer more, wherein the non-woven fabrics is as the top layer with human skin direct contact, require it can lead into inside absorbent resin layer with the urine fast when the urine takes place suddenly, do not remain liquid, the urine does not return and oozes when the activity receives human pressure, keep the surface dry and comfortable, create comfortable good "microclimate" environment for human skin.
Disclosure of Invention
The invention aims to provide an antibacterial material with excellent antibacterial property, hygroscopicity and air permeability, is safe and nontoxic to a human body, and has wide application in adult menstrual pants.
The technical scheme adopted by the invention for realizing the purpose is as follows:
an antibacterial material which is a modified polyamide fiber; the modified polyamide fiber is grafted with apiose isoliquiritin;
the grafting rate of the modified polyamide fiber is 14.62 to 19.57wt%;
the air permeability of the antibacterial material is higher than 545mm/s.
According to the invention, the polyamide fiber is grafted and modified by the apiose isoliquiritin to obtain the antibacterial material, so that the antibacterial performance of the antibacterial material is obviously improved; meanwhile, the antibacterial material can quickly transfer liquid substances and has excellent moisture absorption performance; in addition, the antibacterial material has excellent air permeability, safety and no toxicity, so that the antibacterial material has better use comfort and safety, and can be widely applied to adult menstrual trousers.
The invention also discloses application of the modified polyamide fiber in improving antibacterial property and/or hygroscopicity and/or air permeability of the antibacterial material.
The invention also discloses a preparation method of the antibacterial material, and the prepared antibacterial material has excellent antibacterial, moisture absorption and air permeability performances.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation method of an antibacterial material comprises the following steps:
providing a fiber raw material, washing polyamide fiber with water, and drying to obtain a pretreated fiber raw material;
providing an initiator, dissolving the initiator in a solvent, filtering to remove insoluble impurities, dripping filtrate into methanol with the same volume for crystallization, filtering, washing and drying to obtain a purified initiator;
dissolving the purified initiator, and then adding apiose isoliquiritin to obtain a mixed solution; and soaking the pretreated fiber raw material in the mixed solution, taking out, drying, performing heat treatment, after the reaction is finished, soaking in an ethanol solution, washing, and drying to obtain the modified polyamide fiber.
Preferably, the concentration of the purified initiator is 0.15 to 0.35wt%, and the concentration of the apigenin is 1.5 to 4.5wt%, so that the apigenin is better combined on the surface of the polyamide fiber.
Preferably, the heat temperature is 65 to 85 ℃, and the processing time is 20 to 30min.
Preferably, the preparation method of the antibacterial material further comprises: and (3) soaking the modified polyamide fiber in finishing liquid containing a modified silane coupling agent, taking out, heating, washing and drying to obtain the antibacterial material.
More preferably, the soaking treatment time is 25 to 45min; the heating temperature is 75 to 100 ℃, and the heating time is 1 to 2h.
More preferably, the modified silane coupling agent is N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide modified triisopropoxysilane. The modified silane coupling agent contains more active groups, and can be physically and chemically combined with the active groups in the modified polyamide fiber to obtain an antibacterial material with better hygroscopicity and air permeability, and better safety to human bodies.
More preferably, the content of the modified silane coupling agent in the finishing liquid is 7.5 to 10.5vol%.
The invention also discloses application of the antibacterial material in preparing adult menstrual pants.
According to the invention, the polyamide fiber is grafted and modified by the apiose isoliquiritin to obtain the antibacterial material, so that the antibacterial performance of the antibacterial material is obviously improved; meanwhile, the antibacterial material can quickly transfer liquid substances and has excellent moisture absorption performance; in addition, the antibacterial material has excellent air permeability, safety and nontoxicity, so that the antibacterial material has better use comfort and safety, and can be widely applied to adult menstrual pants. Therefore, the invention is an antibacterial material with excellent antibacterial property, hygroscopicity and air permeability, is safe and nontoxic to human bodies, and has wide application in adult menstrual pants.
Drawings
FIG. 1 is an infrared spectrum before and after the modification of triisopropoxysilane in example 1.
Detailed Description
To further illustrate the present invention, the following detailed description of the antibacterial material provided by the present invention is made with reference to the following examples, but it should be understood that these examples are carried out under the premise of the technical solution of the present invention, and the detailed embodiments and the specific operation procedures are given for further illustrating the features and advantages of the present invention, not for limiting the claims of the present invention, and the scope of the present invention is not limited to the following examples.
