CN110863263A - Composite garment fabric with efficient and lasting antibacterial performance - Google Patents
Composite garment fabric with efficient and lasting antibacterial performance Download PDFInfo
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- CN110863263A CN110863263A CN201911160247.9A CN201911160247A CN110863263A CN 110863263 A CN110863263 A CN 110863263A CN 201911160247 A CN201911160247 A CN 201911160247A CN 110863263 A CN110863263 A CN 110863263A
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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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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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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Abstract
The invention discloses a composite garment fabric with efficient and lasting antibacterial performance, which comprises the following steps: 1) preparing fumaric acid modified polybutylene succinate from 1, 4-butanedioic acid, 1, 4-butanediol and fumaric acid; 2) preparing organic metal framework polybutylene succinate by using the product in the step 1) and aluminum nitrate nonahydrate; 3) preparing a nano silver/graphene oxide compound by using silver nitrate, polyvinylpyrrolidone, ethanol and graphene oxide; 4) adding the compound into dimethylformamide, oscillating and dispersing, and then adding the product obtained in the step 2) to obtain modified organic metal framework polybutylene succinate; 5) mixing the product obtained in the step 4) with cotton fiber, silane coupling agent, maleic anhydride and sodium hydroxide, stirring in a water bath, then putting the mixture and polyester fiber into a screw extruder, and processing to obtain the polyester fiber. The garment material has high-efficiency and lasting excellent antibacterial effect, and meanwhile, the comfort level and the fabric strength of the garment material can well meet the requirements of people, so that the garment material has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of textile fabrics, and particularly relates to a composite garment fabric with efficient and lasting antibacterial performance.
Background
The garment is made of the fabric, the fabric is used for making the garment and serves as one of three elements of the garment, the fabric can explain the style and the characteristics of the garment, the appearance of the color and the shape of the garment is directly controlled, the garment presents the advantages of high price, perfect appearance and soft hand feeling. The existing fabrics are various in variety, but with the improvement of living standard of people, a new variety capable of meeting the needs of different people needs to be provided, the requirements of people on the clothes not only meet the requirements on clothes styles and workmanship, but also meet the requirements on clothes quality, so that the development of clothes forms needs to be followed on the clothes fabrics, and the characteristics of the fabrics with functions, comfort, environmental protection, health and the like become the focus of more and more attention of people, so that the composite clothes fabrics with antibacterial function are held by people.
Chinese patent CN2019103592456 discloses a composite material garment fabric with an antibacterial function, which is obtained by padding the garment fabric in an antibacterial finishing agent, and although the antibacterial requirement can be met in the early stage, the antibacterial garment fabric obtained by padding is easy to cause loss of antibacterial components attached to the fabric along with continuous washing in the use process, so that the antibacterial effect is weakened, and the requirement of long-term use of people cannot be met; chinese patent CN2018106605400 discloses a flame-retardant antibacterial high-performance garment fabric and a preparation method thereof, an antibacterial complexing agent and a fiber raw material are mixed and spun, then twisted into fine sand, and then processed to obtain the antibacterial garment fabric, the antibacterial complexing agent is attached to the surface of the fiber to obtain the fiber with antibacterial effect, and then blended to obtain the antibacterial garment fabric, the antibacterial garment fabric still has the phenomenon of loss of the antibacterial complexing agent in the washing process, and still cannot meet the long-term requirements of people.
Disclosure of Invention
The invention aims to provide a composite garment fabric with efficient and durable antibacterial performance aiming at the existing problems.
