CN112874050A - Efficient antibacterial fabric and preparation method thereof - Google Patents
Efficient antibacterial fabric and preparation method thereof Download PDFInfo
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- CN112874050A CN112874050A CN202110071184.0A CN202110071184A CN112874050A CN 112874050 A CN112874050 A CN 112874050A CN 202110071184 A CN202110071184 A CN 202110071184A CN 112874050 A CN112874050 A CN 112874050A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/02—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising animal or vegetable substances, e.g. cork, bamboo, starch
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/022—Non-woven fabric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/047—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material made of fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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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
- D04H1/40—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
- D04H1/425—Cellulose series
- D04H1/4258—Regenerated cellulose series
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- 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
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- 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
- D06M11/32—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
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
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- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/04—Cellulosic plastic fibres, e.g. rayon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
- B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/718—Weight, e.g. weight per square meter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/06—Pectin; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
Abstract
The invention discloses a high-efficiency antibacterial fabric and a preparation method thereof. The antibacterial property of the nano titanium dioxide subjected to super-strong acidification is enhanced, the surface hydroxyl groups are increased, the nano titanium dioxide can be more fully modified by ferric acetylacetonate, and the nano titanium dioxide has a high-efficiency antibacterial effect; pectin and modified chitosan blend film-forming cladding are in the surface fabric outside, and the activity of photocatalysis is accelerated for antibacterial capacity strengthens, still makes the nanometer titanium dioxide who soaks on the surface fabric even drop and also can continue to carry out antibacterial action on the pectin membrane, has guaranteed that surface fabric antibacterial property is lasting, uses NMMO to dissolve regenerated cellulose fibre, carries out 3D and prints for criss-cross woven structure as the basic unit, and not only more frivolous is also stronger to nanometer titanium dioxide's adsorption affinity.
Description
Technical Field
The invention relates to the field of fabrics, in particular to a high-efficiency antibacterial fabric and a preparation method thereof.
Background
The bacteria, as a type of microorganisms most widely distributed in the human living environment, are ubiquitous, and have a wide variety, strong adaptability and quick reproductive capacity. Especially some harmful pathogenic bacteria seriously threaten human health, not only aggravate wound infection and disease deterioration through direct contact, but also cause diseases by polluting surrounding environments, such as water, food, clothes and the like, and invading human bodies.
The textile is used as a functional article essential for human life, and due to the microporous structure of the textile, the textile is very easy to adsorb and contaminate microorganisms, and in addition, the proper temperature and humidity, secreted grease, sweat and the like on the surface of a human body create favorable conditions for the propagation and breeding of the microorganisms under certain special conditions. Therefore, the research on the antibacterial fabric has a very large development prospect. Therefore, the preparation of the high-efficiency antibacterial fabric is very necessary.
Disclosure of Invention
The invention aims to provide a high-efficiency antibacterial fabric to solve the problems in the background technology.
In order to solve the above technical problem, a first aspect of the present invention provides the following technical solutions: the efficient antibacterial fabric is characterized by comprising the following raw materials in parts by weight:
50-100 parts of regenerated cellulose fiber, 5-10 parts of modified nano titanium dioxide, 5-10 parts of pectin, 5-10 parts of modified chitosan, 5-10 parts of modified pectin film, 20-30 parts of NMMO solution and 5-10 parts of iron acetylacetonate.
Preferably, the modified nano titanium dioxide is prepared by performing super-strong acidification on nano titanium dioxide and then modifying the nano titanium dioxide by using ferric acetylacetonate.
Preferably, the modified chitosan is prepared by grafting 1-hydroxymethyl-5, 5-dimethylhydantoin on the surface of chitosan.
Preferably, the modified pectin film is prepared by blending pectin and modified chitosan.
The second aspect of the present invention provides: a preparation method of a high-efficiency antibacterial fabric is characterized by comprising the following steps:
the process flow is as follows:
preparing modified nano titanium dioxide, preparing a modified pectin film, preparing a base layer, soaking and soaking the fabric, and coating the fabric.