In some embodiments of the present invention, a method of preparing an antimicrobial material comprises the steps of:
providing a fiber raw material, fully washing polyamide fiber with clear water, and drying to constant weight to obtain a pretreated fiber raw material;
providing an initiator, dissolving 4.5 to 7.5 parts by weight of the initiator in 20 to 30 parts by weight of a solvent, filtering to remove insoluble impurities, dripping filtrate into methanol with the same volume for crystallization, filtering, washing crystals with cold methanol, and drying in vacuum at room temperature to obtain a purified initiator;
dissolving the purified initiator in 45 to 55 parts of ethanol solution with the concentration of 60 to 80vol% to ensure that the concentration of the initiator is 0.15 to 0.35wt%, and then adding apioside to obtain a mixed solution, wherein the concentration of the apioside is 1.5 to 4.5wt%; soaking 2.5 to 5.5 parts of pretreated fiber raw material in the mixed solution for 20 to 30min, taking out, drying at 35 to 45 ℃ for 25 to 35min, then carrying out heat treatment at 65 to 85 ℃ for 20 to 30min, after the reaction is finished, soaking in an ethanol solution with the volume fraction of 50 to 60% for 25 to 45min to remove substances remaining on the surface and not completely reacted, then washing with a large amount of pure water to remove the residual ethanol, and drying at 35 to 45 ℃ to constant weight to obtain the modified polyamide fiber, wherein the grafting ratio is 14.62 to 19.57wt%, namely the antibacterial material.
Further, in some embodiments of the present invention, the solvent used in the solution is one of ethanol, methanol, and acetone.
Further optimally, in some embodiments of the invention, the preparation method of the antibacterial material further comprises the following steps: and (2) soaking the prepared modified polyamide fiber in a finishing liquid containing 7.5 to 10.5vol% of a modified silane coupling agent for 25 to 45min, taking out, heating to 75 to 100 ℃, washing for 1 to 2h, washing for 3 to 5 times with clear water, and drying for 25 to 45min at 55 to 65 ℃ to obtain the antibacterial material.
Further, in some embodiments of the present invention, the modified silane coupling agent is prepared by: adding 4.5 to 7.5 parts by weight of N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide into a reaction vessel, reacting in a nitrogen atmosphere, adding 160 to 180 parts by weight of toluene as a solvent, raising the reaction temperature to 50 to 55 ℃, adding 0.15 to 0.25 part by weight of karstedt catalyst, and continuously stirring for 40 to 60min to activate the catalyst; and then slowly dripping 2.5 to 3.2 parts of triisopropoxysilane into the solution, heating to 65 to 75 ℃ after dripping is finished, reacting for 1 to 3 days, filtering to remove impurities in the liquid by suction while the liquid is hot, cooling to room temperature, removing the solvent by rotary evaporation, and recrystallizing to obtain the modified silane coupling agent.
The antibacterial material is prepared into adult menstrual period pants according to a conventional technical scheme.
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
example 1:
a preparation method of an antibacterial material comprises the following steps:
providing a fiber raw material, fully washing polyamide fiber (purchased from Qiongxin Tianding materials science and technology Co., ltd.) with clear water, and drying to constant weight to obtain a pretreated fiber raw material;
providing an initiator, dissolving 5.5 parts by weight of dibenzoyl peroxide (BPO) in 25 parts by weight of chloroform, filtering to remove insoluble impurities, dripping filtrate into methanol with the same volume for crystallization, filtering, washing crystals with cold methanol, and drying in vacuum at room temperature to obtain a purified initiator;
dissolving the purified initiator in 50 parts of 75vol% ethanol solution to make the initiator concentration 0.25wt%, and adding apioside to obtain a mixed solution, wherein the apioside isoliquiritin concentration is 3.5 wt%; soaking 4.5 parts of the pretreated fiber raw material in the mixed solution for 25min, taking out, drying for 30min at 40 ℃, then carrying out heat treatment for 25min at 75 ℃, after the reaction is finished, soaking in an ethanol solution with the volume fraction of 50% for 35min to remove residual unreacted substances on the surface, then washing with a large amount of pure water to remove residual ethanol, and drying at 40 ℃ to constant weight to obtain the modified polyamide fiber, wherein the grafting ratio is 17.82wt%, namely the antibacterial material.
