CN115613211A - Antibacterial warm-keeping flocculus and preparation process thereof - Google Patents

Antibacterial warm-keeping flocculus and preparation process thereof Download PDF

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Publication number
CN115613211A
CN115613211A CN202211104406.5A CN202211104406A CN115613211A CN 115613211 A CN115613211 A CN 115613211A CN 202211104406 A CN202211104406 A CN 202211104406A CN 115613211 A CN115613211 A CN 115613211A
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antibacterial
flocculus
fiber
chitosan oligosaccharide
soaking
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马晓飞
刘洪印
荣小瑛
刘平平
张瑞
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Jixiang Sanbao High Tech Textile Co Ltd
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Jixiang Sanbao High Tech Textile Co Ltd
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    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/02—Cotton wool; Wadding
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • 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
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D04H1/43835—Mixed fibres, e.g. at least two chemically different fibres or fibre blends
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • D06B3/18—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics combined with squeezing, e.g. in padding machines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • 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
    • D06M11/73—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 carbon or compounds thereof
    • D06M11/74—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 carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • 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
    • D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention relates to an antibacterial warm-keeping flocculus and a preparation process thereof, belonging to the technical field of flocculus preparation and comprising the following steps: mixing viscose fibers, cotton fibers and three-dimensional curled hollow polyester fibers, and then opening and carding to obtain a fiber net; rearranging the fiber nets, then sending the fiber nets into a lapping machine for lapping to obtain fiber flocculus, and carrying out needling reinforcement to obtain a semi-finished product; adding a coupling agent KH-560 into an ethanol solution to obtain a first treatment solution, placing the semi-finished product into the first treatment solution for soaking, taking out, drying, placing into a second treatment solution for soaking, rolling off residual liquid, repeating the process, completing three-soaking and three-rolling, and drying to obtain the antibacterial thermal insulating flocculus; the antibacterial particles are connected to the flocculus fibers through chemical bonds, the binding firmness is high, the antibacterial particles are not easy to fall off, the air permeability and the moisture permeability of the flocculus are not influenced, the antibacterial effect of the antibacterial particles is excellent, and the antibacterial particles have multiple antibacterial effects of graphene oxide, chitosan oligosaccharide and quaternary phosphonium salt.

Description

Antibacterial warm-keeping flocculus and preparation process thereof
Technical Field
The invention belongs to the technical field of flocculus preparation, and particularly relates to an antibacterial warm-keeping flocculus and a preparation process thereof.
Background
The flocculus refers to a small slice of flocculent precipitate, and also refers to sheet-type flocculent prepared from plant fiber, animal fiber or chemical fiber for keeping warm, insulating heat or preventing shock.
In winter clothing materials, the wadding piece has good heat insulation and warm keeping effects due to the fluffy structural performance of the wadding piece, and for a long time, people are used to use down, cotton wool, wool wadding and the like as warm keeping wadding pieces.
However, the existing warm-keeping flocculus has poor antibacterial performance, the cost of the antibacterial fiber is high, the antibacterial agent is sprayed by post-treatment, the binding property between the antibacterial agent and the fiber is poor, the antibacterial agent is not washable, and the air permeability between the flocculus and the warm-keeping property of the flocculus are influenced by coating of coatings such as polyurethane and the like, so that the technical problem to be solved at present is to provide the antibacterial warm-keeping flocculus with good performance.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides an antibacterial thermal insulating flocculus and a preparation process thereof.
The purpose of the invention can be realized by the following technical scheme:
an antibacterial warming flocculus is prepared by processing and soaking fiber raw material in antibacterial liquid.
The preparation process of the antibacterial warm-keeping flocculus comprises the following steps:
firstly, uniformly mixing viscose fibers, cotton fibers and three-dimensional curled hollow polyester fibers, and then opening and carding to obtain a fiber net; rearranging the fiber nets by using a disordered roller to enable the fiber nets to form a criss-cross crossed structure, then sending the fiber nets into a lapping machine for lapping to obtain fiber flocculus, and reinforcing the fiber flocculus by needling to obtain a semi-finished product;
and secondly, adding a coupling agent KH-560 into a 90wt% ethanol solution to ensure that the mass fraction of KH-560 is 1.3-1.5%, obtaining a first treatment solution, soaking the semi-finished product in the first treatment solution for 10min, taking out, drying at 60 ℃, soaking in a second treatment solution for 10min, rolling off residual liquid, repeating the process to complete three-soaking and three-rolling, controlling the rolling residual rate to be 40-50%, and then drying at 80 ℃ to obtain the antibacterial thermal insulating flocculus.
