CN114775095B - Antibacterial, mildew-proof, aldehyde-removing and odor-removing multifunctional soft chip and preparation method thereof - Google Patents
Antibacterial, mildew-proof, aldehyde-removing and odor-removing multifunctional soft chip and preparation method thereof Download PDFInfo
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- CN114775095B CN114775095B CN202210524978.2A CN202210524978A CN114775095B CN 114775095 B CN114775095 B CN 114775095B CN 202210524978 A CN202210524978 A CN 202210524978A CN 114775095 B CN114775095 B CN 114775095B
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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
- D01D5/247—Discontinuous hollow structure or microporous structure
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- 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
- D04H1/4391—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 characterised by the shape of the fibres
- D04H1/43916—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 characterised by the shape of the fibres microcellular fibres, e.g. porous or foamed fibres
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- 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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/542—Adhesive fibres
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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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/558—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 by welding together the fibres, e.g. by partially melting or dissolving in combination with mechanical or physical treatments other than embossing
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- 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
- D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
- D04H1/559—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 by welding together the fibres, e.g. by partially melting or dissolving the fibres being within layered webs
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- 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
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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Abstract
The invention belongs to the technical field of functional fiber materials, and discloses an antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip and a preparation method thereof. Adding the silicon dioxide aerogel microspheres into an inorganic antibacterial metal salt solution containing calcium acetate for adsorption treatment, then adding the silicon dioxide aerogel microspheres into a dilute alkali solution for soaking reaction, and washing and drying the product to obtain pore-forming antibacterial particles; mixing the obtained pore-forming antibacterial particles, inorganic aldehyde-removing deodorizing powder and a fiber base material, and performing solution spinning to obtain nascent fiber; carrying out steam heat treatment on the nascent fiber at 160-190 ℃, and carrying out vacuum drying to obtain porous fiber; and finally, weaving, forming, softening and finishing to obtain the multifunctional soft chip with the functions of antibiosis, mildew prevention, aldehyde removal and deodorization. The invention overcomes the defects of poor softness, bulkiness and air permeability of the conventional fiber added with inorganic functional materials and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of functional fiber materials, and particularly relates to an antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip and a preparation method thereof.
Background
The antibacterial and mildewproof fiber is prepared by compounding an antibacterial material and a fiber material, has the functions of resisting bacteria, killing bacteria and preventing mildew, and can prevent infection and infection. The conventional preparation methods include a mixing method and a post-treatment method. The mixing method is that inorganic antibacterial powder material containing silver, copper, zinc and other elements is mixed into polyester, polyamide, polyacrylonitrile and other materials for spinning; the post-treatment method is to dip the formed fiber material with quaternary ammonium salt antibacterial agent or organic antibacterial agent such as fatty imide.
For example, patent CN 112226847A discloses a durable antibacterial and mildewproof fiber, which comprises activated carbon fiber, nano-scale antibacterial agent and polyacrylonitrile; the weight parts of the raw materials are as follows: 15-30 parts of active carbon fiber, 60-70 parts of polyacrylonitrile, and the nano-scale antibacterial agent accounts for 3-8% of the weight of the active carbon fiber. The nano-scale antibacterial agent is at least one of nano-silver, nano-titanium oxide and nano-zinc oxide.
In the former patent CN 111519341B, we disclose a method for preparing a compound antiviral and antibacterial multifunctional PP, PE, PET nonwoven fabric. Adding the silica aerogel microspheres adsorbed with inorganic antibacterial metal ions (such as silver, copper and zinc ions) into a dilute alkali solution for soaking reaction, washing, drying, optionally thermally decomposing, and grinding to obtain inorganic antibacterial particles. The inorganic antibacterial particles are introduced into the fiber matrix to achieve the corresponding antibacterial effect.
The aldehyde-removing deodorizing fiber is made by compounding aldehyde-removing deodorizing material and fiber material, and its conventional preparation method also includes mixing method and post-treatment method. The mixing method is to adopt the materials for removing aldehyde and odor to produce by a blending spinning method; the post-treatment method is to adopt a formaldehyde-removing and odor-eliminating finishing agent and produce the fabric through dyeing, finishing and processing.
In the former patent CN 113652766B, we disclose a preparation method of a compound deodorizing antibacterial antiviral multifunctional fiber. PVA-SiO coated with traditional Chinese medicine antiviral component and organosilicon quaternary ammonium salt antibacterial agent 2 And carrying out mixed spinning on the interpenetrating network particles and the fiber matrix to obtain a product.