Preferably, the method comprises the following specific steps:
(1) placing nano titanium dioxide in a beaker, adding hydrofluoric acid, slowly stirring for 24 hours, filtering, washing for 3-5 times by using absolute ethyl alcohol, mixing the washed nano titanium dioxide with iron acetylacetonate, placing in a round bottom flask, adding excessive absolute ethyl alcohol, magnetically stirring for 0.5 hour, then performing ultrasonic treatment for 20 minutes, placing in a constant-temperature oil bath, stirring and adsorbing for 2 hours, and preparing modified nano titanium dioxide for later use;
(2) weighing chitosan and adding acetic acid into a single-neck flask for dissolving, then adding 1-hydroxymethyl-5, 5-dimethylhydantoin, placing the single-neck flask in a 100 ℃ oil bath environment for reaction, stirring, condensing and refluxing, reacting for 24 hours, slightly cooling the solution after the reaction is finished, and removing the solvent through reduced pressure distillation to obtain a viscous product;
(3) dropwise adding the viscous product into an acetone solution by using a dropper, stirring until the solution is milky, removing a flocculent product, replacing the acetone solution, repeating the operation until the viscous product is completely dropwise added, carrying out suction filtration and washing on the obtained solid matter for 3-5 times by using acetone and ethanol on a suction filtration device, and carrying out vacuum drying on the product for 48 hours at 45 ℃ after renting to obtain the modified chitosan;
(4) preparing a 1.0% modified chitosan acetic acid solution by using 1.0% acetic acid, adding a 4.0% pectin solution, stirring for 2h, washing the obtained white flocculent precipitate to be neutral, dissolving the white flocculent precipitate by using formic acid with the pH value of 1, filtering, coating, and drying at 45 ℃ to obtain a modified pectin film;
(5) preparing an NMMO solution with the mass fraction of 85%, dissolving regenerated cellulose fibers, and printing the fiber solution into a fabric base layer with a criss-cross structure by using a 3D printer;
(6) soaking the fabric base layer in the modified nano titanium dioxide solution for 10-20 min, and drying at 80 ℃;
(7) and (5) coating the dried fabric with the modified pectin film prepared in the step (4) to obtain a finished product.
Preferably, in the step (1): the mass ratio of the nano titanium dioxide to the acetylacetone iron is 4: 1.
preferably, in the step (2): the mass ratio of the chitosan to the 1-hydroxymethyl-5, 5-dimethyl hydantoin is 1: 1.
preferably, in the step (4): the mass ratio of the modified chitosan to the pectin is 1: 1.
preferably, in the step (5): the printing parameters were layer thickness 0.1cm, travel speed 30mm/s, and motion trajectory for the scan.
Compared with the prior art, the invention has the following beneficial effects:
the nanometer titanium dioxide is firstly subjected to super-strong acidification, so that surface electrons are influenced, and simultaneously, crystal phase transformation is effectively inhibited, the forbidden bandwidth of the titanium dioxide is increased, and the redox capability of photo-generated electrons-holes is enhanced; the super acid center formed by the synergistic action of the super acid and the ortho acid generated by the super acid enhances the surface acidity and O of the titanium dioxide again2、O2-And O-The adsorption quantity effectively reduces the recombination of photoinduced electrons and holes, and the photoinduced electrons are adsorbed on the surface of the fabric after being soaked, so that the antibacterial capacity of the fabric is enhanced; the nanometer titanium dioxide subjected to super-strong acidification is modified by ferric acetylacetonate, so that the antibacterial property of the nanometer titanium dioxide subjected to super-strong acidification is enhanced, the surface hydroxyl groups are increased, the modification reaction is more sufficient, the agglomeration is reduced, the photocatalytic activity can be greatly improved, and the fabric soaked by the modified nanometer titanium dioxide under irradiation has high-efficiency antibacterial performance.
