CN112176728A - Antibacterial, antiviral and deodorant cotton fiber and preparation method and application thereof - Google Patents
Antibacterial, antiviral and deodorant cotton fiber and preparation method and application thereof Download PDFInfo
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- CN112176728A CN112176728A CN202010655482.XA CN202010655482A CN112176728A CN 112176728 A CN112176728 A CN 112176728A CN 202010655482 A CN202010655482 A CN 202010655482A CN 112176728 A CN112176728 A CN 112176728A
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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- D06M13/50—Treating 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
- D06M13/503—Treating 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 without bond between a carbon atom and a metal or a boron, silicon, selenium or tellurium atom
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- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Abstract
The invention belongs to the technical field of cotton fibers, and particularly relates to an antibacterial, antiviral and deodorant cotton fiber as well as a preparation method and application thereof. The fiber provided by the invention contains a plant natural antibacterial agent and a complex, the complex is a complex formed by metal ions contained in an inorganic antibacterial agent and phytic acid, and the cotton fiber has good antibacterial and antiviral properties under the combined action of the plant antibacterial agent and the complex; meanwhile, the beta-cyclodextrin effectively protects the natural plant antibacterial agent, and the phenomenon that the natural plant antibacterial agent is damaged or lost in the processing process is avoided; the phytic acid and metal ions in the inorganic antibacterial agent form complexation, so that the stability of the inorganic antibacterial agent is improved, the antibacterial and antiviral durability of the cotton fiber is further improved, and meanwhile, the flame retardance of the cotton fiber is also improved due to the introduction of the phytic acid; the beta-cyclodextrin and the cotton fiber generate graft crosslinking, so that the binding performance of the antibacterial agent and the cotton fiber is further improved, and the antibacterial and antiviral durability of the cotton fiber is improved.
Description
Technical Field
The invention belongs to the technical field of cotton fibers, and particularly relates to an antibacterial, antiviral and deodorant cotton fiber as well as a preparation method and application thereof.
Background
With the development of society, as the living standard of people is improved, more and more pathogenic microorganisms including bacteria and viruses appear, and the bacteria and the viruses pose serious threats to the life health of human beings. With the enhancement of health care consciousness of people, higher requirements are also put forward on living goods.
The cotton fiber has excellent moisture absorption and air permeability, is soft and warm, has no side effect when contacting with skin, has good sanitary performance, but is easy to be polluted by microorganisms, and has poor antibacterial and mildewproof effects, so the application of the cotton fiber is limited. In order to expand the application field of cotton fibers, researches on modification and function compounding on the basis of the cotton fibers are more and more, and particularly, the antibacterial, antiviral, skin-care and health-care effects are rapidly developed.
The natural antibacterial agent extracted from the tea leaves and the Chinese herbal medicines has high antibacterial efficiency, safety and no toxicity. Chinese patent CN201410540645.4 discloses a Chinese herbal medicine antibacterial cotton fiber and a preparation method thereof. The modified cotton fiber is prepared by mixing the Chinese herbal medicine soaking solution into the spinning solution for spinning, and the content of the Chinese herbal medicine antibacterial components in the modified cotton fiber obtained by the treatment mode is limited, so that the persistence of the antibacterial and antiviral functions of the modified cotton fiber is not facilitated.
Chinese patents CN201811252564.9 (a plant source composite functional grass cotton fiber and a preparation method thereof) and CN201811252563.4 (a high-efficiency cool feeling mildew-proof grass cotton and a preparation method thereof) disclose several functional composite grass cotton and preparation methods thereof. According to the technical scheme disclosed by the invention, the function of the cotton fiber is mainly obtained through physical actions such as post-treatment (auxiliary agent adsorption), and the like, and the durability of the antibacterial function of the cotton fiber is influenced due to poor binding performance between the additive substance and the cotton fiber.
How to make cotton fiber have lasting antibacterial and antiviral properties is to be explored.
Disclosure of Invention
In order to solve the technical problems, the invention provides the antibacterial, antiviral and deodorant cotton fiber which has better antibacterial, antiviral durability and deodorant performance.
The invention provides an antibacterial, antiviral and deodorant cotton fiber, which comprises a cotton fiber and a beta-cyclodextrin/antibacterial agent compound;
the beta-cyclodextrin/antibacterial agent complex comprises beta-cyclodextrin and an antibacterial agent adsorbed in the porous pores of the beta-cyclodextrin, wherein the antibacterial agent comprises a plant natural antibacterial agent and a complex, and the complex is a complex of metal ions contained in an inorganic antibacterial agent and phytic acid;
the cotton fiber is grafted and crosslinked with beta-cyclodextrin in the beta-cyclodextrin/antibacterial agent compound.
Preferably, the botanical natural antibacterial agent comprises one or more of tea extract, honeysuckle extract, coptis extract, indigowoad leaf extract, isatis root extract, bupleurum extract, liquorice extract, forsythia extract and astragalus extract;
the inorganic antibacterial agent comprises Zn2+An inorganic antibacterial agent.
Preferably, the mass ratio of the cotton fibers to the beta-cyclodextrin/antibacterial agent compound is 100: 4-10;
the mass ratio of the antibacterial agent to the beta-cyclodextrin is 1-3: 1;
the mass ratio of the plant natural antibacterial agent to the inorganic antibacterial agent is 1-4: 1;
the mass ratio of the inorganic antibacterial agent to the phytic acid is 2-6: 1.