Example 2:
unlike example 1, the method for preparing an antibacterial material was such that the purified initiator was dissolved in 50 parts of 75vol% ethanol solution to give an initiator concentration of 0.35wt%, and the graft ratio of the resulting modified polyamide fiber was 18.61wt%.
Example 3:
a method for preparing an antibacterial material, which is different from example 1, the above-mentioned purified initiator was dissolved in 50 parts of 75vol% ethanol solution so that the concentration of the initiator was 0.25wt%, and then apioside isoliquiritin, in which the concentration of apioside isoliquiritin was 4.5wt%, was added to obtain a mixed solution, and the grafting ratio of the modified polyamide fiber was 19.43wt%.
Example 4:
further optimally, the preparation method of the antibacterial material further comprises the following steps: the modified polyamide fiber in example 1 was immersed in a finishing solution containing 7.5vol% of a modified silane coupling agent for 30min, taken out, heated to 90 ℃ for 1h, washed with clean water for 3 times, and dried at 55 ℃ for 25min to obtain an antibacterial material.
In this embodiment, the preparation method of the modified silane coupling agent comprises: adding 4.5 parts by weight of N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide into a reaction vessel, reacting under a nitrogen atmosphere, adding 160 parts by weight of toluene as a solvent, raising the reaction temperature to 50 ℃, adding 0.15 part by weight of karstedt catalyst, and continuing stirring for 45min to activate the catalyst; and then slowly dropwise adding 3.2 parts of triisopropoxysilane into the solution, heating to 70 ℃ after the dropwise adding is finished, reacting for 1 day, filtering off impurities in the liquid by suction while the liquid is hot, cooling to room temperature, removing the solvent by rotary evaporation, and recrystallizing to obtain the modified silane coupling agent.
Example 5:
a method for preparing an antibacterial material, which is different from that of example 4 in that the modified polyamide fiber of example 1 is replaced with the modified polyamide fiber of example 2.
Example 6:
a method for preparing an antibacterial material, which is different from that of example 4 in that the modified polyamide fiber of example 1 is replaced with the modified polyamide fiber of example 3.
Example 7:
different from the preparation method of the embodiment 4, the modified polyamide fiber in the embodiment 1 is placed in finishing liquid containing 8.5vol% of modified silane coupling agent to be soaked for 30min, and finally the antibacterial material is obtained.
Example 8:
different from the preparation method of the embodiment 4, the modified polyamide fiber in the embodiment 1 is placed in finishing liquid containing 10.5vol% of modified silane coupling agent to be soaked for 30min, and finally the antibacterial material is obtained.
Example 9:
a method of preparing an antimicrobial material, which differs from example 4 in that the modified polyamide fiber of example 1 is replaced with an unmodified polyamide fiber (available from kinson tianding materials science and technology limited).
Example 10:
different from the embodiment 4, the modified polyamide fiber in the embodiment 1 is placed in a finishing liquid containing 7.5vol% of triisopropoxysilane for soaking treatment for 30min, and finally the antibacterial material is obtained.
Comparative example 1:
untreated polyamide fiber (available from Xin, N.Y. material science and technology Co., ltd., in Qidong) was used as comparative example 1.
Test example 1:
infrared spectroscopic determination of modified silane coupling agent
The infrared spectrogram of a sample is measured by a Bruker Vertex70 Fourier infrared spectrometer, and the scanning range is 4000-400cm -1
FIG. 1 is an infrared spectrum before and after the modification of triisopropoxysilane in example 1. As can be seen from FIG. 1, the modified silane coupling agent has an IR spectrum at 3643cm, relative to the IR spectrum of the unmodified triisopropoxysilane -1 A stretching vibration peak of-OH appears nearby; at 3458cm -1 An N-H stretching vibration peak appears nearby; at 1676cm -1 A stretching vibration peak of C = O appears nearby; thus, N- [2- (3, 4-dihydroxyphenyl) ethyl ] is used]And (4) modifying triisopropoxysilane by-2-acrylamide to obtain the modified silane coupling agent.