After the fabric is soaked, an antibacterial film is used for coating, so that a layer of antibacterial coating film is formed on the outer side of the soaked fabric, pectin has antibacterial property and good film forming property, but the mechanical property is low, after the modified chitosan is added, the tensile property of a pectin film can be enhanced, the air permeability is reduced, and a heat-insulating effect is achieved under illumination, the photocatalytic activity is accelerated, so that the antibacterial ability is enhanced, in addition, the modified chitosan is a chitosan halamine compound, and the halogen atoms have positive charges and have oxidability, so that the halamine compound has the advantages of high sterilization speed, durability of the antibacterial property and reproducibility of the antibacterial function, after the halamine compound is grafted onto a chitosan molecular chain, the antibacterial effect of the chitosan can be greatly improved, the chitosan halamine compound is compounded with the pectin to form a film, the antibacterial effect is further achieved, and the antibacterial effect can be continuously achieved on the pectin film even if the nano titanium dioxide soaked on the fabric falls off, the antibacterial property of the fabric is ensured to be lasting.
Preparing a base layer by using natural fiber dissolution and regeneration for 3D printing to prepare the antibacterial fabric; the regenerated cellulose fibers are dissolved by NMMO, 3D printing is carried out to form a criss-cross woven structure as a base layer, the base layer fabric after 3D printing is lighter and thinner, the adsorption force on nano titanium dioxide is stronger, and the fabric finally prepared through soaking and coating of the antibacterial film has the best wearability and high-efficiency antibacterial performance.
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.
The efficient antibacterial fabric is characterized by comprising the following raw materials in parts by weight:
50-100 parts of regenerated cellulose fiber, 5-10 parts of modified nano titanium dioxide, 5-10 parts of pectin, 5-10 parts of modified chitosan, 5-10 parts of modified pectin film, 20-30 parts of NMMO solution and 5-10 parts of iron acetylacetonate.
Preferably, the modified nano titanium dioxide is prepared by performing super-strong acidification on nano titanium dioxide and then modifying the nano titanium dioxide by using ferric acetylacetonate.
Preferably, the modified chitosan is prepared by grafting 1-hydroxymethyl-5, 5-dimethylhydantoin on the surface of chitosan.
Preferably, the modified pectin film is prepared by blending pectin and modified chitosan.
The second aspect of the present invention provides: a preparation method of a high-efficiency antibacterial fabric is characterized by comprising the following steps:
the process flow is as follows:
preparing modified nano titanium dioxide, preparing a modified pectin film, preparing a base layer, soaking and soaking the fabric, and coating the fabric.
Preferably, the method comprises the following specific steps:
(1) placing nano titanium dioxide in a beaker, adding hydrofluoric acid, slowly stirring for 24 hours, filtering, washing for 3-5 times by using absolute ethyl alcohol, mixing the washed nano titanium dioxide with iron acetylacetonate, placing in a round bottom flask, adding excessive absolute ethyl alcohol, magnetically stirring for 0.5 hour, then performing ultrasonic treatment for 20 minutes, placing in a constant-temperature oil bath, stirring and adsorbing for 2 hours, and preparing modified nano titanium dioxide for later use;
(2) weighing chitosan and adding acetic acid into a single-neck flask for dissolving, then adding 1-hydroxymethyl-5, 5-dimethylhydantoin, placing the single-neck flask in a 100 ℃ oil bath environment for reaction, stirring, condensing and refluxing, reacting for 24 hours, slightly cooling the solution after the reaction is finished, and removing the solvent through reduced pressure distillation to obtain a viscous product;
(3) dropwise adding the viscous product into an acetone solution by using a dropper, stirring until the solution is milky, removing a flocculent product, replacing the acetone solution, repeating the operation until the viscous product is completely dropwise added, carrying out suction filtration and washing on the obtained solid matter for 3-5 times by using acetone and ethanol on a suction filtration device, and carrying out vacuum drying on the product for 48 hours at 45 ℃ after renting to obtain the modified chitosan;
(4) preparing a 1.0% modified chitosan acetic acid solution by using 1.0% acetic acid, adding a 4.0% pectin solution, stirring for 2h, washing the obtained white flocculent precipitate to be neutral, dissolving the white flocculent precipitate by using formic acid with the pH value of 1, filtering, coating, and drying at 45 ℃ to obtain a modified pectin film;
(5) preparing an NMMO solution with the mass fraction of 85%, dissolving regenerated cellulose fibers, and printing the fiber solution into a fabric base layer with a criss-cross structure by using a 3D printer;
(6) soaking the fabric base layer in the modified nano titanium dioxide solution for 10-20 min, and drying at 80 ℃;
(7) and (5) coating the dried fabric with the modified pectin film prepared in the step (4) to obtain a finished product.