The invention is realized by the following technical scheme:
a composite garment fabric with efficient and durable antibacterial performance is prepared by the following specific steps:
1) adding a certain amount of 1, 4-succinic acid, 1, 4-butanediol and fumaric acid into a reactor, adding a small amount of tin dichloride, heating to 185 ℃ under the protection of nitrogen, dehydrating for 2-3h, then vacuum-heating to 240 ℃ under 230 ℃ under constant temperature for reaction for 3-4h, cooling to room temperature, purifying the obtained product with chloroform, and vacuum-drying at 45-55 ℃ for 20-25h to obtain fumaric acid modified polybutylene succinate; the method adopts 1, 4-succinic acid and 1, 4-butanediol as raw materials for preparing the polybutylene succinate, and adds a fumaric acid monomer with an unsaturated bond in a molecular main chain of the polybutylene succinate, thereby obtaining a polybutylene succinate copolymer containing the unsaturated bond;
2) adding fumaric acid modified polybutylene succinate into a tetrahydrofuran solution, stirring and dissolving at 45-50 ℃ to obtain a solution A, adding aluminum nitrate nonahydrate into deionized water, stirring and dissolving at normal temperature to obtain a solution B, dropwise adding the solution A into the solution B, stirring and reacting at the rotation speed of 150-200r/min for 1-2h at 50-55 ℃ after dropwise adding, centrifugally separating the obtained suspension, alternately cleaning the product with deionized water and absolute ethyl alcohol for 3-5 times, and drying to obtain the organic metal skeleton polybutylene succinate; aluminum nitrate nonahydrate is used as a metal source, fumaric acid contained in fumaric acid modified polybutylene succinate is used as an organic ligand, and the organic metal skeleton polybutylene succinate with metal aluminum as a skeleton material is prepared through reaction;
3) mixing silver nitrate, polyvinylpyrrolidone and ethanol, adding the mixture into a reactor, stirring the mixture until the mixture is dissolved, adding graphene oxide into the reactor, oscillating and dispersing the mixture for 15 to 25 minutes under 300-400W ultrasonic wave, transferring the mixture into a reaction kettle, reacting the mixture for 20 to 24 hours at 195 ℃ of 180-DEG, cooling the mixture to room temperature after the reaction is completed, repeatedly centrifuging and washing the reaction product for 3 to 4 times by using ethanol, and drying the washed product for 8 to 12 hours in vacuum at 50 to 60 ℃ to obtain a nano silver/graphene oxide compound; the method has the advantages that ethanol is used as a solvent, polyvinylpyrrolidone is used as a template agent, graphene oxide is used as a platform, and a solvothermal method is adopted, so that nano silver particles nucleate and grow on the surface of graphene oxide folds, and a nano silver/graphene oxide compound is formed;
4) adding a nano silver/graphene oxide compound into a dimethylformamide solution, oscillating and dispersing for 10-15min under 350-450W ultrasonic waves, then adding polybutylene succinate with an organic metal framework, stirring for 15-25min at the rotating speed of 300-400r/min, then stirring and reacting for 16-19h at the rotating speed of 100-130r/min under the condition of 130-145 ℃, cooling to room temperature, filtering, sequentially and respectively washing for 3-4 times by using dimethylformamide and a methanol solution, and drying for 15-20h at the temperature of 80-100 ℃ to obtain the modified polybutylene succinate with the organic metal framework; the invention utilizes the oxygen-containing functional group in the nano-silver/graphene oxide compound to react with the hydroxyl in the organic metal framework polybutylene succinate, so that the metal aluminum crystal in the organic metal framework polybutylene succinate grows compactly on the upper surface and the lower surface of the nano-silver/graphene oxide compound, the organic metal framework polybutylene succinate is attached to the micropores of the pore channel structures on the upper surface and the lower surface of the compound to form a three-layer structure similar to a sandwich structure, on one hand, the invention not only can play a certain role in protecting and fixing, can prevent the nano-silver particles filled in the compound from losing, but also the semi-coating polymer layer formed on the surface of the compound can not influence the antibacterial effect of the nano-silver, on the other hand, because the pore channel structure of the organic metal framework polybutylene succinate is mostly micropores, the function of chemical bonds is realized, the composite with proper nano-silver loading capacity is combined with the organic metal framework polybutylene succinate, so that the specific surface area and the pore volume of the obtained modified organic metal framework polybutylene succinate can be further improved, the antibacterial efficiency can be improved, and the antibacterial effect can be enhanced;
5) mixing cotton fibers, modified organic metal skeleton polybutylene succinate, a silane coupling agent, maleic anhydride and a sodium hydroxide solution, then placing the mixture in a water bath at 70-80 ℃, stirring the mixture for 1.5-2.5 hours at the speed of 600-; the added alkali liquor and the added maleic anhydride can play a role in grafting enhancement, wherein the alkali liquor can have a certain swelling effect on cotton fibers, the effective contact area of the cotton fibers and the modified organic metal skeleton polybutylene succinate is increased, the bonding granularity of an interface is increased, the biting force between the cotton fibers and the modified organic metal skeleton polybutylene succinate is improved, the maleic anhydride can be grafted with the cotton fibers under a proper condition to obtain a polymer, and a polar group aldehyde group and an olefin nonpolar chain segment provided by the maleic anhydride can play a role in coupling compatibility, so that the compatibility between the two is improved, the interface bonding force is increased, and the tensile strength of the obtained antibacterial composite fibers is improved;
preferably, the composite garment fabric with efficient and durable antibacterial performance is prepared in the step 1), wherein the ratio of the total amount of 1, 4-succinic acid and fumaric acid to 1, 4-butanediol is 1:1.02-1.08, wherein the amount of fumaric acid accounts for 2-5% of 1, 4-succinic acid; the addition amount of the tin dichloride is 1-2% of the total weight of the reaction system.
