CN114808172A - Graphene multifunctional antiviral and antibacterial soft chip and preparation method thereof - Google Patents
Graphene multifunctional antiviral and antibacterial soft chip and preparation method thereof Download PDFInfo
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- 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
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Abstract
The invention belongs to the technical field of functional fiber materials, and discloses a graphene multifunctional antiviral and antibacterial soft chip and a preparation method thereof. Adding graphene and an inorganic functional powder material into silica sol for surface gel reaction to obtain porous silica and a surface-modified inorganic nano powder material, and then adding the porous silica and the surface-modified inorganic nano powder material into a traditional Chinese medicine antiviral extract containing calcium acetate for adsorption treatment to obtain multifunctional nanoparticles; adding the obtained multifunctional nanoparticles into a fiber spinning solution, carrying out solution spinning to obtain nascent fibers, carrying out steam heat treatment at 160-190 ℃, carrying out vacuum drying to obtain porous fibers, weaving and forming, and carrying out softening finishing to obtain the graphene multifunctional antiviral and antibacterial soft chip. The graphene multifunctional antiviral and antibacterial soft chip has good antiviral and antibacterial effects and health care effects, and has a soft and smooth hand feeling of long-term water washing resistance.
Description
Technical Field
The invention belongs to the technical field of functional fiber materials, and particularly relates to a graphene multifunctional antiviral and antibacterial soft chip and a preparation method thereof.
Background
The functional fiber is the fiber which is added with some special functions besides the existing performance of the fiber. Such as graphene fiber, far infrared fiber, anion fiber, antibacterial deodorizing fiber, antiviral fiber, etc.
Patent CN 110592716 a discloses a preparation method of graphene antibacterial fiber, which comprises the following steps: s01, preprocessing: respectively carrying out vacuum drying on the graphene nano composition and the high-melting-point polymer for later use; s02, granulating and gas conveying: inputting hot air flow into the graphene nano composition to form hot air flow containing the graphene nano composition, and putting the high-melting-point polymer into an extruder to extrude to obtain polymer master batches; s03, melt spinning: melting the polymer master batch to obtain a polymer melt, and quantitatively conveying the polymer melt to a spinneret to spray polymer trickle; s04, traction compounding: introducing hot air flow containing the graphene nano composition to draft the polymer trickle to obtain graphene antibacterial nascent fibers; s05, cooling and forming: and cooling, solidifying and molding the graphene antibacterial nascent fiber to obtain the graphene antibacterial fiber. Patent CN 113564741 a discloses a preparation method of far infrared fiber: mixing the kyanite, the plant carbon and the first dispersing agent, and carrying out wet grinding to obtain powder slurry; the particle size of solid particles in the powder slurry is 0.1-1 mu m; drying and calcining the powder slurry in sequence to obtain the far infrared functional powder; and then carrying out solution spinning or melt spinning on the far infrared functional powder and the fiber base material to obtain the far infrared fiber. Patent CN 113718361 a discloses a graphene anion regenerated cellulose composite fiber and a preparation method thereof, the method comprises: step 1, weighing raw materials in proportion; the raw materials comprise cellulose, a graphene material, a modifier and anion powder; step 2, grinding the negative ion powder by using a ball mill, and then drying; step 3, dispersing cellulose, graphene and a modifier in a solvent, fully dissolving the cellulose by stirring, and preparing a spinning solution; and 4, spinning the spinning solution containing the completely dissolved cellulose obtained in the step 3 by using a dry-jet wet spinning process. The prepared composite fiber has the functions of antibiosis, negative ion release and the like. Patent CN 1546755A discloses a processing method of a durable antibacterial deodorizing fiber fabric, which is to add nano-scale inorganic antibacterial agent into high polymer powder by 3-30% of weight ratio and mix uniformly, and form antibacterial master batch by screw granulation technology. The antibacterial master batch is mixed with the high polymer in a proportion of 0.3-10%, the mixture is spun, the fabric is formed after spinning and weaving, and the fabric processed by the method has the advantages of good antibacterial effect and strong durability after being subjected to aftertreatment by the antibacterial agent. Patent CN 106995943A discloses a sarcandra glabra high-efficiency antibacterial antiviral cellulose fiber, which is prepared by preparing chitosan-functional component composite particles, preparing silicic acid composite colloid, blending and spinning. The content of the chitosan-functional component composite particles in the fiber is 9.5-9.7%, and the content of the silicic acid composite colloid is 23.5%. In our earlier patent CN 112941652 a, a method for preparing an antiviral, antibacterial and degradable multifunctional fiber is disclosed, wherein an antiviral extract of traditional Chinese medicine is adsorbed by inorganic nano powder material surface-modified by porous silica and silane coupling agent, and then the traditional Chinese medicine and the degradable fiber matrix are mixed and spun, so that the fiber has antiviral, antibacterial and health care effects.