Preferably, in the step (1): the mass ratio of the nano titanium dioxide to the acetylacetone iron is 4: 1.
preferably, in the step (2): the mass ratio of the chitosan to the 1-hydroxymethyl-5, 5-dimethyl hydantoin is 1: 1.
preferably, in the step (4): the mass ratio of the modified chitosan to the pectin is 1: 1.
preferably, in the step (5): the printing parameters were layer thickness 0.1cm, travel speed 30mm/s, and motion trajectory for the scan.
Example 1: the high-efficiency antibacterial fabric I comprises the following steps:
a high-efficiency antibacterial fabric comprises the following components in parts by weight:
the weight fraction of the regenerated cellulose fiber is 50 parts, the weight fraction of the modified nano titanium dioxide is 5 parts, the weight fraction of the pectin is 5 parts, the weight fraction of the modified chitosan is 5 parts, the weight fraction of the modified pectin film is 5 parts, the weight fraction of the NMMO solution is 20 parts, and the weight fraction of the iron acetylacetonate is 5 parts.
The preparation method of the fabric comprises the following steps:
(1) placing 5 parts by weight of nano titanium dioxide in a beaker, adding hydrofluoric acid, slowly stirring for 24 hours, filtering, washing for 3 times by using absolute ethyl alcohol, mixing the washed nano titanium dioxide with iron acetylacetonate, placing the mixture in the round-bottom flask, wherein the mass ratio of the nano titanium dioxide to the iron acetylacetonate is 4: 1, adding excessive absolute ethyl alcohol, carrying out magnetic stirring for 0.5h, then carrying out ultrasonic treatment for 20min, and then placing in a constant-temperature oil bath for stirring and adsorption for 2h to prepare modified nano titanium dioxide for later use;
(2) weighing 5 parts by weight of chitosan and acetic acid in a single-neck flask for dissolving, and then adding 1-hydroxymethyl-5, 5-dimethyl hydantoin, wherein the mass ratio of the chitosan to the 1-hydroxymethyl-5, 5-dimethyl hydantoin is 1: 1, placing a single-neck flask in an oil bath environment at 100 ℃ for reaction, stirring, condensing and refluxing, reacting for 24 hours, slightly cooling the solution after the reaction is finished, and removing the solvent by reduced pressure distillation to obtain a viscous product;
(3) dropwise adding the viscous product into an acetone solution by using a dropper, stirring until the solution is milky, removing the flocculent product, replacing the acetone solution, repeating the operation until the viscous product is completely dropwise added, carrying out suction filtration and washing on the obtained solid matter for 3 times by using acetone and ethanol on a suction filtration device, and carrying out vacuum drying on the product for 48 hours at 45 ℃ after renting to obtain the modified chitosan;
(4) preparing a 1.0% modified chitosan acetic acid solution by using 1.0% acetic acid, adding a 4.0% pectin solution, wherein the mass ratio of the modified chitosan to the pectin is 1: 1, stirring for 2 hours, washing the obtained white flocculent precipitate to be neutral, dissolving the white flocculent precipitate by formic acid with pH value of 1, filtering, coating, and drying at 45 ℃ to obtain a modified pectin film;
(5) preparing NMMO solution with the mass fraction of 85%, dissolving regenerated cellulose fibers, and printing the fiber solution into a fabric substrate with a criss-cross structure by using a 3D printer, wherein the printing parameters are the layer thickness of 0.1cm, the moving speed of 30mm/s, and the motion trajectory is in an enhanced cross;
(6) soaking the fabric base layer in the modified nano titanium dioxide solution for 10min, and drying at 80 ℃;
(7) and (5) coating the dried fabric with the modified pectin film prepared in the step (4) to obtain a finished product.