According to the prior art, inorganic functional powder materials are generally required to be utilized in the blending method, but in the actual application process, the soft and fluffy hand feeling and air permeability of the fiber materials added with the inorganic functional powder materials are adversely affected, and in the field of clothing home textile materials, the fluffy, soft and good air permeability use feeling is a great demand of consumers. Therefore, how to realize the antibacterial and deodorant functions of the fiber material and also have good softness and air permeability is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of an antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
The invention also aims to provide the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip comprises the following preparation steps:
(1) Adding the silica aerogel microspheres into an inorganic antibacterial metal salt solution containing calcium acetate for adsorption treatment, then adding the adsorbed silica aerogel microspheres into a dilute alkali solution for soaking reaction, and washing and drying the product to obtain pore-forming antibacterial particles;
(2) Uniformly mixing the pore-forming antibacterial particles obtained in the step (1) with an inorganic aldehyde-removing deodorizing powder material, mixing the mixture with a fiber base material, and then carrying out solution spinning to obtain nascent fiber;
(3) Carrying out steam heat treatment on the nascent fiber obtained in the step (2) at 160-190 ℃, and carrying out vacuum drying to obtain porous fiber;
(4) And (4) weaving and forming the porous fiber obtained in the step (3), and then carrying out softening finishing to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
Further, the particle size range of the silica aerogel microspheres in the step (1) is 20 nm-1.5 μm, and the pore size range is 2-50 nm.
Further preferably, the silica aerogel microspheres in the step (1) refer to silica aerogel microspheres containing carboxyl, which are prepared by the following method:
adjusting the pH value of silica sol to be between 1 and 4 by using an acid solution, then adding 3- [ 3-carboxyl allylamido ] propyl triethoxysilane as a mixed silicon source, stirring and mixing uniformly, continuously stirring and adding absolute ethyl alcohol, adding the obtained mixed solution into an organic solvent, adding an emulsifier for homogenization to obtain an emulsion, then adding ammonia water to adjust the pH value to be between 9 and 11, stirring and mixing uniformly, standing for layering, washing and drying the sediment at the lower layer, and crushing to obtain the silica aerogel microspheres containing carboxyl. The silicon dioxide aerogel microspheres containing carboxyl have better adsorption and fixation performance.
Further, the inorganic antibacterial metal salt solution containing calcium acetate in the step (1) refers to a silver nitrate, copper nitrate or zinc nitrate aqueous solution in which calcium acetate is dissolved; wherein the mass concentration ranges of the calcium acetate and the inorganic antibacterial metal salt are both 0.5-10%.
Further, the adsorption treatment in the step (1) is carried out under the conditions of ultrasound and vacuum stirring, and the adsorption treatment time is 0.5-4 h.
Further, the dilute alkali solution in the step (1) refers to a NaOH solution with the concentration of 0.02-0.05 mol/L.
Further, the drying in the step (1) refers to air drying at the temperature of 100-120 ℃ for 0.5-6 h.
Further, the inorganic aldehyde-removing and deodorizing powder material in the step (2) comprises at least one of nano mineral crystal powder, nano titanium dioxide powder, nano zinc oxide powder and nano diatomite; the particle size range of the inorganic aldehyde-removing and deodorizing powder material is 20 nm-1.5 mu m.
Further, the adding amount of the pore-forming antibacterial particles in the step (2) is 0.2-4% of the mass of the fiber base material; the addition amount of the inorganic aldehyde-removing and deodorizing powder material is 0.5 to 8 percent of the mass of the fiber base material.
Further, the fiber substrate in the step (2) refers to a fiber substrate suitable for solution spinning, such as any one of polyacrylonitrile fiber, polyvinyl alcohol fiber, viscose fiber, acrylic fiber, spandex fiber, polyvinyl chloride fiber, vinylon fiber, polylactic acid fiber, and chitosan fiber.
Further, the solution spinning in the step (2) includes any one of dry spinning, wet spinning and dry-wet spinning.
Further, the steam heat treatment time in the step (3) is 1-6 h.
Further, the temperature of the vacuum drying in the step (3) is 120-140 ℃.