As can be seen from the above prior art, the general preparation method of functional fiber generally adds inorganic functional materials, such as graphene, far infrared additive, anion additive, and antibacterial powder, to the fiber matrix to achieve the required additional characteristics. And the dispersion effect of the inorganic functional material is improved by a certain load dispersion technology. However, in the actual application process, it is found that the soft and fluffy hand feeling and air permeability of the fiber material added with the inorganic functional filler are adversely affected, and in the field of clothing home textile materials, the use feeling of fluffy, soft and good air permeability is a great demand of consumers. Therefore, how to realize that the fiber material has more additional functions and simultaneously has good fluffy and soft hand feeling and air permeability is a technical problem to be solved by the technical personnel in the field.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of a graphene multifunctional antiviral and antibacterial soft chip.
The invention also aims to provide the graphene multifunctional antiviral and antibacterial soft chip prepared by the method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a graphene multifunctional antiviral and antibacterial soft chip comprises the following preparation steps:
(1) adding graphene, inorganic antibacterial powder, far infrared powder and anion powder into silica sol, stirring and mixing uniformly, then adding a silane coupling agent for surface gel reaction, drying in vacuum at 120-200 ℃, and crushing to obtain porous silicon dioxide and a silane coupling agent surface modified inorganic nano powder material;
(2) adding the porous silicon dioxide obtained in the step (1) and the inorganic nano powder material surface-modified by the silane coupling agent into a traditional Chinese medicine antiviral extract containing calcium acetate for adsorption treatment, and freeze-drying to obtain multifunctional nano particles;
(3) adding the multifunctional nano particles obtained in the step (2) into a fiber spinning solution, uniformly stirring and dispersing, and then spinning through a solution to obtain nascent fibers;
(4) carrying out steam heat treatment on the nascent fiber obtained in the step (3) at 160-190 ℃, and drying in vacuum to obtain porous fiber;
(5) and (4) weaving and forming the porous fiber obtained in the step (4), and then carrying out softening finishing to obtain the graphene multifunctional antiviral and antibacterial soft chip.
Further, the inorganic antibacterial powder in the step (1) is at least one selected from nano silver oxide powder, nano copper oxide powder and nano zinc oxide powder; the far infrared powder comprises at least one of vermiculite raw ore powder, medical stone raw ore powder, far infrared ceramic powder, nano zirconia, taiji stone powder and nano manganese oxide; the anion powder comprises at least one of tourmaline anion powder and natural opal mineral powder.
Further, the silane coupling agent in the step (1) is 3- [ 3-carboxyl allylamido ] propyl triethoxysilane which is a silane coupling agent containing carboxyl; the adding amount of the silane coupling agent is 0.1-5% of the mass of the silica sol. The silane coupling agent containing carboxyl has better adsorption and fixation effects on calcium acetate.
Further, in the step (1), the solid content of the silica sol is 10% -30%, and the particle size is 5-80 nm.
Further, the mass ratio of the total mass of the graphene, the inorganic antibacterial powder, the far infrared powder and the negative ion powder to the mass of the silica sol in the step (1) is 1: 2-2: 1.
Further, the antiviral extract of the traditional Chinese medicine in the step (2) comprises at least one antiviral traditional Chinese medicine extract component selected from radix isatidis, dandelion, honeysuckle, wild chrysanthemum flower, folium isatidis, andrographis paniculata, scutellaria baicalensis, coptis chinensis, golden cypress, radix bupleuri, cyrtomium rhizome, fructus forsythiae, polygonum cuspidatum, blackberry lily, rheum officinale, houttuynia cordata, elsholtzia, eupatorium, cacumen biotae, rhizoma polygonati, schisandra chinensis, burdock, radix sileris, purple perilla, verbena, rabdosia rubescens, radix sophorae flavescentis, radix scrophulariae, solanum dulcamara, belvedere fruit, Indian mockstrawberry herb, bezoar, lithospermum, pericarpium citri reticulatae, ageratum and mint; the solvent of the traditional Chinese medicine antiviral extract is an ethanol/water mixed solvent with the volume fraction of 30-50% of ethanol. The addition of a proper amount of ethanol in the solvent system of the invention has a remarkable promoting effect on the adsorption and fixation of calcium acetate.