Example 2: and (2) efficient antibacterial fabric II:
a high-efficiency antibacterial fabric comprises the following components in parts by weight:
the weight fraction of the regenerated cellulose fiber is 100 parts, the weight fraction of the modified nano titanium dioxide is 10 parts, the weight fraction of the pectin is 10 parts, the weight fraction of the modified chitosan is 10 parts, the weight fraction of the modified pectin film is 5 parts, the weight fraction of the NMMO solution is 30 parts, and the weight fraction of the iron acetylacetonate is 10 parts.
The preparation method of the fabric comprises the following steps:
(1) placing 10 parts by weight of nano titanium dioxide in a beaker, adding hydrofluoric acid, slowly stirring for 24 hours, filtering, washing for 3 times by using absolute ethyl alcohol, mixing the washed nano titanium dioxide with iron acetylacetonate, placing the mixture in the round-bottom flask, wherein the mass ratio of the nano titanium dioxide to the iron acetylacetonate is 4: 1, adding excessive absolute ethyl alcohol, carrying out magnetic stirring for 0.5h, then carrying out ultrasonic treatment for 20min, and then placing in a constant-temperature oil bath for stirring and adsorption for 2h to prepare modified nano titanium dioxide for later use;
(2) weighing 10 parts by weight of chitosan and acetic acid into a single-neck flask for dissolving, and then adding 1-hydroxymethyl-5, 5-dimethyl hydantoin, wherein the mass ratio of the chitosan to the 1-hydroxymethyl-5, 5-dimethyl hydantoin is 1: 1, placing a single-neck flask in an oil bath environment at 100 ℃ for reaction, stirring, condensing and refluxing, reacting for 24 hours, slightly cooling the solution after the reaction is finished, and removing the solvent by reduced pressure distillation to obtain a viscous product;
(3) dropwise adding the viscous product into an acetone solution by using a dropper, stirring until the solution is milky, removing the flocculent product, replacing the acetone solution, repeating the operation until the viscous product is completely dropwise added, carrying out suction filtration and washing on the obtained solid matter for 5 times by using acetone and ethanol on a suction filtration device, and carrying out vacuum drying on the product for 48 hours at 45 ℃ after renting to obtain the modified chitosan;
(4) preparing a 1.0% modified chitosan acetic acid solution by using 1.0% acetic acid, adding a 4.0% pectin solution, wherein the mass ratio of the modified chitosan to the pectin is 1: 1, stirring for 2 hours, washing the obtained white flocculent precipitate to be neutral, dissolving the white flocculent precipitate by formic acid with pH value of 1, filtering, coating, and drying at 45 ℃ to obtain a modified pectin film;
(5) preparing NMMO solution with the mass fraction of 85%, dissolving regenerated cellulose fibers, and printing the fiber solution into a fabric substrate with a criss-cross structure by using a 3D printer, wherein the printing parameters are the layer thickness of 0.1cm, the moving speed of 30mm/s, and the motion trajectory is in an enhanced cross;
(6) soaking the fabric base layer in the modified nano titanium dioxide solution for 20min, and drying at 80 ℃;
(7) and (5) coating the dried fabric with the modified pectin film prepared in the step (4) to obtain a finished product.
Comparative example 1
The formulation of comparative example 1 was the same as example 1. The preparation method of the antibacterial fabric is different from that of the example 1 only in that the step (1) is not carried out, the step (6) is directly prepared by using unmodified nano titanium dioxide, and the rest preparation steps are the same as those of the example 1.
Comparative example 2
Comparative example 2 was formulated as in example 1. The preparation method of the antibacterial fabric is different from that of the antibacterial fabric in example 1 only in that the steps (2), (3), (4) and (7) are not carried out, and the rest of the preparation steps are the same as those of the antibacterial fabric in example 1.