Test example 2:
1. determination of antibacterial Properties of antibacterial Material
Taking the concentration of 5.6 multiplied by 10 5 cfu/mL bacteria (Staphylococcus epidermidis, escherichia coli), suspension 100 mL (bacteria final concentration of 5.6X 10) 4 cfu/mL), uniformly smearing on the surface of a culture dish with the diameter of 95mm and containing nutrient agar, respectively taking sample pieces of the antibacterial material, pasting the sample pieces on the culture dish in an aseptic state, placing the sample pieces in a constant-temperature incubator at 37 ℃ for culturing for 24 hours, and then measuring the diameter (mm) of a bacteriostatic circle around the sample material by using a vernier caliper.
TABLE 1 antibacterial Ring diameter (mm) of antibacterial Material
Figure DEST_PATH_IMAGE002
As can be seen from table 1, in examples 1 to 3, the diameter of the inhibition zone of staphylococcus epidermidis is higher than 12.5mm, the diameter of the inhibition zone of escherichia coli is higher than 9.5mm, in comparative example 1, example 4 and example 9, the diameters of the inhibition zones of staphylococcus epidermidis and escherichia coli in example 1 are higher than that in comparative example 1, and the diameters of the inhibition zones of staphylococcus epidermidis and escherichia coli in example 4 are higher than that in example 9, which shows that the antibacterial material is obtained by graft modification of polyamide fiber by apiose isoliquiritin, and the antibacterial performance of the antibacterial material is remarkably improved; in example 4, the diameter of the inhibition zone of staphylococcus epidermidis is higher than 15.5mm, and the diameter of the inhibition zone of escherichia coli is higher than 14mm; comparing example 1 with example 4 and example 10, the diameter of the inhibition zone of staphylococcus epidermidis and escherichia coli in example 4 is higher than that of examples 1 and 10, which shows that the antibacterial material is obtained by further optimizing the soaking of the prepared modified polyamide fiber in finishing liquid containing modified silane coupling agent prepared by N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide and triisopropoxysilane, and the antibacterial performance of the antibacterial material is further improved; probably because the modified polyamide fiber and the modified silane coupling agent are crosslinked to obtain the antibacterial material containing more active groups, the antibacterial material has more excellent antibacterial performance.
2. Determination of moisture absorption Properties of antibacterial Material
According to a test method in GB/T21655.1-2008 'evaluation of moisture absorption quick drying of textiles', the wetting time, the water absorption rate and the liquid water transfer rate of a sample are respectively tested to represent the moisture absorption performance of the fabric; wherein the infiltration time is a time period when the upper surface and the lower surface of the antibacterial material are just infiltrated; water absorption rate reaction rate of the material to liquid water; liquid water transfer rate reflects the ability of the material to move liquid water outward in its plane, the higher its value, the stronger the material's ability to quickly absorb.
TABLE 2 moisture absorption Properties of antibacterial materials
Figure DEST_PATH_IMAGE004
As can be seen from Table 2, the soaking time was less than 12.5s and the water absorption rate was more than 33.5% s in examples 1 to 3 -1 Liquid water transfer rate higher than 13% s -1 Comparing example 1 with comparative example 1, and example 4 with example 9, the soaking time of example 1 is lower than that of comparative example 1, the water absorption rate and the liquid water transfer rate are higher than those of comparative example 1, the soaking time of example 4 is lower than that of example 9, and the water absorption rate and the liquid water transfer rate are higher than those of example 9, which shows that the antibacterial material is obtained by graft modification of polyamide fiber by apiose isoliquiritin, the moisture absorption performance of the antibacterial material is remarkably improved, and the antibacterial material can be rapidly liquid substance; in example 4, the soaking time is less than 10s, and the water absorption rate is higher than 38% s -1 Liquid water transfer rate higher than 15.8% s -1 (ii) a Comparing example 1 with example 4 and example 10, the wetting time of example 4 is lower than that of example 1 and example 10, and the water absorption rate and the liquid water transfer rate are higher than those of example 1 and example 10, which shows that the modified polyamide fiber obtained by soaking the modified polyamide fiber in the solution containing N- [2- (3, 4-dihydroxyphenyl) ethyl ] ethyl]The finishing liquid of the modified silane coupling agent prepared from the-2-acrylamide and the triisopropoxysilane is further optimized to obtain the antibacterial material, so that the moisture absorption performance of the antibacterial material is further improved, and the antibacterial material can be widely applied to the preparation of adult menstrual pants.