Further, the weaving and forming in the step (4) means that after the porous fibers are loosened, the porous fibers and the low-melting-point bonding fibers are mixed, carded and lapped into sheets in a mode that the middle layer is the low-melting-point bonding fibers and the upper layer and the lower layer are the porous fibers, and then the sheets are pre-bonded and shaped by thermal bonding through physical rolling.
Further, the soft finishing in the step (4) adopts an amino silicone oil emulsion soft finishing agent, and the soft finishing step comprises the following steps: adding the formed fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 0.5-1 h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 70% -80%, then placing the mixture into a drying oven for drying at 85-95 ℃, and shaping for 20-60 s at 150-170 ℃ to obtain the antibacterial, mildew-proof, aldehyde-removing and odor-removing multifunctional soft chip.
An antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip is prepared by the method.
The multifunctional antibacterial, mildewproof, aldehyde-removing and odor-removing soft chip is applied to industrial products such as home furnishings, hotels, nursing homes, mattresses for textiles, automobile seats, outdoor articles and the like.
The principle of the invention is as follows: the pore-forming agent calcium acetate and the inorganic antibacterial metal salt are adsorbed and fixed by the silica aerogel microspheres, then the pore-forming agent calcium acetate and the inorganic antibacterial metal salt are soaked in a dilute alkali solution for reaction and are subsequently dried, and the adsorbed inorganic antibacterial metal salt reacts in situ to generate a non-migratory antibacterial metal oxide so as to improve the uniformity and the stability of the inorganic antibacterial metal oxide in a fiber matrix. Then, the solution spinning is carried out to obtain the nascent fiber. The obtained nascent fiber is subjected to steam heat treatment at 160-190 ℃, in the heat treatment process, a pore-forming agent calcium acetate is subjected to thermal decomposition to form acetone and calcium carbonate, and the acetone escapes from the fiber base material at high temperature to form the porous structure fiber. Compared with common fibers, the porous fiber has better softness and bulkiness, and the strength of the fiber cannot be reduced under the reinforcing effect of the silicon dioxide aerogel microspheres and the nano calcium carbonate generated in situ. In the subsequent softening finishing process, the porous structure fiber has better bonding force with the softening finishing agent, and the softening finishing effect is further obviously enhanced.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, the special pore-foaming agent particles are introduced into the fiber matrix and the fiber with the porous structure is subjected to high-temperature steam heat treatment, so that the obtained porous structure fiber has permanently improved softness and bulkiness, and the defects of poor softness, bulkiness and air permeability of the conventional fiber material added with the inorganic antibacterial and mildewproof material and the inorganic aldehyde-removing and deodorizing material are overcome.
(2) According to the invention, special silicon dioxide aerogel microspheres are adopted to adsorb and fix the pore-forming agent calcium acetate, so that the uniformity and stability of the pore-forming agent calcium acetate in the fiber matrix are improved. In the subsequent thermal decomposition pore-forming process, the pores of the silica aerogel microspheres provide a guiding function for the escape of acetone gas, and the formed porous structure is uniform. And the fiber strength is not obviously reduced under the reinforcing effect of the silica aerogel microspheres and the nano calcium carbonate generated in situ.
(3) The porous structure fiber prepared by the invention has better combination effect with the soft finishing agent, the soft finishing effect is further obviously enhanced, and the obtained soft chip has long-term washable smooth hand feeling.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The silica aerogel microspheres containing carboxyl groups described in the following examples were prepared by the following method:
adjusting the pH value of silica sol to about 3.0 by using an acid solution, adding 3- [ 3-carboxyl allylamido ] propyl triethoxysilane as a mixed silicon source, stirring and mixing uniformly, continuously stirring and adding absolute ethyl alcohol, adding the obtained mixed solution into acetone, adding an emulsifier OP-10, homogenizing to obtain emulsion, then adding ammonia water to adjust the pH value to about 10.0, stirring and mixing uniformly, standing and layering, washing and drying the sediment on the lower layer, and crushing to obtain the silica aerogel microspheres containing carboxyl. The particle size range of the mesoporous silica is 0.1-1 mu m, and the pore diameter range is 10-40 nm.