Further, the mass concentration of the calcium acetate in the traditional Chinese medicine antiviral extract in the step (2) is 0.5-10%.
Further, the adsorption treatment in the step (2) is carried out under the conditions of ultrasound and vacuum stirring, and the adsorption treatment time is 0.5-4 h. The traditional Chinese medicine extracting solution and the calcium acetate solution can be remarkably promoted to be immersed into the pores of the porous silicon dioxide by ultrasonic and vacuum stirring, and the adsorption and fixation of the active ingredients of the traditional Chinese medicine and the calcium acetate are realized.
Further, the fiber spinning solution in the step (3) is 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; the solution spinning includes any one of dry spinning, wet spinning and dry-wet spinning.
Preferably, the adding amount of the multifunctional nanoparticles in the step (3) is 1-15% of the mass of the fiber base material.
Further, the steam heat treatment time in the step (4) is 1-6 h.
Further, the temperature of the vacuum drying in the step (4) is 120-140 ℃.
Further, the weaving and forming in the step (5) 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 (5) adopts amino silicone oil emulsion soft finishing agent, and the soft finishing step comprises: 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 mangling rate is 70% -80%, then placing the obtained product into an oven to be dried at 85-95 ℃, and shaping for 20-60 s at 150-170 ℃ to obtain the graphene multifunctional antiviral and antibacterial soft chip.
A graphene multifunctional antiviral antibacterial soft chip is prepared by the method.
The graphene multifunctional antiviral and antibacterial soft chip is applied to industrial products such as home, hotel, nursing home mattresses, textiles, automobile seats, outdoor products and the like.
The principle of the invention is as follows: firstly, inorganic functional nanoparticles are used as templates, a porous silicon dioxide layer is prepared on the surfaces of the inorganic functional nanoparticles by a low-cost silica sol-gel method, and the compatibility and the adsorption and fixation effects of the porous silicon dioxide layer on a pore-forming agent and antiviral components of traditional Chinese medicines are improved by a specific silane coupling agent. And then mixing the multifunctional nano particles adsorbed with the pore-forming agent and the traditional Chinese medicine antiviral components with a fiber spinning solution, and then spinning through the solution to obtain the nascent fiber. And (3) carrying out steam heat treatment on the obtained nascent fiber at 160-190 ℃, wherein 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 porous silicon dioxide 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) the invention integrates inorganic antibacterial and inorganic health care functions and traditional Chinese medicine antiviral functions into the same particle, can simultaneously play the antibacterial, antiviral and health care functions, and can improve the antibacterial and antiviral activities to a certain extent by adding pore-foaming agent to form porous fiber.
(2) According to the invention, the special pore-forming agent is introduced into the fiber matrix and the high-temperature steam heat treatment is carried out, 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 inorganic functional nanoparticles are overcome.
(3) According to the invention, the inorganic nano powder material with the surface modified by the porous silicon dioxide and the silane coupling agent is used for adsorbing and fixing the pore-forming agent calcium acetate in advance, so that the thermal decomposition stability and uniformity of the inorganic nano powder material in the fiber base material can be obviously improved, the soft and fluffy hand feeling is better, and no obvious adverse effect is caused on the fiber strength.
(4) 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 antiviral extract of the traditional Chinese medicine described in the following examples is prepared by the following method:
according to the mass parts, 30 parts of isatis root, 20 parts of dandelion, 20 parts of honeysuckle, 10 parts of wild chrysanthemum flower, 10 parts of folium isatidis, 10 parts of andrographis paniculata, 5 parts of pericarpium citri reticulatae, 5 parts of ageratum and 5 parts of mint are added into 500 parts of ethanol water solution to be decocted, filtered, filtrate is concentrated, and the volume fraction of ethanol is adjusted to be 40%, so that the antiviral extracting solution of the traditional Chinese medicine is obtained.