Preferably, the composite garment fabric with efficient and durable antibacterial performance comprises the following steps of 2), wherein the solution A accounts for 6-10% by mass, and the solution B accounts for 7-12% by mass; the rotation speed of the centrifugal separation is 5000-7000r/min, and the centrifugal time is 15-20 min; the drying temperature is 50-60 ℃, and the drying time is 10-15 h.
Preferably, the composite clothing fabric with efficient and durable antibacterial performance is prepared in the step 3), wherein in the reaction system, the mass-to-volume ratio of silver nitrate, polyvinylpyrrolidone, graphene oxide and ethanol is 3-4g:5-5.5g:1g:320-360ml, wherein the ethanol is absolute ethanol.
Preferably, in the preparation step 4), the mass-volume ratio of the nano-silver/graphene oxide compound to the dimethylformamide solution is 1:45-65g/ml, wherein the addition amount of the nano-silver/graphene oxide compound accounts for 2.5-8.0% of the finally obtained modified organic metal skeleton polybutylene succinate.
Preferably, in the preparation step 5), the mass ratio of the cotton fiber, the modified organic metal skeleton polybutylene succinate, the maleic anhydride, the silane coupling agent, the sodium hydroxide solution and the polyester fiber is 80-100:15-25:3-6:2-3:20-35:8-15, wherein the concentration of the sodium hydroxide solution is 2-6%; the melting temperature is 165-190 ℃, the spinning temperature of the spinning box is 235-255 ℃, and the spinning speed is 2800-3200 m/min; the warp density of the antibacterial composite garment fabric is 70-85 pieces/cm, and the weft density is 50-65 pieces/cm.
Compared with the prior art, the invention has the following advantages:
according to the composite garment fabric with the antibacterial function, the nano silver with the antibacterial function is loaded in the graphene oxide to obtain the composite, then the composite reacts with the organic metal skeleton polybutylene succinate to form the modified organic metal skeleton polybutylene succinate with a sandwich-like structure, on one hand, the loss of nano silver particles filled in the composite can be prevented, the antibacterial durability is improved, on the other hand, the antibacterial efficiency can be improved, the antibacterial effect is enhanced, the antibacterial polymer reacts with cotton fibers and then is subjected to melt spinning with the polyester fibers, and the efficient and durable antibacterial fabric can be obtained.
Detailed Description
The present invention will be further described with reference to specific embodiments.
Example 1
A composite garment fabric with efficient and durable antibacterial performance is prepared by the following specific steps:
1) adding a certain amount of 1, 4-succinic acid, 1, 4-butanediol and fumaric acid into a reactor, adding a small amount of tin dichloride, heating to 170 ℃ under the protection of nitrogen, dehydrating for 3h, then heating to 230 ℃ in vacuum, reacting at constant temperature for 4h, cooling to room temperature, purifying the obtained product with chloroform, and drying at 45 ℃ in vacuum for 25h to obtain fumaric acid modified polybutylene succinate;
2) adding fumaric acid modified polybutylene succinate into a tetrahydrofuran solution, stirring and dissolving at 50 ℃ to obtain a solution A, adding aluminum nitrate nonahydrate into deionized water, stirring and dissolving at normal temperature to obtain a solution B, dropwise adding the solution A into the solution B, stirring at the rotating speed of 150r/min for 20min after dropwise adding, performing centrifugal separation on the obtained suspension, alternately cleaning the product for 3 times by using deionized water and absolute ethyl alcohol, and drying to obtain organic metal skeleton polybutylene succinate;