The invention also provides a preparation method of the antibacterial, antiviral and deodorant cotton fiber, which comprises the following steps:
firstly mixing beta-cyclodextrin, a plant natural antibacterial agent, an inorganic antibacterial agent and water to obtain a beta-cyclodextrin/antibacterial agent compound dispersion system;
carrying out second mixing on the cotton fibers and the beta-cyclodextrin/antibacterial agent compound dispersion system to obtain adsorbed cotton fibers;
sequentially carrying out stabilization treatment and irradiation treatment on the adsorption cotton fiber to obtain antibacterial, antiviral and deodorant cotton fiber;
the stabilizing solution is phytic acid aqueous solution.
Preferably, the method further comprises pretreating the cotton fiber before the second mixing, wherein the pretreatment comprises mercerizing and plasma etching which are sequentially performed.
Preferably, the mercerizing agent for mercerizing comprises a sodium hydroxide solution, the concentration of the sodium hydroxide solution is 200-280 g/L, the bath ratio of mercerizing is 1: 10-25, the temperature is 20-30 ℃, and the time is 40-80 s;
the working gas of the plasma etching is air, the output power is 100-300W, and the time is 1-3 min.
Preferably, the first mixing comprises the steps of:
thirdly mixing the beta-cyclodextrin with water to obtain a saturated solution of the beta-cyclodextrin;
fourthly, mixing the plant natural antibacterial agent, the inorganic antibacterial agent and the saturated solution of the beta-cyclodextrin to obtain a beta-cyclodextrin/antibacterial agent compound dispersion system;
the mass ratio of the total mass of the plant natural antibacterial agent and the inorganic antibacterial agent to the beta-cyclodextrin is 1-6: 1;
the mass ratio of the plant natural antibacterial agent to the inorganic antibacterial agent is 1-4: 1.
Preferably, the second mixing mode is soaking, the soaking temperature is 15-50 ℃, and the time is 1-2 hours.
Preferably, the bath ratio of the soaking is 1: 10-20.
Preferably, the irradiation intensity of the irradiation treatment is 30-70 kGy, and the time is 60-120 s.
The invention also provides the application of the antibacterial, antiviral and deodorant cotton fiber in the technical scheme or the antibacterial, antiviral and deodorant cotton fiber prepared by the preparation method in the technical scheme in textiles.
The antibacterial, antiviral and deodorant cotton fiber provided by the invention comprises cotton fiber and a beta-cyclodextrin/antibacterial agent compound; the beta-cyclodextrin/antibacterial agent complex comprises beta-cyclodextrin and an antibacterial agent adsorbed in the porous pores of the beta-cyclodextrin, wherein the antibacterial agent comprises a plant natural antibacterial agent and a complex, and the complex is a complex of metal ions contained in an inorganic antibacterial agent and phytic acid; the cotton fiber is grafted and crosslinked with beta-cyclodextrin in the beta-cyclodextrin/antibacterial agent compound. The antibacterial, antiviral and deodorant cotton fiber provided by the invention contains a plant natural antibacterial agent and a complex, the complex is a complex of metal ions contained in an inorganic antibacterial agent and phytic acid, and under the combined action of the natural plant antibacterial agent and the complex, the cotton fiber has good antibacterial and antiviral properties; the beta-cyclodextrin effectively protects the natural plant antibacterial agent, avoids the phenomenon that the natural plant antibacterial agent is damaged or lost in the processing process, and the beta-cyclodextrin and the cotton fiber generate graft crosslinking, so that the binding performance of the antibacterial agent and the cotton fiber is further improved, and meanwhile, the antibacterial and antiviral durability of the cotton fiber is improved; the phytic acid and metal ions contained in the inorganic antibacterial agent are complexed to form a complex, so that the stability of the inorganic antibacterial agent is improved, the content of the inorganic antibacterial agent in the fiber is ensured, and the antibacterial and antiviral durability of the fiber is improved. Therefore, the antibacterial, antiviral and deodorant cotton fiber provided by the invention has lasting and good antibacterial and antiviral properties.
Moreover, in the invention, the introduction of the phytic acid also improves the flame retardance of the cotton fiber; the porous structure in the beta-cyclodextrin can also adsorb odor gas, so that the fiber has a deodorizing effect.
Detailed Description
The invention provides an antibacterial, antiviral and deodorant cotton fiber, which comprises a cotton fiber and a beta-cyclodextrin/antibacterial agent compound;
the beta-cyclodextrin/antibacterial agent complex comprises beta-cyclodextrin and an antibacterial agent adsorbed in the porous pores of the beta-cyclodextrin, wherein the antibacterial agent comprises a plant natural antibacterial agent and a complex, and the complex is a complex of metal ions contained in an inorganic antibacterial agent and phytic acid;
the cotton fiber is grafted and crosslinked with beta-cyclodextrin in the beta-cyclodextrin/antibacterial agent compound.
In the present invention, all the raw materials are commercially available products well known to those skilled in the art unless otherwise specified.
The antibacterial, antiviral and deodorant cotton fiber provided by the invention comprises cotton fiber. In the invention, the surface of the cotton fiber preferably comprises holes, the holes are preferably obtained by performing plasma etching treatment on the cotton fiber, and the holes are more favorable for adsorbing the beta-cyclodextrin/antibacterial agent compound.