Comparative example 3
The formulation of comparative example 3 was the same as example 1. The preparation method of the antibacterial fabric is different from that of the embodiment 1 only in the step (5), and the step (5) is replaced by the step of preparing the fabric by spinning the regenerated cellulose fibers. The rest of the preparation steps are the same as example 1.
Test example 1
1. Test method
Example 1 and comparative examples 1, 2 and 3 are control tests, and the national standard GB/T20994.3-2008, evaluation part 3 of antibacterial performance of textiles: the oscillating method carries out antibacterial property quantitative test on the antibacterial fabric, tests the antibacterial rate of the fiber without water washing, and comprises the following steps: coli ATCC11229, klebsiella pneumoniae ATCC 4352.
2. Test results
The bacteriostatic rate of the example 1 is compared with that of the comparative examples 1 and 2.
TABLE 1 antibacterial Rate
| Escherichia coli ATCC11229 | Klebsiella pneumoniae ATCC4352 | |
| Example 1 | 67.9 | 95.3 |
| Comparative example 1 | 44.2 | 71.9 |
| Comparative example 2 | 43.6 | 65.4 |
| Comparative example 3 | 58.2 | 73.6 |
Compared with the bacteriostatic rates of comparative examples 1, 2 and 3, the bacteriostatic fabric prepared in example 1 has higher bacteriostatic ability, which indicates that the modified nano titanium dioxide, the antibacterial film and the base layer prepared by 3D printing can increase the bacteriostatic rate of the bacteriostatic fabric to different degrees, and indicates that the high-efficiency bacteriostatic fabric prepared in the invention has excellent bacteriostatic performance.
Test example 2
1. Test method
Example 1 and comparative examples 1, 2 and 3 are control tests, and after the example 1 and the comparative examples 1 and 2 are washed 3 times, the national standard GB/T20994.3-2008, evaluation part 3 of antibacterial performance of textiles: the oscillating method carries out antibacterial property quantitative test on the antibacterial fabric, tests the antibacterial rate of the fiber without water washing, and comprises the following steps: coli ATCC11229, klebsiella pneumoniae ATCC 4352.
2. Test results
The bacteriostatic rate of example 1 is compared with that of comparative examples 1 and 2 after multiple times of washing.
Table 2 antibacterial rate of antibacterial fabric after 3 times of washing
| Escherichia coli ATCC11229 | Klebsiella pneumoniae ATCC4352 | |
| Example 1 | 67.7 | 92.3 |
| Comparative example 1 | 40.2 | 65.9 |
| Comparative example 2 | 23.6 | 49.4 |
| Comparative example 3 | 54.3 | 70.9 |
By comparing the bacteriostasis rates of the embodiment 1 and the antibacterial fabrics of the comparative examples 1, 2 and 3 after 3 times of cleaning, the influence of the bacteriostasis rate of the embodiment 1 is not greatly changed, which shows that the high-efficiency antibacterial fabric prepared by the invention has lasting bacteriostasis capability, and indicates that the high-efficiency antibacterial fabric prepared by the invention has excellent bacteriostasis performance and lasting bacteriostasis capability.
Test example 3
1. Test method
Example 1 and comparative example 3 are control tests, and example 1 and comparative example 3 are weighed and compared.
2. Test results
Example 1 was compared to comparative example 3 by weight.
TABLE 3 weights
| Weight (D) | |
| Example 1 | 9.7g |
| Comparative example 3 | 15.3g |
Compared with the comparative example 3, the antibacterial fabric prepared in the example 1 is obviously lighter, and the fact that the fabric base layer prepared by 3D printing has higher wearability is proved, which indicates that the efficient antibacterial fabric prepared by the invention has excellent antibacterial performance, light weight and excellent performance.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The efficient antibacterial fabric is characterized by comprising the following raw materials in parts by weight: 50-100 parts of regenerated cellulose fiber, 5-10 parts of modified nano titanium dioxide, 5-10 parts of pectin, 5-10 parts of modified chitosan, 5-10 parts of modified pectin film, 20-30 parts of NMMO solution and 5-10 parts of iron acetylacetonate.