3) mixing silver nitrate, polyvinylpyrrolidone and ethanol, adding the mixture into a reactor, stirring the mixture until the mixture is dissolved, adding graphene oxide into the reactor, oscillating and dispersing the mixture for 25min under 300W ultrasonic waves, transferring the mixture into a reaction kettle, reacting the mixture for 24h at 180 ℃, cooling the reaction product to room temperature after the reaction is completed, repeatedly centrifuging and washing the reaction product for 3 times by using ethanol, and drying the washed product for 12h in vacuum at 50 ℃ to obtain a nano silver/graphene oxide compound;
4) adding a nano silver/graphene oxide compound into a dimethylformamide solution, oscillating and dispersing for 10min under 350W ultrasonic waves, then adding organic metal framework polybutylene succinate, stirring for 25min at the rotating speed of 300r/min, then stirring for reacting for 19h at the rotating speed of 100r/min at the temperature of 130 ℃, cooling to room temperature, filtering, sequentially and respectively washing for 3 times by using the dimethylformamide solution and a methanol solution, and drying for 20h at the temperature of 80 ℃ to obtain modified organic metal framework polybutylene succinate;
5) mixing cotton fibers, modified organic metal skeleton polybutylene succinate, a silane coupling agent, maleic anhydride and a sodium hydroxide solution, placing the mixture in a water bath at 70 ℃, stirring the mixture for 2.5 hours at 600r/min, then placing the mixture and polyester fibers into a screw extruder, melting the mixture, extruding the mixture through a spinning nozzle of a spinning box, cooling and solidifying the mixture to obtain antibacterial composite fibers, and then spinning the antibacterial composite fibers to obtain the antibacterial composite garment material.
Preferably, in the preparation step 1), the ratio of the total amount of the 1, 4-succinic acid and the fumaric acid to the 1, 4-butanediol is 1:1.02, wherein the amount of the fumaric acid accounts for 2 percent of the 1, 4-succinic acid; the addition amount of the tin dichloride is 1 percent of the total weight of the reaction system.
Preferably, in the preparation step 2), the mass fraction of the solution A is 6%, and the mass fraction of the solution B is 7%; the rotation speed of the centrifugal separation is 5000r/min, and the centrifugal time is 20 min; the drying temperature is 50 ℃, and the drying is carried out for 15 h.
Preferably, in the preparation step 3), the mass-to-volume ratio of the silver nitrate, the polyvinylpyrrolidone, the graphene oxide and the ethanol in the reaction system is 3g:5g:1g:320ml, and the ethanol is absolute ethanol.
Preferably, in the preparation step 4), the mass-to-volume ratio of the nano-silver/graphene oxide composite to the dimethylformamide solution is 1:45g/ml, wherein the addition amount of the nano-silver/graphene oxide composite accounts for 2.5% of the finally obtained modified organic metal skeleton polybutylene succinate.
Preferably, in the preparation step 5), the mass ratio of the cotton fiber, the modified organic metal skeleton polybutylene succinate, the maleic anhydride, the silane coupling agent, the sodium hydroxide solution and the polyester fiber is 80:15:3:2:20:8, wherein the concentration of the sodium hydroxide solution is 2%; the melting temperature is 165 ℃, the spinning temperature of the spinning box is 235 ℃, and the spinning speed is 2800 m/min; the warp density of the antibacterial composite garment fabric is 70 pieces/cm, and the weft density is 50 pieces/cm.
And (3) evaluating the antibacterial performance of the fabric prepared by the method according to GB/T20944.3-2008 GBT20944.3-2008 textile: and (2) performing standard test of oscillation method, performing antibacterial effect test on staphylococcus aureus, escherichia coli and candida albicans to obtain the antibacterial rate of 98.2%, continuously washing the fabric in a washing machine for 48 hours, drying, and performing the antibacterial effect test again to obtain the antibacterial rate of 97.5%.