Wherein the dosage ratio of the semi-finished product to the first treatment liquid to the second treatment liquid is 1g:10mL of: 10mL, wherein the second treatment liquid is prepared from antibacterial particles, distilled water and a penetrating agent JFC-1 according to the mass ratio of 10-15:100-120:2-3, and mixing.
Further, the antibacterial particles are prepared by the following steps:
ultrasonically dispersing graphene oxide in distilled water to obtain a suspension, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide into the suspension, stirring for 30min, adding modified chitosan oligosaccharide, reacting for 1-1.5h under magnetic stirring at 60 ℃, adding absolute ethyl alcohol after the reaction is finished, centrifuging, washing the precipitate with 2wt% acetic acid solution, and drying at 60 ℃ to constant weight to obtain antibacterial particles, wherein the mass ratio of the graphene oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the modified chitosan oligosaccharide is 1:0.2:0.4-0.5:1.5-2.0.
The graphene oxide has excellent ductility and dispersibility, rich groups and a sharp lamellar structure, and has a sterilization effect through modes of oxidative stress, physical capture, physical cutting, membrane component extraction and the like.
Further, the modified chitosan oligosaccharide is prepared by the following steps:
step S21, under the ice bath condition, adding chitosan oligosaccharide into methane sulfonic acid, stirring and reacting for 30-60min to obtain amino-protected chitosan oligosaccharide, wherein the dosage ratio of the chitosan oligosaccharide to the methane sulfonic acid is 0.02mol:30mL, adopting methane sulfonic acid to protect amino, and having the advantages that methane sulfonic acid not only can act on a reaction medium of the next step, but also can not influence the produced ester bond under the deprotection reaction condition;
step S22, putting (3-carboxypropyl) triphenyl phosphonium bromide into a round-bottom flask, and adding SOCl 2 Stirring at 60 deg.C for 5-6h, absorbing tail gas with 10wt% NaOH solution, removing SOCl by rotary evaporation after reaction 2 To obtain acyl chloride quaternary phosphonium salt; (3-carboxypropyl) triphenylphosphonium bromide and SOCl 2 The dosage ratio is 0.02mol:17-20mL;
step S23, mixing the amino-protected oligosaccharide, acyl chloride quaternary phosphonium salt and anhydrous DMF, reacting for 4-6h at room temperature, recovering tail gas with alkali liquor, and after the reaction is finished, carrying out reduced pressure distillation to remove DMF to obtain grafted chitosan oligosaccharide, wherein the dosage ratio of the amino-protected oligosaccharide to the acyl chloride quaternary phosphonium salt to the anhydrous DMF is 15.4-16.7g:0.86-0.95g:200-250mL;
step S24, adding the grafted chitosan oligosaccharide into deionized water, stirring to completely dissolve the grafted chitosan oligosaccharide, adjusting the pH value to 8.0 by using ammonia water, separating out a precipitate, centrifuging at the rotating speed of 11000r/min for 5min, washing the precipitate by using acetone, and drying to obtain the modified chitosan oligosaccharide, wherein the mass ratio of the grafted chitosan oligosaccharide to the deionized water is 1:10, and the mass fraction of ammonia water is 25%.
Chitosan oligosaccharide is a natural antibacterial agent, has the characteristics of excellent biocompatibility, biological safety and the like, but has a common antibacterial effect, quaternary phosphonium salt is a new generation of high-efficiency, broad-spectrum and low-toxicity bactericide, the P element and the N element of quaternary ammonium salt belong to the same group element, and the quaternary ammonium salt has similar molecular structure and chemical property, but has better heat resistance and wide pH value application range.