Example 1
The preparation method of the multifunctional antibacterial, mildewproof, aldehyde-removing and deodorizing soft chip of the embodiment comprises the following preparation steps:
(1) Adding the silicon dioxide aerogel microspheres containing carboxyl into an aqueous solution containing calcium acetate and silver nitrate, and carrying out adsorption treatment for 2 hours under negative pressure and ultrasonic conditions, wherein the mass concentration of the calcium acetate is 5% and the mass concentration of the silver nitrate is 6%. And then adding the adsorbed silicon dioxide aerogel microspheres into a NaOH aqueous solution with the concentration of 0.04mol/L for soaking reaction for 2 hours. Washing the product with water, and drying by blowing at 110-120 ℃ for 4h to obtain the pore-forming antibacterial particles.
(2) Uniformly mixing the pore-forming antibacterial particles obtained in the step (1), nano-mineral crystal powder and nano-titanium dioxide powder, and then adding the mixture into an acrylic fiber spinning solution to be uniformly stirred and mixed, wherein the adding amount of the pore-forming antibacterial particles is 2% of the mass of the fiber base material, the adding amount of the nano-mineral crystal powder is 3% of the mass of the fiber base material, and the adding amount of the nano-titanium dioxide powder is 3% of the mass of the fiber base material. And then spinning by a dry-wet method to obtain the nascent fiber.
(3) And (3) carrying out steam heat treatment on the nascent fiber obtained in the step (2) at 170 ℃ for 3h, then cooling to 130 ℃ and carrying out vacuum drying to obtain the porous fiber.
(4) And (3) weaving and forming the porous fiber obtained in the step (3), adding the formed fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 1 hour at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 75%, then placing the fiber material into an oven to dry at 90 ℃, and setting for 30 seconds at 160 ℃ to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
Example 2
The preparation method of the multifunctional antibacterial, mildewproof, aldehyde-removing and deodorizing soft chip of the embodiment comprises the following preparation steps:
(1) Adding the silicon dioxide aerogel microspheres containing carboxyl into an aqueous solution containing calcium acetate and copper nitrate, and carrying out adsorption treatment for 4 hours under the conditions of negative pressure and ultrasound, wherein the mass concentration of the calcium acetate is 2%, and the mass concentration of the copper nitrate is 3%. Then adding the adsorbed silica aerogel microspheres into a NaOH aqueous solution with the concentration of 0.05mol/L for soaking reaction for 4 hours. Washing the product with water, and drying by blowing at 110-120 ℃ for 4h to obtain the pore-forming antibacterial particles. The adsorbed amount of calcium acetate was found to be 71mg/g.
(2) Uniformly mixing the pore-forming antibacterial particles obtained in the step (1), nano-ore crystal powder and nano-titanium dioxide powder, and then adding the mixture into a polylactic acid fiber spinning solution to be uniformly stirred and mixed, wherein the adding amount of the pore-forming antibacterial particles is 4% of the mass of the fiber base material, the adding amount of the nano-ore crystal powder is 2% of the mass of the fiber base material, and the adding amount of the nano-titanium dioxide powder is 2% of the mass of the fiber base material. And then spinning by a dry-wet method to obtain the nascent fiber.
(3) And (3) carrying out steam heat treatment on the nascent fiber obtained in the step (2) at 180 ℃ for 3h, then cooling to 140 ℃ and carrying out vacuum drying to obtain the porous fiber.
(4) And (4) weaving and molding the porous fiber obtained in the step (3), then adding the molded fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 0.5h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 80%, then placing the fiber material into an oven to dry at 85 ℃, and setting for 45s at 150 ℃ to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
Example 3
The preparation method of the multifunctional antibacterial, mildewproof, aldehyde-removing and deodorizing soft chip of the embodiment comprises the following preparation steps:
(1) Adding the silicon dioxide aerogel microspheres containing carboxyl into an aqueous solution containing calcium acetate and silver nitrate, and carrying out adsorption treatment for 1h under negative pressure and ultrasonic conditions, wherein the mass concentration of the calcium acetate is 8% and the mass concentration of the silver nitrate is 5%. And then adding the adsorbed silica aerogel microspheres into a NaOH aqueous solution with the concentration of 0.02mol/L for soaking reaction for 4 hours. Washing the product with water, and drying by blowing at 115-120 ℃ for 4h to obtain the pore-forming antibacterial particles.
(2) Uniformly mixing the pore-forming antibacterial particles obtained in the step (1), nano-ore crystal powder and nano-titanium dioxide powder, adding the mixture into a polyvinyl alcohol fiber spinning solution, and uniformly stirring and mixing the mixture, wherein the adding amount of the pore-forming antibacterial particles is 0.5% of the mass of the fiber base material, the adding amount of the nano-ore crystal powder is 1% of the mass of the fiber base material, and the adding amount of the nano-titanium dioxide powder is 1% of the mass of the fiber base material. Then, the nascent fiber is obtained through wet spinning.