The antibacterial, antiviral and deodorant cotton fiber provided by the invention also comprises a beta-cyclodextrin/antibacterial agent compound, and the cotton fiber is grafted and crosslinked with the beta-cyclodextrin in the beta-cyclodextrin/antibacterial agent compound. In the present invention, the beta-cyclodextrin/antimicrobial agent complex comprises beta-cyclodextrin and an antimicrobial agent adsorbed within the pores of the beta-cyclodextrin; in the invention, the mass ratio of the antibacterial agent to the beta-cyclodextrin is preferably 1-3: 1, and more preferably 2-3: 1.
In the present invention, the antibacterial agent includes a plant natural antibacterial agent and a complex of a metal ion contained in an inorganic antibacterial agent and phytic acid. In the present invention, the botanical natural antibacterial agent preferably includes one or more of a tea extract, a honeysuckle extract, a coptis extract, a folium isatidis extract, an isatis root extract, a bupleurum extract, a licorice extract, a forsythia extract and an astragalus extract, and when the botanical natural antibacterial agent includes a plurality of extracts, the present invention does not specifically limit the compounding ratio of the specific extracts as long as the amount of the botanical natural antibacterial agent can be satisfied. In an embodiment of the present invention, the botanical natural antibacterial agent preferably comprises a mixture of tea leaf extract, honeysuckle extract and coptis extract, a mixture of tea leaf extract, indigowoad leaf extract and indigowoad root extract, a mixture of tea leaf extract, bupleurum extract and licorice extract, or a mixture of tea leaf extract, forsythia extract and astragalus extract; the mass ratio of the tea extract, the honeysuckle extract and the coptis extract is 2:2:1, the mass ratio of the tea extract, the folium isatidis extract and the isatis root extract is 2:1:2, the mass ratio of the tea extract, the bupleurum extract and the liquorice extract is 2:1:1, and the mass ratio of the tea extract, the forsythia extract and the astragalus extract is 3:1: 1.
In the present invention, the inorganic antibacterial agent preferably includes Zn2+Inorganic antibacterial agent, said Zn2+The inorganic antimicrobial agent preferably comprises ZnCl2Or ZnSO4. In the invention, the mass ratio of the inorganic antibacterial agent to the phytic acid is preferably 2-6: 1, and more preferably 3-4: 1. In the invention, the mass ratio of the plant natural antibacterial agent to the inorganic antibacterial agent is preferably 1-4: 1, and more preferably 2-3: 1.
In the invention, the mass ratio of the cotton fibers to the beta-cyclodextrin/antibacterial agent compound is preferably 100: 4-10, and more preferably 100: 8-9.
The invention also provides a preparation method of the antibacterial, antiviral and deodorant cotton fiber, which comprises the following steps:
firstly mixing beta-cyclodextrin, a plant natural antibacterial agent, an inorganic antibacterial agent and water to obtain a beta-cyclodextrin/antibacterial agent compound dispersion system;
carrying out second mixing on the cotton fibers and the beta-cyclodextrin/antibacterial agent compound dispersion system to obtain adsorbed cotton fibers;
sequentially carrying out stabilization treatment and irradiation treatment on the adsorption cotton fiber to obtain antibacterial, antiviral and deodorant cotton fiber;
the stabilizing solution is phytic acid aqueous solution.
The beta-cyclodextrin/antibacterial agent composite dispersion system is prepared by mixing beta-cyclodextrin, a plant natural antibacterial agent, an inorganic antibacterial agent and water for the first time. In the present invention, the first mixing preferably includes the steps of:
thirdly mixing the beta-cyclodextrin with water to obtain a saturated solution of the beta-cyclodextrin;
and fourthly, mixing the plant natural antibacterial agent, the inorganic antibacterial agent and the saturated solution of the beta-cyclodextrin to obtain a beta-cyclodextrin/antibacterial agent compound dispersion system.
The beta-cyclodextrin and water are subjected to third mixing to obtain a saturated solution of the beta-cyclodextrin. In the invention, the water preferably comprises deionized water, and the temperature of the third mixing is preferably 40-70 ℃, and more preferably 46-58 ℃. The amount of water used in the present invention is not particularly limited as long as a saturated solution of β -cyclodextrin can be obtained. The mixing method of the third mixing is not particularly limited in the present invention, as long as the third mixing can be uniformly mixed.
After the saturated solution of the beta-cyclodextrin is obtained, the invention carries out fourth mixing on the plant natural antibacterial agent, the inorganic antibacterial agent and the saturated solution of the beta-cyclodextrin to obtain a beta-cyclodextrin/antibacterial agent compound dispersion system. In the present invention, the temperature of the fourth mixing is preferably the same as the temperature of the third mixing. In the invention, the mass ratio of the total mass of the plant natural antibacterial agent and the inorganic antibacterial agent to the beta-cyclodextrin is preferably 1-6: 1, and more preferably 2-4: 1. (ii) a The mass ratio of the plant natural antibacterial agent to the inorganic antibacterial agent is preferably 1-4: 1, and more preferably 2-3: 1. In the invention, the fourth mixing is preferably carried out under stirring conditions, the stirring preferably comprises a first stirring and a second stirring which are sequentially carried out, the rotation speed of the first stirring is preferably 1500-2500 r/min, more preferably 1750-2105 r/min, and the time of the first stirring is preferably 15-30 min, more preferably 21-26 min; the rotation speed of the second stirring is preferably 500-800 r/min, more preferably 560-695 r/min, and the time of the second stirring is preferably 1.5-3 h, more preferably 2-2.5 h. In the present invention, the second stirring is performed immediately after the first stirring is completed. The mixing sequence of the fourth mixing in the present invention is not particularly limited, and may be performed by a mixing sequence known to those skilled in the art.