Example 2
A composite garment fabric with efficient and durable antibacterial performance is prepared by the following specific steps:
1) adding a certain amount of 1, 4-succinic acid, 1, 4-butanediol and fumaric acid into a reactor, adding a small amount of stannic chloride, heating to 175 ℃ under the protection of nitrogen, dehydrating for 2.5h, then heating to 235 ℃ in vacuum, reacting at constant temperature for 3.5h, cooling to room temperature, purifying the obtained product with chloroform, and drying at 50 ℃ in vacuum for 23h to obtain fumaric acid modified polybutylene succinate;
2) adding fumaric acid modified polybutylene succinate into a tetrahydrofuran solution, stirring and dissolving at 52 ℃ to obtain a solution A, adding aluminum nitrate nonahydrate into deionized water, stirring and dissolving at normal temperature to obtain a solution B, dropwise adding the solution A into the solution B, stirring at the rotating speed of 180r/min for 15min after dropwise adding, performing centrifugal separation on the obtained suspension, alternately cleaning the product with deionized water and absolute ethyl alcohol for 4 times, and drying to obtain organic metal skeleton polybutylene succinate;
3) mixing silver nitrate, polyvinylpyrrolidone and ethanol, adding the mixture into a reactor, stirring the mixture until the mixture is dissolved, adding graphene oxide into the reactor, oscillating the mixture under 350W ultrasonic waves for 20min, transferring the mixture into a reaction kettle, reacting the mixture for 21h at 185 ℃, cooling the reaction product to room temperature after the reaction is completed, repeatedly centrifuging and washing the reaction product for 3 times by using ethanol, and drying the washed product for 10h at 55 ℃ in vacuum to obtain a nano silver/graphene oxide compound;
4) adding a nano silver/graphene oxide compound into a dimethylformamide solution, oscillating and dispersing for 12min under 400W ultrasonic waves, then adding organic metal framework polybutylene succinate, stirring for 20min at the rotation speed of 350r/min, then stirring for reacting for 17h at the rotation speed of 120r/min at the temperature of 135 ℃, cooling to room temperature, filtering, sequentially and respectively washing for 3 times by using the dimethylformamide solution and a methanol solution, and drying for 18h at the temperature of 90 ℃ to obtain modified organic metal framework polybutylene succinate;
5) mixing cotton fibers, modified organic metal skeleton polybutylene succinate, a silane coupling agent, maleic anhydride and a sodium hydroxide solution, placing the mixture in a water bath at 75 ℃, stirring the mixture for 2 hours at 700r/min, then placing the mixture and polyester fibers into a screw extruder, melting the mixture, extruding the mixture through a spinning nozzle of a spinning box, cooling and solidifying the mixture to obtain antibacterial composite fibers, and then spinning the antibacterial composite fibers to obtain the antibacterial composite garment fabric.
Preferably, in the preparation step 1), the ratio of the total amount of the 1, 4-succinic acid and the fumaric acid to the 1, 4-butanediol is 1:1.05, wherein the amount of the fumaric acid accounts for 3 percent of the 1, 4-succinic acid; the addition amount of the tin dichloride is 1.5 percent of the total weight of the reaction system.
Preferably, in the preparation step 2), the mass fraction of the solution A is 8%, and the mass fraction of the solution B is 10%; the rotation speed of the centrifugal separation is 600r/min, and the centrifugal time is 18 min; the drying temperature is 55 ℃, and the drying is carried out for 12 hours.
Preferably, in the preparation step 3), the mass-to-volume ratio of the silver nitrate, the polyvinylpyrrolidone, the graphene oxide and the ethanol in the reaction system is 3.5g:5.2g:1g:340ml, wherein the ethanol is absolute ethanol.
Preferably, in the preparation step 4), the mass-to-volume ratio of the nano-silver/graphene oxide composite to the dimethylformamide solution is 1:55g/ml, wherein the addition amount of the nano-silver/graphene oxide composite accounts for 6.5% of the finally obtained modified organic metal skeleton polybutylene succinate.
Preferably, in the preparation step 5), the mass ratio of the cotton fiber, the modified organic metal skeleton polybutylene succinate, the maleic anhydride, the silane coupling agent, the sodium hydroxide solution and the polyester fiber is 90:20:5:2.5:28:12, wherein the concentration of the sodium hydroxide solution is 3%; the melting temperature is 175 ℃, the spinning temperature of the spinning box is 245 ℃, and the spinning speed is 3000 m/min; the warp density of the antibacterial composite garment fabric is 80 pieces/cm, and the weft density is 60 pieces/cm.
And (3) evaluating the antibacterial performance of the fabric prepared by the method according to GB/T20944.3-2008 GBT20944.3-2008 textile: and (2) performing standard test of oscillation method, performing antibacterial effect test on staphylococcus aureus, escherichia coli and candida albicans to obtain the antibacterial rate of 98.9%, continuously washing the fabric in a washing machine for 48 hours, drying, and performing the antibacterial effect test again to obtain the antibacterial rate of 98.1%.