3. Determination of air permeability of antibacterial material
The air permeability R (mm/s) of the fabric was tested using a fabric air permeameter according to GB/T5453-1997 textile fabric air permeability test method. The test area is 5cm 2 The sample pressure difference was 100Pa.
TABLE 3 air permeability of antibacterial Material
Figure DEST_PATH_IMAGE006
As can be seen from table 3, the air permeability of examples 1 to 3 is higher than 545mm/s, comparative example 1, example 4 and example 9 compare example 1, example 1 has higher air permeability than comparative example 1, and example 4 has higher air permeability than example 9, which shows that the antibacterial material obtained by graft modification of polyamide fiber with apiose isoliquiritin significantly improves the air permeability of the antibacterial material, so that the antibacterial material has better air permeability and comfort; the air permeability of example 4 is higher than 582mm/s; comparing example 1 with example 4 and example 10, the air permeability of example 4 is higher than that of example 1 and example 10, which shows that the modified polyamide fiber obtained is soaked in the finishing liquid containing the modified silane coupling agent prepared by N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide and triisopropoxysilane for further optimization treatment to obtain the antibacterial material, and the air permeability of the antibacterial material is further improved; probably because the modified polyamide fiber and the modified silane coupling agent are crosslinked to obtain a better internal reticular structure, the antibacterial material has better air permeability.
4. Determination of cytotoxicity of antibacterial materials
Weighing an antibacterial material sample, placing the antibacterial material sample into a sterile test tube after autoclaving, then respectively adding RPMI1640 culture solution into the test tube to make the mass concentration of the sample reach 100g/L, and placing the test tube into a 37 ℃ incubator for leaching for 48 hours. Filtering with 0.22 μm microporous filter, loading into sterile test tube, making into leaching solution of antibacterial material sample, and storing in refrigerator at 4 deg.C. 2% calf serum RPMI1640 was used as negative control, 5% dimethylsulfoxide was used as positive control.
3mL of each of the experimental group, the negative control group (2% calf serum RPMI 1640) and the positive control group (5% dimethyl sulfoxide) were placed in 6-well cell culture dishes, and 4X 10 cells were added 4 3m 1/ml L-929 cell suspension, put at 5% CO 2 Culturing in an incubator at 37 deg.C and 100% humidity for 72h, and observing the form and growth of the experimental cells under an inverted microscope. The relative cell proliferation rate (RGR) and cytotoxicity of the material were determined by MTT colorimetry.
(1) At a concentration of 4X 10 4 The cell suspension was inoculated into 3 96-well plates at 200u1 per well, and cultured in an incubator containing 5% of C02 at 37 ℃ for 24 hours
(2) Discarding stock solution after observing cell adherence, washing with PBS for 2 times, discarding stock solution, adding leaching solution of antibacterial material sample, negative control group (2% calf serum RPMI 1640) and positive control group (5% dimethyl sulfoxide), repeating each extracting solution for 4 wells/plate at 200 μ L/well, and placing processed 96-well plate in 5% CO 2 、37℃After culturing in an incubator for 72h, the cell morphology and growth were observed.
(3) Discarding the stock culture solution at 72h, adding 20. Mu.L of MTT (mass concentration of 5 mg/mL), 5% 2 After incubation at 37 ℃ for 4h, the culture was terminated. After the supernatant was aspirated, 100. Mu.L of DMSO was added to each well, the mixture was shaken at 600r/min for 10min, and the absorbance (OD) was measured at 490nm with a microplate reader, and the results were recorded.
(4) Diluting the experimental leaching liquor with 2% calf serum RPMI1640 culture solution according to volume fractions of 75%, 50%, 25%, 10% and 1%, respectively, then taking 200 μ L of each dilution solution with various concentrations to repeat the above experiment, similarly taking 2% calf serum RPMI1640 as a negative control group and 5% dimethyl sulfoxide as a positive control group, measuring the relative proliferation rate (RGR) of L-929 cell culture for 72h by MTT colorimetry, and evaluating the cytotoxicity of the diluted material.