Example 1
The preparation method of the multifunctional antiviral and antibacterial graphene software chip of the embodiment comprises the following preparation steps:
(1) adding 20 parts by mass of graphene, 40 parts by mass of nano silver oxide antibacterial powder, 50 parts by mass of far infrared ceramic powder and 50 parts by mass of tourmaline negative ion powder into 200 parts by mass of silica sol (with the solid content of 15% and the particle size of 30-50 nm), uniformly stirring and mixing, then adding 4 parts by mass of 3- [ 3-carboxyl allylamido ] propyl triethoxysilane for surface gel reaction, drying in vacuum at 150-160 ℃, and crushing to the particle size of less than 1.5 mu m to obtain porous silicon dioxide and a surface modified inorganic nano powder material.
(2) Adding the porous silicon dioxide and the surface modified inorganic nano powder material obtained in the step (1) into a traditional Chinese medicine antiviral extract containing 6 wt% of calcium acetate, performing adsorption treatment for 2 hours under the conditions of ultrasonic and vacuum stirring, filtering, taking the solid, and freeze-drying to obtain the multifunctional nano particles.
(3) And (3) adding the multifunctional nanoparticles obtained in the step (2) into an acrylic fiber spinning solution, uniformly stirring and dispersing, wherein the adding amount of the multifunctional nanoparticles is 8% of the mass of the acrylic fiber base material, and then spinning by a dry method and a wet method to obtain the nascent fiber.
(4) And (4) carrying out steam heat treatment on the nascent fiber obtained in the step (3) at 170 ℃ for 3h, then cooling to 130 ℃ and carrying out vacuum drying to obtain the porous fiber.
(5) And (3) weaving and molding the porous fiber obtained in the step (4), then adding the molded fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 1h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 75%, then placing the obtained product into an oven to dry at 90 ℃ and shape for 30s at 160 ℃ to obtain the graphene multifunctional antiviral antibacterial soft chip.
Example 2
The preparation method of the multifunctional antiviral and antibacterial graphene software chip of the embodiment comprises the following preparation steps:
(1) adding 15 parts by mass of graphene, 25 parts by mass of nano copper oxide antibacterial powder, 30 parts by mass of far infrared ceramic powder and 30 parts by mass of tourmaline negative ion powder into 200 parts by mass of silica sol (solid content is 10%, particle size is 5-30 nm), uniformly stirring and mixing, then adding 3 parts by mass of 3- [ 3-carboxyl allyl amido ] propyl triethoxysilane for surface gel reaction, drying in vacuum at 150-160 ℃, and crushing to particle size smaller than 1.5 mu m to obtain porous silicon dioxide and surface modified inorganic nano powder material.
(2) Adding the porous silicon dioxide and the surface modified inorganic nano powder material obtained in the step (1) into a traditional Chinese medicine antiviral extract containing 10 wt% of calcium acetate, performing adsorption treatment for 1h under the conditions of ultrasonic and vacuum stirring, filtering, taking the solid, and freeze-drying to obtain the multifunctional nano particles.
(3) And (3) adding the multifunctional nano particles obtained in the step (2) into a viscose fiber spinning solution, uniformly stirring and dispersing, wherein the adding amount of the multifunctional nano particles is 12% of the mass of the viscose fiber base material, and then carrying out wet spinning to obtain the nascent fiber.
(4) And (4) carrying out steam heat treatment on the nascent fiber obtained in the step (3) at 180 ℃ for 3h, then cooling to 140 ℃ and carrying out vacuum drying to obtain the porous fiber.
(5) And (3) weaving and molding the porous fiber obtained in the step (4), then adding the molded fiber material into an amino silicone oil emulsion soft 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 obtained product into an oven to dry at 85 ℃, and shaping for 45s at 150 ℃ to obtain the graphene multifunctional antiviral antibacterial soft chip.
Example 3
The preparation method of the multifunctional antiviral and antibacterial graphene software chip of the embodiment comprises the following preparation steps:
(1) according to the mass parts, 30 parts of graphene, 60 parts of nano zinc oxide antibacterial powder, 70 parts of far infrared ceramic powder and 70 parts of tourmaline negative ion powder are added into 200 parts of silica sol (with the solid content being 30 percent and the particle size being 50-80 nm), the mixture is stirred and mixed uniformly, then 8 parts of 3- [ 3-carboxyl allyl amido ] propyl triethoxysilane by mass is added for surface gel reaction, the mixture is dried in vacuum at the temperature of 150-160 ℃, and the powder is crushed to the particle size being less than 1.5 mu m, so that the porous silicon dioxide and the surface modified inorganic nano powder material are obtained.