(3) And (3) carrying out steam heat treatment on the nascent fiber obtained in the step (2) at 160 ℃ for 6h, then cooling to 130 ℃ and carrying out vacuum drying to obtain the porous fiber.
(4) And (3) weaving and forming the porous fiber obtained in the step (3), adding the formed fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 1 hour at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 70%, then placing the fiber material into an oven to dry at 95 ℃, and setting for 20 seconds at 170 ℃ to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
Comparative example 1
Compared with the example 2, the comparative example has no pore-forming agent calcium acetate, and the preparation steps are as follows:
(1) Adding the silicon dioxide aerogel microspheres containing carboxyl into a copper nitrate aqueous solution with the mass concentration of 3%, and carrying out adsorption treatment for 4 hours under the conditions of negative pressure and ultrasound. Then adding the adsorbed silica aerogel microspheres into a NaOH aqueous solution with the concentration of 0.05mol/L for soaking reaction for 4 hours. Washing the product with water, and drying the product by blowing air at the temperature of 110-120 ℃ for 4h to obtain the antibacterial particles.
(2) And (2) uniformly mixing the antibacterial particles obtained in the step (1), nano-ore crystal powder and nano-titanium dioxide powder, and then adding the mixture into the polylactic acid fiber spinning solution to be uniformly stirred and mixed, wherein the addition amount of the antibacterial particles is 4% of the mass of the fiber base material, the addition amount of the nano-ore crystal powder is 2% of the mass of the fiber base material, and the addition amount of the nano-titanium dioxide powder is 2% of the mass of the fiber base material. And then spinning by a dry-wet method to obtain the nascent fiber.
(3) And (3) carrying out steam heat treatment on the nascent fiber obtained in the step (2) at 180 ℃ for 3h, then cooling to 140 ℃ and carrying out vacuum drying to obtain the heat-treated fiber.
(4) And (4) weaving and molding the heat-treated fiber obtained in the step (3), then adding the molded fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 0.5h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 80%, then placing the fiber material into an oven to dry at 85 ℃, and setting for 45s at 150 ℃ to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
Comparative example 2
Compared with the example 2, the pore-forming agent calcium acetate is not adsorbed and fixed in advance, and the preparation method comprises the following specific steps:
(1) Adding the silicon dioxide aerogel microspheres containing carboxyl into a copper nitrate aqueous solution with the mass concentration of 3%, and carrying out adsorption treatment for 4 hours under the conditions of negative pressure and ultrasound. And then adding the adsorbed silica aerogel microspheres into a NaOH aqueous solution with the concentration of 0.05mol/L for soaking reaction for 4 hours. Washing the product with water, and drying the product by blowing air at the temperature of 110-120 ℃ for 4h to obtain the antibacterial particles.
(2) And (2) uniformly mixing the antibacterial particles obtained in the step (1), nano-mineral crystal powder and nano-titanium dioxide powder, adding the mixture into the polylactic acid fiber spinning solution, uniformly stirring and mixing, and then adding calcium acetate to dissolve uniformly, wherein the adding amount of the antibacterial particles is 4% of the mass of the fiber base material, the adding amount of the nano-mineral crystal powder is 2% of the mass of the fiber base material, the adding amount of the nano-titanium dioxide powder is 2% of the mass of the fiber base material, and the adding amount of the calcium acetate is 0.284% of the mass of the fiber base material (the actual adding amount of the calcium acetate in the embodiment 2). And then spinning by a dry-wet method to obtain the nascent fiber.
(3) And (3) carrying out steam heat treatment on the nascent fiber obtained in the step (2) at 180 ℃ for 3h, then cooling to 140 ℃ and carrying out vacuum drying to obtain the porous fiber.
(4) And (4) weaving and molding the porous fiber obtained in the step (3), then adding the molded fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 0.5h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 80%, then placing the fiber material into an oven to dry at 85 ℃, and setting for 45s at 150 ℃ to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
1. The antibacterial, aldehyde-removing and deodorizing performances of the products obtained in the above example 2 and comparative examples 1 to 2 were tested. The antibacterial performance test is according to GB/T20944.3-2008, and the test bacteria are staphylococcus aureus (S.aureus) and escherichia coli (coli); the odor eliminating performance test is carried out according to GB/T33610.2-2017, and the test gas is ammonia gas; the formaldehyde removal performance test refers to a deodorization performance test, and the ammonia gas in the test gas is replaced by formaldehyde. The test results are shown in table 1 below.