RGR = OD value of experimental group/OD value of negative control group
TABLE 4 cytotoxicity assessment ranking
Relative proliferation Rate (RGR%) Cytotoxicity grading (CTS) Evaluation of results
≥100 0 Has no cytotoxicity
75~99 Has no cytotoxicity
50~74 Mild cytotoxicity
25~49 Moderate cytotoxicity
1~24 Moderate cytotoxicity
0 Severe cytotoxicity
The results of the cytotoxicity test of the samples of the antibacterial material are shown in table 5.
TABLE 5 relative cell proliferation Rate and cytotoxicity ranking of antimicrobial materials
Test group RGR (%) Cytotoxicity grading
Example 1 101.2 0
Example 2 100.4 0
Example 3 102.1 0
Example 4 103.5 0
Example 9 95.1
Example 10 100.8 0
As can be seen from Table 5, the relative cell proliferation rate of examples 1-4 is higher than 100%, and the antibacterial material has no cytotoxicity, i.e., the obtained antibacterial material is nontoxic to human bodies and has better use safety; comparing example 4 with example 9, the relative cell proliferation rate of example 4 is higher than that of example 9, and the cytotoxicity grading is lower than that of example 9, which shows that the antibacterial material is obtained by grafting polyamide fiber with apiose isoliquiritin, and the use safety of the antibacterial material is improved; comparing example 1 with example 4 and example 10, the relative cell proliferation rate of example 4 is higher than that of example 1 and example 10, which shows that the prepared modified polyamide fiber is soaked in the finishing liquid containing the modified silane coupling agent prepared by N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide and triisopropoxysilane for further optimization treatment to obtain the antibacterial material, and the cell compatibility of the antibacterial material is further improved, so that the antibacterial material is safe and nontoxic to human body.
Although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention.

Claims (5)

1. An antibacterial material which is a modified polyamide fiber; the modified polyamide fiber is grafted with apiose isoliquiritin;
the grafting rate of the modified polyamide fiber is 14.62 to 19.57wt%;
the air permeability of the antibacterial material is higher than 545mm/s;
the preparation method of the antibacterial material comprises the following steps:
providing a fiber raw material, washing polyamide fiber with water, and drying to obtain a pretreated fiber raw material;
providing an initiator, dissolving the initiator in a solvent, filtering to remove insoluble impurities, dripping filtrate into methanol with the same volume for crystallization, filtering, washing and drying to obtain a purified initiator;
dissolving the purified initiator, and then adding apiose isoliquiritin to obtain a mixed solution; soaking the pretreated fiber raw material in the mixed solution, taking out, drying, then carrying out heat treatment, after the reaction is finished, soaking in an ethanol solution, washing, and drying to obtain modified polyamide fiber;
the concentration of the purified initiator is 0.15 to 0.35wt%, and the concentration of the apiose isoliquiritin is 1.5 to 4.5wt%;
the preparation method of the antibacterial material further comprises the following steps: placing the modified polyamide fiber into finishing liquid containing a modified silane coupling agent for soaking treatment, taking out, heating, washing and drying to obtain an antibacterial material, namely an antibacterial material;
the modified silane coupling agent is N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide modified triisopropoxysilane.
2. An antimicrobial material according to claim 1, wherein: the heat temperature is 65 to 85 ℃, and the processing time is 20 to 30min.
3. An antimicrobial material according to claim 1, wherein: the preparation method of the modified silane coupling agent comprises the following steps: adding 4.5 to 7.5 parts by weight of N- [2- (3, 4-dihydroxyphenyl) ethyl ] -2-acrylamide into a reaction vessel, reacting in a nitrogen atmosphere, adding 160 to 180 parts by weight of toluene as a solvent, heating the reaction temperature to 50 to 55 ℃, adding 0.15 to 0.25 part by weight of karstedt catalyst, and continuously stirring for 40 to 60min to activate the catalyst; and then slowly dripping 2.5 to 3.2 parts of triisopropoxysilane into the solution, heating to 65 to 75 ℃ after dripping is finished, reacting for 1 to 3 days, filtering to remove impurities in the liquid by suction while the liquid is hot, cooling to room temperature, removing the solvent by rotary evaporation, and recrystallizing to obtain the modified silane coupling agent.
4. An antimicrobial material according to claim 1, wherein: the content of the modified silane coupling agent in the finishing liquid is 7.5-10.5 vol%.
5. Use of an antimicrobial material according to claim 1 in the manufacture of adult menstrual pants.
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