Furthermore, the fiber fineness of the three-dimensional curled hollow polyester fiber is 1.5-2.4dtex, and the length is 4-6cm.
Furthermore, the fiber fineness of the viscose fiber is 1.8-2.2dtex, and the length is 4-8.5cm.
Furthermore, the fineness of the cotton fiber is 1.5-2.4dtex, and the length is 2-5.5cm.
The invention has the beneficial effects that:
compared with the traditional antibacterial treatment liquid treatment, the antibacterial warm-keeping flocculus adopts the first treatment liquid (KH-560 ethanol solution) to treat, and then utilizes the second treatment liquid containing antibacterial particles to treat, wherein silicon hydroxyl on polysiloxane formed by hydrolysis of KH-560 reacts with hydroxyl on the flocculus fibers, hydroxyl on the antibacterial particles and other groups, so that the antibacterial particles are connected to the flocculus fibers through chemical bonds, the binding firmness is high, the antibacterial particles are not easy to fall off, the air permeability and the moisture permeability of the flocculus are not influenced, and the antibacterial effect of the antibacterial particles is excellent, and the flocculus has the antibacterial effects of graphene oxide, multi-chitosan oligosaccharide and quaternary phosphorus salt.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An antibacterial particle, which is prepared by the following steps:
ultrasonically dispersing 1g of graphene oxide in 100mL of distilled water to obtain a suspension, adding 0.2g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.4g of N-hydroxysuccinimide into the suspension, stirring for 30min, adding 1.5g of modified chitosan oligosaccharide, reacting for 1h at 60 ℃, magnetically stirring, adding absolute ethyl alcohol after the reaction is finished, centrifuging, washing a precipitate with 2wt% of acetic acid solution, and drying at 60 ℃ to constant weight to obtain the antibacterial particles.
The modified chitosan oligosaccharide is prepared by the following steps:
under the ice bath condition, adding 0.02mol of chitosan oligosaccharide into 30mL of methanesulfonic acid, and stirring for reaction for 30min to obtain amino-protected chitosan oligosaccharide; 0.02mol (3-carboxypropyl) triphenylphosphonium bromide is placed in a round-bottom flask, and 17mL SOCl is added 2 Stirring at 60 deg.C for 5h, absorbing tail gas with 10wt% NaOH solution, and removing SOCl by rotary evaporation after reaction 2 To obtain acyl chloride quaternary phosphonium salt; mixing 15.4g of amino-protected chitosan oligosaccharide, 0.86g of acyl chloride quaternary phosphonium salt and 200mL of anhydrous DMF, reacting for 4h at room temperature, recovering tail gas with alkali liquor, and after the reaction is finished, distilling under reduced pressure to remove DMF to obtain grafted chitosan oligosaccharide; adding the grafted chitosan oligosaccharide into deionized water, stirring to completely dissolve the grafted chitosan oligosaccharide, adjusting the pH value to 8.0 by using ammonia water, separating out a precipitate, centrifuging for 5min at the rotating speed of 11000r/min, washing the precipitate by using acetone, and drying to obtain the modified chitosan oligosaccharide, wherein the mass ratio of the grafted chitosan oligosaccharide to the deionized water is 1:10, and the mass fraction of ammonia water is 25%.
Example 2
An antibacterial particle is prepared by the following steps:
ultrasonically dispersing 1g of graphene oxide in 100mL of distilled water to obtain a suspension, adding 0.2g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.5g of N-hydroxysuccinimide into the suspension, stirring for 30min, adding 2.0g of modified chitosan oligosaccharide, reacting for 1.5h at 60 ℃, adding absolute ethyl alcohol after the reaction is finished, centrifuging, washing the precipitate with 2wt% of acetic acid solution, and drying at 60 ℃ to constant weight to obtain the antibacterial particles.