TABLE 1
As can be seen from the results in Table 1, the porous fiber prepared by adding the pore-foaming agent calcium acetate has no adverse effect on the antibacterial performance of the product, and the aldehyde-removing and odor-eliminating performance is obviously improved. By adsorbing and fixing the pore-forming agent calcium acetate in advance, the improvement of the aldehyde-removing and odor-removing performance is more remarkable. The reason is that the pore-forming agent calcium acetate is adsorbed and fixed in advance through the silicon dioxide aerogel microsphere carrier, so that the opening uniformity of porous fibers is improved, and the adsorption and decomposition capacity of test gas is stronger.
2. The soft bulk (evaluated by hand touch, with a hand feel rating of 5 points at the highest and 0 points at the lowest, and evaluated by five persons at the same time, with average values), the stiffness (measured in accordance with ZB W04003-87, fabric stiffness test method, oblique cantilever method; the lower the stiffness, the better the softness of the fabric), the water-wash resistance (measured in accordance with GB/T8629-2001, home Wash and drying procedure for textile test), and the fiber strength (measured in accordance with ISO 5079-1995) of the products obtained in example 2 and comparative examples 1-2 above were as shown in Table 2 below.
TABLE 2
As can be seen from the results in Table 2, the softness and bulkiness of the porous fiber obtained by adding the pore-foaming agent are remarkably improved, and the strength of the fiber is not obviously reduced due to the generation of a porous structure. It can be seen from the results of comparative example 2 that, in the case where the pore-forming agent calcium acetate is not adsorbed and fixed in advance by using the silica aerogel microspheres, the softness and bulkiness thereof are reduced to a certain extent, and the fiber strength is significantly reduced. The result shows that the loading of the silica aerogel microspheres has an obvious effect on improving the uniformity and stability of the pore-forming agent calcium acetate in the fiber matrix, and in the subsequent thermal decomposition pore-forming process, the pores of the silica aerogel microspheres provide a guiding effect on the escape of decomposed gas, so that the formed porous structure is uniform. And the particle size and the dispersion degree of the calcium carbonate generated by decomposition can be controlled, and the strength of the fiber is maintained not to be obviously reduced.
3. The soft finish of the products obtained in example 2 and comparative examples 1 to 2 above was tested: the smoothness after finishing is evaluated by measuring the static friction coefficient (mus) and the dynamic friction coefficient (mu d) of the fabric by a friction coefficient instrument, and the smooth hand feeling after finishing is evaluated by a touch method, wherein the A grade is very smooth, the B grade is relatively smooth, and the C grade is relatively coarse. The test results are shown in table 3 below.
TABLE 3
As can be seen from the results in Table 3, the soft chips obtained by the present invention are soft finished by amino silicone oil emulsion, and after 20 times of water washing, the smoothness is basically unchanged, while the smoothness of comparative example 1 and comparative example 2 is obviously reduced. The porous structure fiber prepared by the specific method can obviously enhance the water washing resistance of soft finishing, and the reason is that the uniform porous structure of the fiber and the soft finishing agent have better combination effect, and the obtained soft chip has long-term water washing resistance and smooth hand feeling.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. The preparation method of the multifunctional soft chip with the functions of antibiosis, mildew prevention, aldehyde removal and deodorization is characterized by comprising the following preparation steps:
(1) Adding the silica aerogel microspheres into an inorganic antibacterial metal salt solution containing calcium acetate for adsorption treatment, then adding the adsorbed silica aerogel microspheres into a dilute alkali solution for soaking reaction, and washing and drying the product to obtain pore-forming antibacterial particles;
(2) Uniformly mixing the pore-forming antibacterial particles obtained in the step (1) with an inorganic aldehyde-removing deodorizing powder material, mixing the mixture with a fiber base material, and then carrying out solution spinning to obtain nascent fiber;
(3) Carrying out steam heat treatment on the nascent fiber obtained in the step (2) at 160-190 ℃, and drying in vacuum to obtain porous fiber;
(4) Weaving and forming the porous fiber obtained in the step (3), and then performing softening finishing to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip;
the particle size range of the silica aerogel microspheres in the step (1) is from 20nm to 1.5 mu m, and the pore size range is from 2 to 50nm; the silicon dioxide aerogel microspheres refer to silicon dioxide aerogel microspheres containing carboxyl, and are prepared by the following method:
adjusting the pH value of silica sol to 1~4 by using an acid solution, adding 3- [ 3-carboxyl allylamido ] propyl triethoxysilane as a mixed silicon source, stirring and mixing uniformly, continuously stirring and adding absolute ethyl alcohol, adding the obtained mixed solution into an organic solvent, adding an emulsifier for homogenization to obtain an emulsion, adding ammonia water to adjust the pH value to 9-11, stirring and mixing uniformly, standing for layering, washing, drying and crushing a lower-layer precipitate to obtain a carboxyl-containing silica aerogel microsphere;
the dilute alkali solution in the step (1) is a NaOH solution with the concentration of 0.02 to 0.05mol/L; the drying is carried out by blowing and drying at the temperature of 100 to 120 ℃ for 0.5 to 6 hours.