After the beta-cyclodextrin/antibacterial agent compound dispersion system is obtained, the cotton fibers and the beta-cyclodextrin/antibacterial agent compound dispersion system are mixed for the second time to obtain the adsorption cotton fibers. According to the invention, the cotton fibers are preferably pretreated before the second mixing, and the pretreatment preferably comprises mercerization and plasma etching which are sequentially carried out. In the present invention, the cotton fiber is preferably cotton fiber obtained after carding
In the present invention, the mercerization is preferably carried out by impregnating cotton fibers with a mercerizing agent. The invention preferably performs carding treatment on the cotton fibers before the impregnation, has no special requirement on the carding treatment, and adopts a mode known by the technical personnel in the field. In the invention, the mercerizing agent preferably comprises a sodium hydroxide solution, and the concentration of the sodium hydroxide solution is preferably 200-280 g/L, and more preferably 225-253 g/L; the mercerizing bath ratio is preferably 1: 10-25, more preferably 1: 15-20, and the mercerizing bath ratio is preferably the volume ratio of the mass of the cotton fibers to the mercerizing agent; the mercerizing temperature is preferably 20-30 ℃, and more preferably 23-26 ℃; the time is preferably 40 to 80 seconds, and more preferably 55 to 68 seconds. In the invention, the roundness of the mercerized cotton fiber is increased, the surface is smooth, and the subsequent full treatment of the cotton fiber is facilitated.
In the invention, after mercerization, preferably, the mercerized cotton fiber is subjected to first pressing, water washing, acid washing and drying in sequence. The first press is not limited in any way, and the process known to those skilled in the art can be adopted to ensure that the moisture content of the cotton fiber after the first press is preferably 60-90%, and more preferably 75.2-83%. In the present invention, the first press may remove a portion of the mercerizing agent in the fiber to reduce the amount of the water-washing and acid-washing solutions.
In the invention, the temperature of the water washing is preferably 20-30 ℃, and more preferably 22-26 ℃; the mass ratio of the water for washing to the cotton fibers is preferably 15-35: 1, and more preferably 21-28: 1. The invention has no special requirement on the pH value of the cotton fiber after washing, and the pH value of the cotton fiber after acid washing can meet the requirement.
In the invention, the solution for acid washing preferably comprises an acid solution, the acid solution preferably comprises a hydrochloric acid solution or a sulfuric acid solution, and the concentration of the acid solution is preferably 20-50 g/L, and more preferably 28-39 g/L. In the invention, the pickling temperature is preferably 20-30 ℃, and more preferably 22-26 ℃. In the invention, the pH value of the acid-washed cotton fiber is preferably 6-8, and more preferably 6.5-7.5. The invention has no special limitation on the dosage of the solution for acid washing, as long as the pH value of the acid-washed cotton fiber can meet the requirement. The pH detection method of the cotton fiber is not specially limited, and the conventional technical means in the field can be adopted. In the invention, the pickling process preferably further comprises a second pressing process of the pickled cotton fibers, wherein the second pressing process can remove pickling solution in the pickled cotton fibers, so that the energy consumption for drying is reduced.
The pH value of the cotton fiber is limited to 6-8, so that the cotton fiber can be ensured to have good performance after being dried, if the acidity of the cotton fiber is too high, the cotton fiber is crisp and fragile and is easy to break, and if the alkalinity of the cotton fiber is too high, the surface of the cotton fiber is whitened, so that the attractiveness is affected; meanwhile, the corrosivity of the cotton fibers can be increased, so that a large amount of dust is generated in the subsequent opening process of the cotton fibers, the mechanical property of the cotton fibers is influenced, and the subsequent use of the cotton fibers is influenced.
In the invention, the drying temperature is preferably 105-120 ℃, more preferably 112-115 ℃, and the time is preferably 30-50 min, more preferably 36-41 min.
In the invention, the working gas for plasma etching is preferably air; the output power of the plasma etching is preferably 100-300W, and more preferably 150-230W; the time is preferably 1 to 3min, more preferably 2 to 2.5 min. In the invention, the plasma etching treatment enables a plurality of holes to be formed on the surface of the mercerized cotton fiber, which is beneficial to adsorbing beta-cyclodextrin/antibacterial agent compounds, and simultaneously increases the surface area of the mercerized cotton fiber so as to improve the content of antibacterial agent in the antibacterial, antiviral and deodorant cotton fiber; meanwhile, more hydrophilic groups such as carboxyl are formed on the surface of the cotton fiber after mercerization through plasma etching treatment, and the hydrophilic groups can be subjected to graft crosslinking reaction with beta-cyclodextrin under irradiation conditions.
In the invention, the second mixing mode is preferably soaking, and the soaking temperature is preferably 15-50 ℃, and more preferably 28-40 ℃; the soaking time is preferably 1-2 hours, more preferably 1.5 hours, and the soaking bath ratio is preferably 1: 10-20, more preferably 1: 15-20. In the present invention, the bath ratio of the soaking is the ratio of the mass of the cotton fiber to the volume of the dispersion of the β -cyclodextrin/antibacterial agent complex. The invention preferably turns over the cotton fibers in the soaking process, the frequency of turning over is preferably once every 10min, and the turning over can enable the cotton fibers to fully adsorb the beta-cyclodextrin/antibacterial agent compound in the beta-cyclodextrin/antibacterial agent compound dispersion system.