The modified chitosan oligosaccharide is prepared by the following steps:
under the ice bath condition, adding 0.02mol of chitosan oligosaccharide into 30mL of methane sulfonic acid, and stirring for reaction for 60min to obtain amino-protected chitosan oligosaccharide; 0.02mol (3-carboxypropyl) triphenylphosphonium bromide is placed in a round-bottom flask, and 20mL SOCl is added 2 Stirring reaction at 60 deg.C for 6h, absorbing tail gas with 10wt% NaOH solution, and after the reaction, rotary distilling to remove SOCl 2 To obtain acyl chloride quaternary phosphonium salt; mixing 16.7g of amino-protected chitosan oligosaccharide, 0.95g of acyl chloride quaternary phosphonium salt and 250mL of anhydrous DMF, reacting for 6 hours at room temperature, recovering tail gas with alkali liquor, and after the reaction is finished, carrying out reduced pressure distillation to remove DMF to obtain grafted chitosan oligosaccharide; adding the grafted chitosan oligosaccharide into deionized water, stirring to completely dissolve the grafted chitosan oligosaccharide, adjusting the pH value to 8.0 by using ammonia water, separating out a precipitate, centrifuging for 5min at the rotating speed of 11000r/min, washing the precipitate by using acetone, and drying to obtain the modified chitosan oligosaccharide, wherein the mass ratio of the grafted chitosan oligosaccharide to the deionized water is 1:10, and the mass fraction of ammonia water is 25%.
Comparative example 1
An antibacterial particle is prepared by the following steps:
ultrasonically dispersing 1g of graphene oxide in distilled water to obtain a suspension, adding 0.2g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.5g of N-hydroxysuccinimide into the suspension, stirring for 30min, adding 2.0g of chitosan oligosaccharide, reacting for 1.5h at 60 ℃, adding absolute ethyl alcohol after the reaction is finished, centrifuging, washing a precipitate with 2wt% of acetic acid solution, and drying at 60 ℃ to constant weight to obtain the antibacterial particles.
Comparative example 2
The present comparative example is graphene oxide.
Comparative example 3
This comparative example is a chitosan oligosaccharide with a molecular weight of 1.5kDa.
Example 3
An antibacterial warming flocculus is prepared by processing fiber raw material and soaking in antibacterial solution.
The preparation process of the antibacterial warm-keeping flocculus comprises the following steps:
step one, uniformly mixing viscose fibers, cotton fibers and three-dimensional curled hollow polyester fibers, and then opening and carding to obtain a fiber net; rearranging the fiber nets by using a disordered roller to enable the fiber nets to form a criss-cross crossed structure, then sending the fiber nets into a lapping machine for lapping to obtain fiber flocculus, and reinforcing the fiber flocculus by needling to obtain a semi-finished product;
and secondly, adding a coupling agent KH-560 into a 90wt% ethanol solution to ensure that the mass fraction of KH-560 is 1.3% to obtain a first treatment solution, soaking the semi-finished product in the first treatment solution for 10min, taking out, drying at 60 ℃, soaking in a second treatment solution for 10min, rolling off residual liquid, repeating the process to finish three-soaking and three-rolling, controlling the rolling residual rate at 40%, and drying at 80 ℃ to obtain the antibacterial thermal insulating flocculus.
Wherein the dosage ratio of the semi-finished product to the first treatment liquid to the second treatment liquid is 1g:10mL of: 10mL, and the second treatment liquid was prepared from the antibacterial particles of example 1, distilled water, and a penetrant JFC-1 in a mass ratio of 10:100:2, mixing the components.
The fiber fineness of the three-dimensional curled hollow polyester fiber is 1.5dtex, the length of the three-dimensional curled hollow polyester fiber is 4cm, the fiber fineness of the viscose fiber is 1.8dtex, the length of the viscose fiber is 4cm, the fiber fineness of the cotton fiber is 1.5dtex, and the length of the cotton fiber is 2cm.
Example 4
An antibacterial warming flocculus is prepared by processing and soaking fiber raw material in antibacterial liquid.