(2) Adding the porous silicon dioxide and the surface modified inorganic nano powder material obtained in the step (1) into a traditional Chinese medicine antiviral extract containing 1 wt% of calcium acetate, performing adsorption treatment for 4 hours under the conditions of ultrasonic and vacuum stirring, filtering, taking the solid, and freeze-drying to obtain the multifunctional nano particles.
(3) And (3) adding the multifunctional nanoparticles obtained in the step (2) into the polylactic acid fiber spinning solution, uniformly stirring and dispersing, wherein the adding amount of the multifunctional nanoparticles is 5% of the mass of the polylactic acid fiber base material, and then spinning by a dry method and a wet method to obtain the nascent fiber.
(4) And (4) carrying out steam heat treatment on the nascent fiber obtained in the step (3) at 160 ℃ for 6h, then cooling to 130 ℃ and carrying out vacuum drying to obtain the porous fiber.
(5) And (3) weaving and molding the porous fiber obtained in the step (4), then adding the molded fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 1h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 70%, then placing the obtained product into an oven to dry at 95 ℃, and shaping for 20s at 170 ℃ to obtain the graphene multifunctional antiviral antibacterial soft chip.
Comparative example 1
Compared with the example 1, the comparative example has no pore-forming agent calcium acetate, and the preparation steps are as follows:
(1) adding 20 parts by mass of graphene, 40 parts by mass of nano silver oxide antibacterial powder, 50 parts by mass of far infrared ceramic powder and 50 parts by mass of tourmaline negative ion powder into 200 parts by mass of silica sol (with the solid content of 15% and the particle size of 30-50 nm), uniformly stirring and mixing, then adding 4 parts by mass of 3- [ 3-carboxyl allylamido ] propyl triethoxysilane for surface gel reaction, drying in vacuum at 150-160 ℃, and crushing to the particle size of less than 1.5 mu m to obtain porous silicon dioxide and a surface modified inorganic nano powder material.
(2) Adding the porous silicon dioxide and the surface modified inorganic nano powder material obtained in the step (1) into the antiviral extracting solution of the traditional Chinese medicine, carrying out adsorption treatment for 2 hours under the conditions of ultrasonic and vacuum stirring, filtering, taking the solid, and freeze-drying to obtain the multifunctional nano particles.
(3) And (3) adding the multifunctional nanoparticles obtained in the step (2) into an acrylic fiber spinning solution, uniformly stirring and dispersing, wherein the adding amount of the multifunctional nanoparticles is 8% of the mass of the acrylic fiber base material, and then spinning by a dry method and a wet method to obtain the nascent fiber.
(4) And (4) carrying out steam heat treatment on the nascent fiber obtained in the step (3) at 170 ℃ for 3h, then cooling to 130 ℃ and carrying out vacuum drying to obtain the heat-treated fiber.
(5) And (4) weaving and forming the heat-treated fibers obtained in the step (4), then adding the formed fiber materials into an amino silicone oil emulsion softening finishing agent, soaking for 1h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 75%, then placing the obtained product into an oven to dry at 90 ℃ and shape for 30s at 160 ℃ to obtain the graphene multifunctional antiviral and antibacterial soft chip.
Comparative example 2
Compared with the embodiment 1, the pore-forming agent calcium acetate is not adsorbed and fixed in advance, and is mixed and added into the fiber spinning solution in the step (3), and the preparation steps are as follows:
(1) adding 20 parts by mass of graphene, 40 parts by mass of nano silver oxide antibacterial powder, 50 parts by mass of far infrared ceramic powder and 50 parts by mass of tourmaline negative ion powder into 200 parts by mass of silica sol (solid content is 15%, particle size is 30-50 nm), uniformly stirring and mixing, then adding 4 parts by mass of 3- [ 3-carboxyl allyl amido ] propyl triethoxysilane for surface gel reaction, drying in vacuum at 150-160 ℃, and crushing to particle size smaller than 1.5 mu m to obtain porous silicon dioxide and surface modified inorganic nano powder material.