2. The efficient bacteriostatic fabric according to claim 1, which is characterized in that: the modified nano titanium dioxide is prepared by performing super-strong acidification on nano titanium dioxide and then modifying the nano titanium dioxide by using ferric acetylacetonate.
3. The efficient bacteriostatic fabric according to claim 1, which is characterized in that: the modified chitosan is prepared by grafting 1-hydroxymethyl-5, 5-dimethylhydantoin on the surface of chitosan.
4. The efficient bacteriostatic fabric according to claim 1, which is characterized in that: the modified pectin film is prepared by blending pectin and modified chitosan.
5. The preparation method of the high-efficiency antibacterial fabric is characterized in that the process flow for preparing the antibacterial fabric is as follows: preparing modified nano titanium dioxide, preparing a modified pectin film, preparing a base layer, soaking and soaking the fabric, and coating the fabric.
6. The preparation method of the efficient bacteriostatic fabric according to claim 5, characterized by comprising the following specific steps:
(1) placing nano titanium dioxide in a beaker, adding hydrofluoric acid, slowly stirring for 24 hours, filtering, washing for 3-5 times by using absolute ethyl alcohol, mixing the washed nano titanium dioxide with iron acetylacetonate, placing in a round bottom flask, adding excessive absolute ethyl alcohol, magnetically stirring for 0.5 hour, then performing ultrasonic treatment for 20 minutes, placing in a constant-temperature oil bath, stirring and adsorbing for 2 hours, and preparing modified nano titanium dioxide for later use;
(2) weighing chitosan and adding acetic acid into a single-neck flask for dissolving, then adding 1-hydroxymethyl-5, 5-dimethylhydantoin, placing the single-neck flask in a 100 ℃ oil bath environment for reaction, stirring, condensing and refluxing, reacting for 24 hours, slightly cooling the solution after the reaction is finished, and removing the solvent through reduced pressure distillation to obtain a viscous product;
(3) dropwise adding the viscous product into an acetone solution by using a dropper, stirring until the solution is milky, removing a flocculent product, replacing the acetone solution, repeating the operation until the viscous product is completely dropwise added, carrying out suction filtration and washing on the obtained solid matter for 3-5 times by using acetone and ethanol on a suction filtration device, and carrying out vacuum drying on the product for 48 hours at 45 ℃ after renting to obtain the modified chitosan;
(4) preparing a 1.0% modified chitosan acetic acid solution by using 1.0% acetic acid, adding a 4.0% pectin solution, stirring for 2h, washing the obtained white flocculent precipitate to be neutral, dissolving the white flocculent precipitate by using formic acid with the pH value of 1, filtering, coating, and drying at 45 ℃ to obtain a modified pectin film;
(5) preparing an NMMO solution with the mass fraction of 85%, dissolving regenerated cellulose fibers, and printing the fiber solution into a fabric base layer with a criss-cross structure by using a 3D printer;
(6) soaking the fabric base layer in the modified nano titanium dioxide solution for 10-20 min, and drying at 80 ℃;
(7) and (5) coating the dried fabric with the modified pectin film prepared in the step (4) to obtain a finished product.
7. The preparation method of the efficient bacteriostatic fabric according to claim 6, characterized in that in the step (1): the mass ratio of the nano titanium dioxide to the acetylacetone iron is 4: 1.
8. the preparation method of the efficient bacteriostatic fabric according to claim 6, characterized in that in the step (2): the mass ratio of the chitosan to the 1-hydroxymethyl-5, 5-dimethyl hydantoin is 1: 1.
9. the preparation method of the high-efficiency bacteriostatic fabric according to claim 6, characterized in that in the step (4): the mass ratio of the modified chitosan to the pectin is 1: 1.
10. the preparation method of the high-efficiency bacteriostatic fabric according to claim 6, characterized in that in the step (5): the printing parameters were layer thickness 0.1cm, travel speed 30mm/s, and motion trajectory for the scan.
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