The preparation process of the antibacterial warm-keeping flocculus comprises the following steps:
firstly, uniformly mixing viscose fibers, cotton fibers and three-dimensional curled hollow polyester fibers, and then opening and carding to obtain a fiber net; rearranging the fiber nets by using a disordered roller to enable the fiber nets to form a criss-cross crossed structure, then sending the fiber nets into a lapping machine for lapping to obtain fiber flocculus, and reinforcing the fiber flocculus through needling to obtain a semi-finished product;
and secondly, adding a coupling agent KH-560 into a 90wt% ethanol solution to ensure that the mass fraction of KH-560 is 1.4% to obtain a first treatment solution, soaking the semi-finished product in the first treatment solution for 10min, taking out, drying at 60 ℃, soaking in a second treatment solution for 10min, rolling off residual liquid, repeating the process to finish three-soaking and three-rolling, controlling the rolling residual rate at 45%, and drying at 80 ℃ to obtain the antibacterial thermal insulating flocculus.
Wherein the dosage ratio of the semi-finished product to the first treatment liquid to the second treatment liquid is 1g:10mL of: 10mL, the second treatment liquid was prepared from the antibacterial particles of example 2, distilled water and the penetrant JFC-1 in a mass ratio of 13:110:2.5 mixing.
The fiber fineness of the three-dimensional curled hollow polyester fiber is 2.4dtex, the length of the three-dimensional curled hollow polyester fiber is 6cm, the fiber fineness of the viscose fiber is 2.2dtex, the length of the viscose fiber is 8.5cm, the fiber fineness of the cotton fiber is 2.4dtex, and the length of the cotton fiber is 2cm.
Example 5
An antibacterial warming flocculus is prepared by processing fiber raw material and soaking in antibacterial solution.
The preparation process of the antibacterial warm-keeping flocculus comprises the following steps:
step one, uniformly mixing viscose fibers, cotton fibers and three-dimensional curled hollow polyester fibers, and then opening and carding to obtain a fiber net; rearranging the fiber nets by using a disordered roller to enable the fiber nets to form a criss-cross crossed structure, then sending the fiber nets into a lapping machine for lapping to obtain fiber flocculus, and reinforcing the fiber flocculus through needling to obtain a semi-finished product;
and secondly, adding a coupling agent KH-560 into a 90wt% ethanol solution to ensure that the mass fraction of KH-560 is 1.5% to obtain a first treatment solution, soaking the semi-finished product in the first treatment solution for 10min, taking out, drying at 60 ℃, soaking in a second treatment solution for 10min, rolling to remove residual liquid, repeating the process to complete three-soaking and three-rolling, controlling the rolling residual rate at 50%, and drying at 80 ℃ to obtain the antibacterial thermal insulating flocculus.
Wherein the dosage ratio of the semi-finished product to the first treatment liquid to the second treatment liquid is 1g:10mL of: 10mL, and the second treatment liquid was prepared from the antibacterial particles of example 3, distilled water, and a penetrant JFC-1 in a mass ratio of 15:120:3, and mixing.
The fiber fineness of the three-dimensional curled hollow polyester fiber is 2.4dtex, the length of the three-dimensional curled hollow polyester fiber is 4cm, the fiber fineness of the viscose fiber is 1.8dtex, the length of the viscose fiber is 8.5cm, the fiber fineness of the cotton fiber is 2.4dtex, and the length of the cotton fiber is 2cm.
Comparative example 4
The antibacterial particles in example 4 were replaced with the substances in comparative example 1, and the rest of the raw materials and the preparation process were the same as in example 4.
Comparative example 5
The antibacterial particles of example 5 were substituted for the material of comparative example 2, and the remaining raw materials and preparation process were the same as example 5.
Comparative example 6
The antibacterial particles in example 5 were replaced with the substances in comparative example 3, and the rest of the raw materials and the preparation process were the same as in example 5.
The batts prepared in examples 3-5 and comparative examples 4-6 were tested according to GB/T20944.3-2008, evaluation of antibacterial properties of textiles section 3: the oscillating method tests the bacteriostatic rates of staphylococcus aureus and escherichia coli, the wadding of the examples and the comparative examples are respectively washed 30 times when the washing fastness is tested, the bacteriostatic rates of the staphylococcus aureus and the escherichia coli are tested again, and the test results are shown in table 1:
TABLE 1
Figure BDA0003840924890000091
As can be seen from Table 1, the batts prepared in examples 3-5 have superior antimicrobial properties and high wash fastness compared to comparative examples 4-6.