After the adsorption cotton fiber is obtained, the invention sequentially carries out stabilization treatment and irradiation treatment on the adsorption cotton fiber to obtain the antibacterial, antiviral and deodorant cotton fiber.
According to the invention, the adsorbed cotton fibers are preferably subjected to third pressing before stabilization treatment, and the mass ratio of the product after the third pressing to the cotton fibers is preferably 2-5: 1, and more preferably 2-3: 1. In the invention, the third press can remove water in the adsorbed cotton fibers, and the influence of dilution of the phytic acid aqueous solution in the stabilizing treatment process is avoided, so that the stabilizing treatment effect is ensured.
In the invention, the solution for stabilizing is phytic acid aqueous solution, and the concentration of the phytic acid aqueous solution is preferably 5-15 g/L, and more preferably 8.5-12.6 g/L. In the invention, the stabilizing treatment is preferably to soak the adsorption cotton fiber in a phytic acid aqueous solution, and the bath ratio of the stabilizing treatment is preferably 1: 5-15, and more preferably 1: 8-12; the soaking temperature is preferably 50-70 ℃, more preferably 56-65 ℃, and the time is preferably 0.5-1.5 h, more preferably 1-1.2 h; in the present invention, the bath ratio of the stabilization treatment is the ratio of the mass of the adsorbed cotton fibers to the volume of the phytic acid aqueous solution. The metal ions contained in the inorganic antibacterial agent are complexed with the phytic acid to form a complex through the stabilizing treatment, so that the stability of the inorganic antibacterial agent is enhanced, and the durability of antibiosis, antivirus and deodorization of the cotton fiber is improved; meanwhile, the formed complex forms a coating layer on the surface of part of the plant natural antibacterial agent, and further effectively protects and reduces the loss of the plant natural antibacterial agent.
In the present invention, the stabilizing treatment preferably further comprises dewatering, oiling, fourth pressing, wet opening and drying, which are sequentially performed.
In the invention, the moisture content of the dehydrated cotton fiber is preferably 70-95%, and more preferably 78-90%. The invention is not particularly limited in the manner of the dehydration, as long as the moisture content of the dehydrated cotton fiber can meet the requirement.
In the present invention, the upper oil bath for upper oil preferably includes an emulsion and a solvent. In the present invention, the emulsion is preferably available from HONOLMGR of Japan bamboo fat and oil (Suzhou) Co., Ltd, and the solvent is preferably water. In the invention, the concentration of HONOLMGR in the oiling bath liquid is preferably 4-7 g/L, and more preferably 5-6 g/L.
In the invention, the moisture content of the fourth pressed cotton fiber is preferably 60-90%, and more preferably 66-78%. In the present invention, the fourth pressing mode is not particularly limited as long as the desired moisture content can be achieved.
The invention has no special requirement on wet opening cotton and can be realized by adopting the conventional means in the field.
In the invention, the drying temperature is preferably 95-115 ℃, more preferably 102-108 ℃, and the time is preferably 40-80 min, more preferably 55-65 min.
In the invention, the irradiation treatment is preferably electron beam irradiation, and the irradiation intensity of the irradiation treatment is preferably 30-70 kGy, and more preferably 38-55 kGy; the time is 60 to 120s, and more preferably 85 to 108 s. In the invention, the irradiation treatment enables the cotton fiber and the beta-cyclodextrin to form graft crosslinking, so that the bonding strength of the beta-cyclodextrin and the cotton fiber is improved, and the antibacterial and antiviral durability of the antibacterial, antiviral and deodorant cotton fiber is further improved. In the invention, the grafting crosslinking is preferably a grafting crosslinking reaction between hydrophilic groups formed after plasma etching of cotton fibers and hydroxyl groups on the surface of beta-cyclodextrin.
The antibacterial, antiviral and deodorant cotton fiber prepared by the preparation method has better glossiness, contains a plant natural antibacterial agent, an inorganic antibacterial agent and beta-cyclodextrin, and holes in the beta-cyclodextrin can adsorb peculiar smell to achieve the effect of deodorization.
The invention also provides the application of the antibacterial, antiviral and deodorant cotton fiber in the technical scheme or the application of the antibacterial, antiviral and deodorant cotton fiber prepared by the preparation method in the technical scheme in textiles.
The antibacterial, antiviral and deodorant cotton fiber provided by the invention is processed into textiles, has lasting antibacterial and antiviral properties and has a deodorant function. The textile preferably comprises clothing, ornaments, bedding and the like.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
The embodiment of the invention has no limitation on the grade of the dosage of each raw material, and the raw materials can be prepared by adopting any weight grade as long as the raw materials are mixed according to a specific ratio.