2. The method for preparing the multifunctional soft chip with antibacterial, mildewproof, aldehyde removal and deodorization functions as claimed in claim 1, wherein the inorganic antibacterial metal salt solution containing calcium acetate in the step (1) is silver nitrate, copper nitrate or zinc nitrate aqueous solution in which calcium acetate is dissolved; wherein the mass concentration ranges of the calcium acetate and the inorganic antibacterial metal salt are both 0.5-10%.
3. The preparation method of the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip according to claim 1, wherein the adsorption treatment in the step (1) is performed under the conditions of ultrasonic and vacuum stirring, and the adsorption treatment time is 0.5 to 4 hours.
4. The preparation method of the multifunctional soft chip with antibacterial, mildewproof, aldehyde removing and deodorizing functions as claimed in claim 1, wherein the inorganic aldehyde removing and deodorizing powder material in the step (2) comprises at least one of nano mineral crystal powder, nano titanium dioxide powder, nano zinc oxide powder and nano diatomite; the particle size range of the inorganic aldehyde-removing and odor-eliminating powder material is from 20nm to 1.5 mu m.
5. The preparation method of the multifunctional soft chip with antibacterial, mildewproof, aldehyde removal and deodorization functions as claimed in claim 4, wherein the adding amount of the pore-forming antibacterial particles in the step (2) is 0.2-4% of the mass of the fiber base material; the addition amount of the inorganic aldehyde-removing and deodorizing powder material is 0.5-8% of the mass of the fiber base material.
6. The method for preparing the multifunctional soft chip with the functions of antibiosis, mildew prevention, aldehyde removal and deodorization according to claim 1, wherein the fiber base material in the step (2) is any one of polyvinyl alcohol fiber, viscose fiber, acrylic fiber, spandex fiber, polyvinyl chloride fiber, polyvinyl alcohol fiber, polylactic acid fiber and chitosan fiber; the solution spinning includes any one of dry spinning, wet spinning and dry-wet spinning.
7. The preparation method of the multifunctional soft chip with antibacterial, mildewproof, aldehyde removal and deodorization functions as claimed in claim 1, wherein the steam heat treatment time in the step (3) is 1 to 6 hours; the temperature of the vacuum drying is 120 to 140 ℃.
8. The preparation method of the multifunctional soft chip with antibacterial, mildewproof, aldehyde removal and deodorization functions as claimed in claim 1, wherein the softening finishing in step (4) adopts amino silicone oil emulsion softening finishing agent, and the softening finishing step comprises: adding the formed fiber material into an amino silicone oil emulsion soft finishing agent, soaking for 0.5-1h at normal temperature, soaking for two times and rolling at a mangling rate of 70-80%, then putting into an oven, drying at 85-95 ℃, and shaping for 20-60s at 150-170 ℃ to obtain the antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip.
9. An antibacterial, mildewproof, aldehyde-removing and deodorizing multifunctional soft chip, which is prepared by the method of any one of claims 1~8.
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| CN115806297A (en) * | 2022-12-01 | 2023-03-17 | 华侨大学 | Preparation method of antibacterial hydrophobic silica aerogel composite material |
| CN116535868A (en) * | 2023-04-11 | 2023-08-04 | 中广核高新核材集团（东莞）祈富新材料有限公司 | Improved antibacterial mildew-proof TPE and production method thereof |
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