In the description of the specification, reference to the description of "one embodiment," "an example," "a specific example" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only, and it will be appreciated by those skilled in the art that various modifications, additions and substitutions can be made to the embodiments described without departing from the scope of the invention as defined in the appended claims.

Claims (6)

1. A preparation process of an antibacterial warm-keeping flocculus is characterized by comprising the following steps:
firstly, mixing viscose fibers, cotton fibers and three-dimensional curled hollow polyester fibers, and then opening and carding to obtain a fiber net; rearranging the fiber nets, then sending the fiber nets into a lapping machine for lapping to obtain fiber flocculus, and carrying out needling reinforcement to obtain a semi-finished product;
secondly, adding a coupling agent KH-560 into an ethanol solution to enable the mass fraction of KH-560 to be 1.3-1.5% to obtain a first treatment solution, soaking the semi-finished product in the first treatment solution, taking out, drying at 60 ℃, soaking in a second treatment solution for 10min, rolling off residual liquid, repeating the process to finish three-soaking and three-rolling, and drying at 80 ℃ to obtain the antibacterial thermal insulation flocculus;
wherein the dosage ratio of the semi-finished product to the first treatment liquid to the second treatment liquid is 1g:10mL of: 10mL, wherein the second treatment liquid is prepared from antibacterial particles, distilled water and a penetrating agent JFC-1 according to the mass ratio of 10-15:100-120:2-3, and mixing.
2. The process for preparing the antibacterial warm-keeping flocculus according to claim 1, wherein the antibacterial particles are prepared by the following steps:
ultrasonically dispersing graphene oxide in distilled water, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, stirring, adding modified chitosan oligosaccharide, magnetically stirring at 60 ℃ for reacting for 1-1.5h, and performing post-treatment to obtain the antibacterial particles.
3. The preparation process of the antibacterial warm-keeping wadding sheet according to claim 2, wherein the mass ratio of the graphene oxide to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide to the modified chitosan oligosaccharide is 1:0.2:0.4-0.5:1.5-2.0.
4. The process for preparing the antibacterial warm-keeping flocculus according to claim 2, wherein the modified chitosan oligosaccharide is prepared by the following steps:
step S21, under the ice bath condition, adding chitosan oligosaccharide into methanesulfonic acid, and stirring for reaction for 30-60min to obtain amino-protected chitosan oligosaccharide;
step S22, putting (3-carboxypropyl) triphenyl phosphonium bromide into a round-bottom flask, and adding SOCl 2 Stirring and reacting for 5-6h at 60 ℃, and performing post-treatment to obtain acyl chloride quaternary phosphonium salt;
step S23, mixing the amino protective shell oligosaccharide, the acyl chloride quaternary phosphonium salt and the anhydrous DMF, reacting for 4-6h at room temperature, and performing post-treatment to obtain grafted chitosan;
and S24, adding the grafted chitosan oligosaccharide into deionized water, stirring to completely dissolve the grafted chitosan oligosaccharide, adjusting the pH value to 8.0 by using ammonia water, centrifuging, washing and drying the precipitate to obtain the modified chitosan oligosaccharide.
5. The process for preparing the antibacterial thermal insulating flocculus according to claim 4, wherein in the step S23, the ratio of the dosage of the amino protective shell oligosaccharide to the dosage of the acyl chloride quaternary phosphonium salt to the dosage of the anhydrous DMF is 15.4-16.7g:0.86-0.95g:200-250mL.
6. An antibacterial thermal insulating wadding, characterized in that it is produced by the process according to any one of claims 1 to 5.
CN202211104406.5A 2022-09-09 2022-09-09 Antibacterial warm-keeping flocculus and preparation process thereof Pending CN115613211A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116695332A (en) * 2023-08-04 2023-09-05 常州赛凡寝具科技有限公司 Preparation method of plant extract modified polyester fiber mat

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116695332A (en) * 2023-08-04 2023-09-05 常州赛凡寝具科技有限公司 Preparation method of plant extract modified polyester fiber mat
CN116695332B (en) * 2023-08-04 2023-10-13 常州赛凡寝具科技有限公司 Preparation method of plant extract modified polyester fiber mat

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