Example 1
Soaking cotton fibers subjected to cotton carding in a sodium hydroxide solution (200g/L, 20 ℃) for 80s at a bath ratio of 1:10, squeezing (the water content of the cotton fibers after squeezing is 60%), washing with water (20 ℃) and acid (20g/L hydrochloric acid, 20 ℃) according to the mass ratio of the water to the cotton fibers of 15:1 to enable the pH value of the mercerized cotton fibers to be 8; drying the mercerized cotton fiber at 105 ℃ for 50min, and then carrying out plasma etching to obtain the pretreated cotton fiber, wherein the working gas of the plasma etching is air, the output power is 100W, and the time is 3 min;
mixing the beta-cyclodextrin with water (40 ℃) to obtain a saturated solution of the beta-cyclodextrin;
mixing saturated solution of beta-cyclodextrin, plant natural extract (folium Camelliae sinensis extract, flos Lonicerae extract and Coptidis rhizoma extract at mass ratio of 2:2: 1), and ZnCl2Mixing, stirring at 1500r/min for 30min, and stirring at 500r/min for 1.5h to obtain a beta-cyclodextrin/antibacterial agent composite dispersion system; wherein ZnCl is2ZnCl and plant natural extract with the mass ratio of 1:12And the mass ratio of the total mass of the plant natural extracts to the beta-cyclodextrin is 1: 1;
soaking the pretreated cotton fibers in a beta-cyclodextrin/antibacterial agent composite dispersion system for 1h (50 ℃), and turning over the pretreated cotton fibers once every 10min in the soaking process to obtain adsorbed cotton fibers; wherein the bath ratio of soaking is 1: 20;
squeezing the adsorbed cotton fiber (the mass ratio of the squeezed product to the cotton fiber is 2:1), soaking in phytic acid aqueous solution (5g/L) (50 deg.C, bath ratio is 1:5) for 1.5h, and stabilizing; dehydrating the stabilized product (the water content after dehydration is 70%), oiling, squeezing (the water content after squeezing is 60%), wet opening, drying and irradiating to obtain antibacterial, antiviral and deodorant cotton fibers; the concentration of HONOLMGR in the oiling bath liquid for oiling is 4 g/L; the drying temperature is 95 ℃ and the drying time is 80 min; the irradiation intensity of the electron beam irradiation treatment was 30kGy and the time was 120 s.
Example 2
Soaking cotton fibers subjected to cotton carding in a sodium hydroxide solution (225g/L, 23 ℃) for 68 seconds at a bath ratio of 1:15, pressing (the water content of the cotton fibers after pressing is 75.2%), and then washing with water (22 ℃) and acid (20g/L hydrochloric acid, 22 ℃) according to the mass ratio of the water to the cotton fibers of 21:1 to ensure that the pH value of the cotton fibers subjected to mercerization is 7; drying the mercerized cotton fiber at 112 ℃ for 41min, and then carrying out plasma etching to obtain the pretreated cotton fiber, wherein the working gas of the plasma etching is air, the output power is 150W, and the time is 2.5 min;
mixing the beta-cyclodextrin with water (46 ℃) to obtain a saturated solution of the beta-cyclodextrin;
mixing saturated solution of beta-cyclodextrin, plant natural extract (mixture of folium Camelliae sinensis extract, folium Isatidis extract, and radix Isatidis extract at a mass ratio of 2:1:2), and Zn2+ZnSO as antibacterial agent4Mixing, stirring at 1750r/min for 26min, and stirring at 560r/min for 2h to obtain a beta-cyclodextrin/antibacterial agent composite dispersion system; in which ZnSO4ZnSO with the mass ratio of 1:2 to the plant natural extract4And the mass ratio of the total mass of the plant natural extracts to the beta-cyclodextrin is 2: 1;
soaking the pretreated cotton fibers in a beta-cyclodextrin/antibacterial agent composite dispersion system for 1.5h (40 ℃), and turning the pretreated cotton fibers once every 10min in the soaking process to obtain adsorbed cotton fibers; wherein the bath ratio of soaking is 1: 17;
squeezing the adsorbed cotton fiber (the mass ratio of the squeezed product to the cotton fiber is 3:1), soaking in phytic acid aqueous solution (8.5g/L) (56 deg.C, bath ratio is 1:8) for 1.2h, and stabilizing; dehydrating the stabilized product (the water content after dehydration is 78%), oiling, squeezing (the water content after squeezing is 66%), wet opening, drying and irradiating to obtain antibacterial, antiviral and deodorant cotton fibers; the concentration of HONOLMGR in the oiling bath liquid for oiling is 5 g/L; the drying temperature is 102 ℃, and the drying time is 65 min; the irradiation intensity of the electron beam irradiation treatment was 38kGy and the time was 108 s.
Example 3
Soaking cotton fibers subjected to cotton carding in a sodium hydroxide solution (253g/L at 26 ℃) for 55 seconds at a bath ratio of 1:20, squeezing (the water content of the cotton fibers after squeezing is 83%), and then washing with water (26 ℃) and acid (39g/L hydrochloric acid at 26 ℃) according to the mass ratio of the water to the cotton fibers of 28:1 to ensure that the pH value of the cotton fibers subjected to mercerization is 6.5; drying the mercerized cotton fiber at 115 ℃ for 36min, and then carrying out plasma etching to obtain the pretreated cotton fiber, wherein the working gas of the plasma etching is air, the output power is 230W, and the time is 2 min;
mixing beta-cyclodextrin with water (58 ℃),obtaining a saturated solution of beta-cyclodextrin; mixing saturated solution of beta-cyclodextrin, plant natural extract (mixture of folium Camelliae sinensis extract, bupleuri radix extract, and Glycyrrhrizae radix extract at a mass ratio of 2:1:1) and Zn2+Antibacterial agent ZnCl2Mixing, stirring at 2105r/min for 21min, and stirring at 695r/min for 2.5h to obtain a beta-cyclodextrin/antibacterial agent composite dispersion system; wherein ZnCl is2ZnCl and plant natural extract with the mass ratio of 1:32And the mass ratio of the total mass of the plant natural extracts to the beta-cyclodextrin is 4: 1;
soaking the pretreated cotton fibers in a beta-cyclodextrin/antibacterial agent composite dispersion system for 1.5h (28 ℃), and turning the pretreated cotton fibers once every 10min in the soaking process to obtain adsorbed cotton fibers; wherein the bath ratio of soaking is 1: 15;
squeezing the adsorbed cotton fiber (the mass ratio of the squeezed product to the cotton fiber is 4:1), soaking in phytic acid aqueous solution (12.6g/L) (65 deg.C, bath ratio is 1:12) for 1h, and stabilizing; dehydrating the stabilized product (the water content after dehydration is 90%), oiling, squeezing (the water content after squeezing is 78%), wet opening, drying and irradiating to obtain antibacterial, antiviral and deodorant cotton fibers; the concentration of HONOLMGR in the oiling bath liquid for oiling is 6 g/L; the drying temperature is 108 ℃, and the drying time is 55 min; the irradiation intensity of the electron beam irradiation treatment was 55kGy for 85 s.