Example 3
A composite garment fabric with efficient and durable antibacterial performance is prepared by the following specific steps:
1) adding a certain amount of 1, 4-succinic acid, 1, 4-butanediol and fumaric acid into a reactor, adding a small amount of stannic chloride, heating to 185 ℃ under the protection of nitrogen, dehydrating for 2h, then heating to 240 ℃ in vacuum, reacting at constant temperature for 3h, cooling to room temperature, purifying the obtained product with chloroform, and drying at 55 ℃ in vacuum for 20h to obtain fumaric acid modified polybutylene succinate;
2) adding fumaric acid modified polybutylene succinate into a tetrahydrofuran solution, stirring and dissolving at 55 ℃ to obtain a solution A, adding aluminum nitrate nonahydrate into deionized water, stirring and dissolving at normal temperature to obtain a solution B, dropwise adding the solution A into the solution B, stirring at the rotating speed of 200r/min for 10min after dropwise adding, performing centrifugal separation on the obtained suspension, alternately cleaning the product with deionized water and absolute ethyl alcohol for 5 times, and drying to obtain organic metal skeleton polybutylene succinate;
3) mixing silver nitrate, polyvinylpyrrolidone and ethanol, adding the mixture into a reactor, stirring the mixture until the mixture is dissolved, adding graphene oxide into the reactor, oscillating the mixture under 400W ultrasonic waves for dispersing the mixture for 15min, transferring the mixture into a reaction kettle, reacting the mixture for 20h at 195 ℃, cooling the mixture to room temperature after the reaction is completed, repeatedly centrifuging and washing the reaction product for 4 times by using ethanol, and drying the washed product for 8h under vacuum at 60 ℃ to obtain a nano silver/graphene oxide compound;
4) adding a nano silver/graphene oxide compound into a dimethylformamide solution, oscillating and dispersing for 10min under 450W ultrasonic waves, then adding organic metal framework polybutylene succinate, stirring for 15min at the rotation speed of 400r/min, then stirring and reacting for 19h at the rotation speed of 100r/min at the temperature of 145 ℃, cooling to room temperature, filtering, sequentially and respectively washing for 4 times by using the dimethylformamide solution and a methanol solution, and drying for 15h at the temperature of 100 ℃ to obtain modified organic metal framework polybutylene succinate;
5) mixing cotton fibers, modified organic metal skeleton polybutylene succinate, a silane coupling agent, maleic anhydride and a sodium hydroxide solution, placing the mixture in a water bath at 80 ℃, stirring the mixture for 1.5 hours at 800r/min, then placing the mixture and polyester fibers into a screw extruder, melting the mixture, extruding the mixture through a spinning nozzle of a spinning box, cooling and solidifying the mixture to obtain antibacterial composite fibers, and then spinning the antibacterial composite fibers to obtain the antibacterial composite garment material.
Preferably, in the preparation step 1), the ratio of the total amount of the 1, 4-succinic acid and the fumaric acid to the 1, 4-butanediol is 1:1.08, wherein the amount of the fumaric acid accounts for 5 percent of the 1, 4-succinic acid; the addition amount of the tin dichloride is 2 percent of the total weight of the reaction system.
Preferably, in the preparation step 2), the mass fraction of the solution A is 10%, and the mass fraction of the solution B is 12%; the rotating speed of the centrifugal separation is 7000r/min, and the centrifugal time is 15 min; the drying temperature is 60 ℃, and the drying time is 10 hours.
Preferably, in the preparation step 3), the mass-to-volume ratio of the silver nitrate, the polyvinylpyrrolidone, the graphene oxide and the ethanol in the reaction system is 4g:5.5g:1g:360ml, wherein the ethanol is absolute ethanol.
Preferably, in the preparation step 4), the mass-to-volume ratio of the nano-silver/graphene oxide composite to the dimethylformamide solution is 1:65g/ml, wherein the addition amount of the nano-silver/graphene oxide composite accounts for 8.0% of the finally obtained modified organic metal skeleton polybutylene succinate.
Preferably, in the preparation step 5), the mass ratio of the cotton fiber, the modified organic metal skeleton polybutylene succinate, the maleic anhydride, the silane coupling agent, the sodium hydroxide solution and the polyester fiber is 100:25:6:3:35:15, wherein the concentration of the sodium hydroxide solution is 6%; the melting temperature is 190 ℃, the spinning temperature of the spinning box is 255 ℃, and the spinning speed is 3200 m/min; the warp density of the antibacterial composite garment fabric is 85 pieces/cm, and the weft density is 65 pieces/cm.