(2) Adding the porous silicon dioxide and the surface modified inorganic nano powder material obtained in the step (1) into the antiviral extracting solution of the traditional Chinese medicine, carrying out adsorption treatment for 2 hours under the conditions of ultrasonic and vacuum stirring, filtering, taking the solid, and freeze-drying to obtain the multifunctional nano particles.
(3) And (3) adding the multifunctional nanoparticles obtained in the step (2) into an acrylic fiber spinning solution, uniformly stirring and dispersing, wherein the adding amount of the multifunctional nanoparticles is 8% of the mass of the acrylic fiber base material, adding calcium acetate (in terms of saturated adsorption amount) with the same adsorption amount as that in the example 1, uniformly mixing, and then carrying out dry-wet spinning to obtain the nascent fiber.
(4) And (4) carrying out steam heat treatment on the nascent fiber obtained in the step (3) at 170 ℃ for 3h, then cooling to 130 ℃ and carrying out vacuum drying to obtain the porous fiber.
(5) And (3) weaving and molding the porous fiber obtained in the step (4), then adding the molded fiber material into an amino silicone oil emulsion softening finishing agent, soaking for 1h at normal temperature, soaking for two times and rolling for two times, wherein the mangle rolling rate is 75%, then placing the obtained product into an oven to dry at 90 ℃ and shape for 30s at 160 ℃ to obtain the graphene multifunctional antiviral antibacterial soft chip.
Firstly, the antiviral and antibacterial properties of the products obtained in the above example 1 and comparative examples 1-2 were tested. The antiviral performance detection requirement and basis are WS 628-2018; ISO 18184-; the test viruses were influenza A H1N1 and coronavirus Hcov-229E. The antibacterial performance test is in accordance with GB/T20944.3-2008, and the test bacteria are staphylococcus aureus (S.aureus) and escherichia coli (coli). The test results are shown in table 1 below.
TABLE 1
As can be seen from the results in Table 1, the antibacterial and antiviral activity of the present invention can be improved to a certain extent by adding the pore-forming agent to form the porous fiber.
Secondly, the soft bulk (evaluated by a touch method, the highest hand feeling evaluation score is 5 points, the lowest hand feeling evaluation score is 0 points, five persons evaluate simultaneously, the average score is taken), the stiffness (tested by referring to ZB W04003-87 inclined plane cantilever method for fabric stiffness test method), the softness of the fabric is better when the stiffness is smaller), the water washing resistance (tested by GB/T8629-2001 family washing and drying program for textile test) and the fiber strength (tested by standard ISO 5079-1995) of the products obtained in the example 1 and the comparative examples 1-2 are shown in the following table 2.
TABLE 2
As can be seen from the results in Table 2, the soft bulkiness and the washing resistance of the porous fiber obtained by adding the pore-foaming agent are remarkably improved, and higher fiber strength can be maintained. It can be seen from the results of comparative example 2 that when the pore-forming agent calcium acetate is not adsorbed and fixed in advance, the softness and bulkiness of the fiber spinning solution in step (3) are reduced to some extent and the fiber strength is significantly reduced. The load of the porous silicon dioxide and the surface modified inorganic nano powder material has 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 porous silicon dioxide provide a guiding effect on the escape of decomposition 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.
Thirdly, the soft finishing effect of the products obtained in the above example 1 and comparative examples 1-2 is 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 fiber with a porous structure prepared by the specific method of the invention can remarkably enhance the water washing resistance of soft finishing, and the smoothness is basically unchanged after 20 times of water washing. The reason for this is that the uniform porous structure of the fiber has a better bonding effect with the soft finishing agent, and the obtained soft chip has a long-term water-washing-resistant 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 (10)
1. A preparation method of a graphene multifunctional antiviral and antibacterial soft chip is characterized by comprising the following preparation steps:
(1) adding graphene, inorganic antibacterial powder, far infrared powder and anion powder into silica sol, stirring and mixing uniformly, then adding a silane coupling agent for surface gel reaction, drying in vacuum at 120-200 ℃, and crushing to obtain porous silicon dioxide and a silane coupling agent surface modified inorganic nano powder material;
(2) adding the porous silicon dioxide obtained in the step (1) and the inorganic nano powder material surface-modified by the silane coupling agent into a traditional Chinese medicine antiviral extract containing calcium acetate for adsorption treatment, and freeze-drying to obtain multifunctional nano particles;
(3) adding the multifunctional nano particles obtained in the step (2) into a fiber spinning solution, uniformly stirring and dispersing, and then spinning through a solution to obtain nascent fibers;
(4) carrying out steam heat treatment on the nascent fiber obtained in the step (3) at 160-190 ℃, and drying in vacuum to obtain porous fiber;
(5) and (4) weaving and forming the porous fiber obtained in the step (4), and then carrying out softening finishing to obtain the graphene multifunctional antiviral and antibacterial soft chip.