Example 4
Soaking cotton fibers subjected to cotton carding in a sodium hydroxide solution (280g/L, 30 ℃) for 40s at a bath ratio of 1:20, squeezing (the water content of the cotton fibers after squeezing is 90%), washing with water (30 ℃) and acid (50g/L hydrochloric acid, 30 ℃) according to the mass ratio of the water to the cotton fibers of 35:1 to ensure that the pH value of the cotton fibers subjected to mercerization is 6; drying the mercerized cotton fiber at 120 ℃ for 30min, and then carrying out plasma etching to obtain the pretreated cotton fiber, wherein the working gas of the plasma etching is air, the output power is 300W, and the time is 1 min;
mixing beta-cyclodextrin with water (70 deg.C) to obtain beta-cyclodextrinA fine saturated solution; mixing saturated solution of beta-cyclodextrin, plant natural extract (mixture of folium Camelliae sinensis extract, fructus forsythiae extract and radix astragali extract at a mass ratio of 3:1:1) and Zn2+ZnSO as antibacterial agent4Mixing, stirring at 2500r/min for 15min, and stirring at 800r/min for 3h to obtain a beta-cyclodextrin/antibacterial agent composite dispersion system; in which ZnSO4ZnSO with the mass ratio of plant natural extract of 1:44And the mass ratio of the total mass of the plant natural extracts to the beta-cyclodextrin is 6: 1;
soaking the pretreated cotton fibers in a beta-cyclodextrin/antibacterial agent composite dispersion system for 2h (15 ℃), and turning the pretreated cotton fibers once every 10min in the soaking process to obtain adsorbed cotton fibers; wherein the bath ratio of soaking is 1: 10;
squeezing the adsorbed cotton fiber (the mass ratio of the squeezed product to the cotton fiber is 5:1), soaking in phytic acid aqueous solution (15g/L) (70 deg.C, bath ratio is 1:15) for 0.5h, and stabilizing; dehydrating the stabilized product (the water content after dehydration is 95%), oiling, squeezing (the water content after squeezing is 90%), wet opening, drying and irradiating to obtain antibacterial, antiviral and deodorant cotton fibers; the concentration of HONOLMGR in the oiling bath liquid for oiling is 7 g/L; the drying temperature is 115 ℃ and the drying time is 40 min; the irradiation intensity of the electron beam irradiation treatment was 70kGy for 60 s.
Test example:
according to JISL 1902: 2008 antibacterial effect of textile antibacterial performance test method, the antibacterial activity value and the bactericidal activity value of the antibacterial, antiviral and deodorant cotton fibers prepared in examples 1-4 are detected, and the results are listed in table 1.
The invention detects the antiviral activity values of the antibacterial, antiviral and deodorant cotton fibers prepared in the embodiments 1-4 on influenza A virus and influenza B virus according to ISO198184:2014 'antiviral test method of textile products', and the results are listed in Table 1.
TABLE 1 antibacterial, antiviral, deodorant Cotton fibers prepared in examples 1-4 have antibacterial and antiviral Properties
As can be seen from the data in Table 1, the antibacterial, antiviral and deodorant cotton fiber provided by the invention has higher bacteriostatic activity value and bactericidal activity value, and simultaneously has higher antiviral activity values on influenza A virus and influenza B virus, and has better antibacterial and antiviral properties.
The deodorization performance of the antibacterial, antiviral and deodorant cotton fibers prepared in the embodiments 1-4 is detected by a detection tube method according to ISO17299-2-2014 textile deodorization performance determination part 2, and the results are listed in Table 2.
TABLE 2 deodorant Properties of antibacterial, antiviral, deodorant cotton fibers prepared in examples 1 to 4
| Examples | Example 1 | Example 2 | Example 3 | Example 4 |
| Ammonia gas elimination ratio (%) | 81 | 83 | 84 | 86 |
| Acetic acid elimination ratio (%) | 74 | 76 | 79 | 82 |
Note: removal rate (initial concentration-post-adsorption concentration)/initial concentration 100
The data in table 2 show that the antibacterial, antiviral and deodorant cotton fiber provided by the invention has higher ammonia gas elimination rate and acetic acid elimination rate, so that the cotton fiber has good deodorization performance.
The antibacterial, antiviral and deodorant cotton fibers prepared in examples 1 to 4 were washed 50 times according to standard FZ/T73023-2006 appendix c4. simplified washing conditions and washing methods in the procedure, and then according to JISL 1902: 2008 and ISO198184:2014, the antibacterial, antiviral and deodorant performances of the antibacterial, antiviral and deodorant cotton fiber after 50 times of washing are detected, and the results are listed in Table 3; the deodorizing performance of the antibacterial, antiviral and deodorizing cotton fibers after washing 50 times was measured according to ISO17299-2-2014 textile deodorizing performance measurement part 2, and the results are shown in Table 4.