2. The method for preparing the graphene multifunctional antiviral and antibacterial soft chip according to claim 1, wherein the inorganic antibacterial powder in the step (1) is at least one selected from nano silver oxide powder, nano copper oxide powder and nano zinc oxide powder; the far infrared powder is at least one of vermiculite raw ore powder, medical stone raw ore powder, far infrared ceramic powder, nano zirconia, taiji stone powder and nano manganese oxide; the anion powder is at least one of tourmaline anion powder and natural opal mineral powder.
3. The method for preparing a graphene multifunctional antiviral and antibacterial soft chip as claimed in claim 1, wherein the silane coupling agent in step (1) is 3- [ 3-carboxyallylamido ] propyltriethoxysilane; the adding amount of the silane coupling agent is 0.1-5% of the mass of the silica sol; the solid content of the silica sol is 10% -30%, and the particle size is 5-80 nm.
4. The method for preparing the graphene multifunctional antiviral and antibacterial soft chip according to claim 1, wherein the ratio of the total mass of the graphene, the inorganic antibacterial powder, the far infrared powder and the negative ion powder to the mass of the silica sol in the step (1) is 1:2 to 2: 1.
5. The method for preparing a graphene multifunctional antiviral and antibacterial soft chip according to claim 1, wherein the Chinese medicinal antiviral extract in step (2) comprises at least one antiviral extract component of Chinese medicinal herbs selected from radix Isatidis, herba Taraxaci, flos Lonicerae, flos Chrysanthemi Indici, folium Isatidis, herba Andrographitis, radix Scutellariae, rhizoma Coptidis, cortex Phellodendri, radix bupleuri, rhizoma Osmundae, fructus forsythiae, rhizoma Polygoni Cuspidati, rhizoma Belamcandae, radix Et rhizoma Rhei, herba Houttuyniae, herba Moslae, herba Eupatorii, cacumen Platycladi, rhizoma Polygonati, fructus Schisandrae chinensis, fructus Arctii, radix Saposhnikoviae, Perillae, herba Verbenae, Rabdosia Rubescens (Hemsl.) Hara, radix Sophorae Flavescentis, radix scrophulariae, herba Solani Lyrati, Kochiae fructus, herba Duchesneae Indicae, calculus bovis, radix Arnebiae, pericarpium Citri Reticulatae Chachiensis, herba Agastaches, and herba Menthae; the solvent of the traditional Chinese medicine antiviral extract is an ethanol/water mixed solvent with the volume fraction of 30-50% of ethanol.
6. The method for preparing a graphene multifunctional antiviral and antibacterial soft chip according to claim 1, wherein the mass concentration of the calcium acetate in the Chinese medicinal antiviral extract in the step (2) is 0.5-10%; the adsorption treatment is carried out under the conditions of ultrasound and vacuum stirring, and the adsorption treatment time is 0.5-4 h.
7. The method for preparing a multifunctional graphene antiviral and antibacterial soft chip according to claim 1, wherein the fiber spinning solution in step (3) is 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; the solution spinning comprises any one of dry spinning, wet spinning and dry-wet spinning; the adding amount of the multifunctional nano particles is 1-15% of the mass of the fiber base material.
8. The method for preparing the graphene multifunctional antiviral and antibacterial soft chip according to claim 1, wherein the steam heat treatment time in the step (4) is 1-6 h; the temperature of vacuum drying is 120-140 ℃.
9. The method for preparing the graphene multifunctional antiviral and antibacterial soft chip according to claim 1, wherein the soft finishing in step (5) is performed by using an amino silicone oil emulsion soft finishing agent, and the soft finishing step comprises: 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 mangling rate is 70% -80%, then placing the obtained product into an oven to be dried at 85-95 ℃, and shaping for 20-60 s at 150-170 ℃ to obtain the graphene multifunctional antiviral and antibacterial soft chip.
10. A graphene multifunctional antiviral and antibacterial soft chip, which is prepared by the method of any one of claims 1 to 9.
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