TABLE 3 antibacterial and antiviral properties of cellulose fibers prepared in examples 1 to 4 after washing 50 times
TABLE 4 deodorization Performance after washing 50 times of fibers prepared in examples 1 to 4
| Examples | Example 1 | Example 2 | Example 3 | Example 4 |
| Ammonia gas elimination ratio (%) | 79 | 80 | 82 | 85 |
| Acetic acid elimination ratio (%) | 72 | 75 | 78 | 80 |
It can be seen from tables 3 and 4 that the antibacterial, antiviral and deodorant cotton fiber provided by the present invention still has high antibacterial, antiviral and deodorant performance after 50 times of washing, which proves that the antibacterial, antiviral and deodorant cotton fiber provided by the present invention has lasting antibacterial, antiviral and deodorant performance.
The antibacterial, antiviral and deodorant cotton fiber provided by the invention has lasting antibacterial and antiviral properties, and can inhibit the growth of bacteria and viruses, so that the odor generated by the bacteria or the viruses is reduced; meanwhile, the beta-cyclodextrin contained in the antibacterial, antiviral and deodorant cotton fiber provided by the invention has a porous structure capable of adsorbing odor gas to achieve the aim of deodorization.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (11)
1. An antibacterial, antiviral, deodorant cotton fiber comprises cotton fiber and beta-cyclodextrin/antibacterial agent complex;
the beta-cyclodextrin/antibacterial agent complex comprises beta-cyclodextrin and an antibacterial agent adsorbed in the porous pores of the beta-cyclodextrin, wherein the antibacterial agent comprises a plant natural antibacterial agent and a complex, and the complex is a complex of metal ions contained in an inorganic antibacterial agent and phytic acid;
the cotton fiber is grafted and crosslinked with beta-cyclodextrin in the beta-cyclodextrin/antibacterial agent compound.
2. The antibacterial, antiviral, deodorant cotton fiber according to claim 1, wherein the botanical natural antibacterial agent comprises one or more of tea extract, honeysuckle extract, coptis extract, isatis leaf extract, isatis root extract, bupleurum extract, glycyrrhiza extract, forsythia extract and astragalus extract;
the inorganic antibacterial agent comprises Zn2+An inorganic antibacterial agent.
3. The antibacterial, antiviral and deodorant cotton fiber according to claim 1, wherein the mass ratio of the cotton fiber to the beta-cyclodextrin/antibacterial agent compound is 100: 4-10;
the mass ratio of the antibacterial agent to the beta-cyclodextrin is 1-3: 1;
the mass ratio of the plant natural antibacterial agent to the inorganic antibacterial agent is 1-4: 1;
the mass ratio of the inorganic antibacterial agent to the phytic acid is 2-6: 1.
4. A method for preparing the antibacterial, antiviral and deodorant cotton fiber according to any one of claims 1 to 3, characterized by comprising the steps of:
firstly mixing beta-cyclodextrin, a plant natural antibacterial agent, an inorganic antibacterial agent and water to obtain a beta-cyclodextrin/antibacterial agent compound dispersion system;
carrying out second mixing on the cotton fibers and the beta-cyclodextrin/antibacterial agent compound dispersion system to obtain adsorbed cotton fibers;
sequentially carrying out stabilization treatment and irradiation treatment on the adsorption cotton fiber to obtain antibacterial, antiviral and deodorant cotton fiber;
the stabilizing solution is phytic acid aqueous solution.
5. The preparation method according to claim 4, characterized by further comprising pretreating the cotton fibers before the second mixing, wherein the pretreatment comprises mercerizing and plasma etching which are sequentially performed.
6. The preparation method according to claim 5, characterized in that the mercerizing agent for mercerizing comprises a sodium hydroxide solution, the concentration of the sodium hydroxide solution is 200-280 g/L, the bath ratio for mercerizing is 1: 10-25, the temperature is 20-30 ℃, and the time is 40-80 s;
the working gas of the plasma etching is air, the output power is 100-300W, and the time is 1-3 min.
7. The method of manufacturing according to claim 4, wherein the first mixing comprises the steps of:
thirdly mixing the beta-cyclodextrin with water to obtain a saturated solution of the beta-cyclodextrin;
fourthly, mixing the plant natural antibacterial agent, the inorganic antibacterial agent and the saturated solution of the beta-cyclodextrin to obtain a beta-cyclodextrin/antibacterial agent compound dispersion system;
the mass ratio of the total mass of the plant natural antibacterial agent and the inorganic antibacterial agent to the beta-cyclodextrin is 1-6: 1;
the mass ratio of the plant natural antibacterial agent to the inorganic antibacterial agent is 1-4: 1.
8. The preparation method according to claim 4 or 5, wherein the second mixing is carried out by soaking at 15-50 ℃ for 1-2 h.
9. The method according to claim 8, wherein the bath ratio of the soaking is 1: 10-20.
10. The method according to claim 4, wherein the irradiation treatment is performed at an irradiation intensity of 30 to 70kGy for a period of 60 to 120 seconds.
11. Use of the antibacterial, antiviral and deodorant cotton fiber according to any one of claims 1 to 3 or the antibacterial, antiviral and deodorant cotton fiber prepared by the preparation method according to any one of claims 4 to 10 in textiles.
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