And (3) evaluating the antibacterial performance of the fabric prepared by the method according to GB/T20944.3-2008 GBT20944.3-2008 textile: and (2) performing standard test of oscillation method, performing antibacterial effect test on staphylococcus aureus, escherichia coli and candida albicans to obtain the antibacterial rate of 98.4%, continuously washing the fabric in a washing machine for 48 hours, drying, and performing the antibacterial effect test again to obtain the antibacterial rate of 97.8%.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention.
Claims (6)
1. The composite garment fabric with the efficient and durable antibacterial performance is characterized by comprising the following specific preparation methods:
1) adding a certain amount of 1, 4-succinic acid, 1, 4-butanediol and fumaric acid into a reactor, adding a small amount of tin dichloride, heating to 185 ℃ under the protection of nitrogen, dehydrating for 2-3h, then vacuum-heating to 240 ℃ under 230 ℃ under constant temperature for reaction for 3-4h, cooling to room temperature, purifying the obtained product with chloroform, and vacuum-drying at 45-55 ℃ for 20-25h to obtain fumaric acid modified polybutylene succinate;
2) adding fumaric acid modified polybutylene succinate into a tetrahydrofuran solution, stirring and dissolving at 50-55 ℃ to obtain a solution A, adding aluminum nitrate nonahydrate into deionized water, stirring and dissolving at normal temperature to obtain a solution B, dropwise adding the solution A into the solution B, stirring at the rotation speed of 150-200r/min for 10-20min after the dropwise adding is finished, performing centrifugal separation on the obtained suspension, alternately cleaning the product with deionized water and absolute ethyl alcohol for 3-5 times, and drying to obtain organic metal skeleton polybutylene succinate;
3) mixing silver nitrate, polyvinylpyrrolidone and ethanol, adding the mixture into a reactor, stirring the mixture until the mixture is dissolved, adding graphene oxide into the reactor, oscillating and dispersing the mixture for 15 to 25 minutes under 300-400W ultrasonic wave, transferring the mixture into a reaction kettle, reacting the mixture for 20 to 24 hours at 195 ℃ of 180-DEG, cooling the mixture to room temperature after the reaction is completed, repeatedly centrifuging and washing the reaction product for 3 to 4 times by using ethanol, and drying the washed product for 8 to 12 hours in vacuum at 50 to 60 ℃ to obtain a nano silver/graphene oxide compound;
4) adding a nano silver/graphene oxide compound into a dimethylformamide solution, oscillating and dispersing for 10-15min under 350-450W ultrasonic waves, then adding polybutylene succinate with an organic metal framework, stirring for 15-25min at the rotating speed of 300-400r/min, then stirring and reacting for 16-19h at the rotating speed of 100-130r/min under the condition of 130-145 ℃, cooling to room temperature, filtering, sequentially and respectively washing for 3-4 times by using dimethylformamide and a methanol solution, and drying for 15-20h at the temperature of 80-100 ℃ to obtain the modified polybutylene succinate with the organic metal framework;
5) mixing cotton fiber, modified organic metal skeleton polybutanediol succinate, silane coupling agent, maleic anhydride and sodium hydroxide solution, placing the mixture in water bath at 70-80 ℃, stirring for 1.5-2.5h at the speed of 600-.
2. The composite garment fabric with efficient and durable antibacterial performance as claimed in claim 1, wherein in the preparation step 1), the ratio of the total content of the 1, 4-succinic acid and the fumaric acid to the 1, 4-butanediol is 1:1.02-1.08, wherein the content of the fumaric acid accounts for 2-5% of the 1, 4-succinic acid; the addition amount of the tin dichloride is 1-2% of the total weight of the reaction system.
3. The composite garment fabric with efficient and durable antibacterial performance as claimed in claim 1, wherein in the preparation step 2), the mass fraction of the solution A is 6-10%, and the mass fraction of the solution B is 7-12%; the rotation speed of the centrifugal separation is 5000-7000r/min, and the centrifugal time is 15-20 min; the drying temperature is 50-60 ℃, and the drying time is 10-15 h.
4. The composite garment material with efficient and durable antibacterial performance as claimed in claim 1, wherein in the preparation step 3), the mass-to-volume ratio of silver nitrate, polyvinylpyrrolidone, graphene oxide and ethanol in the reaction system is 3-4g:5-5.5g:1g:320-360ml, wherein the ethanol is absolute ethanol.
5. The composite garment fabric with efficient and durable antibacterial performance according to claim 1, wherein in the preparation step 4), the mass-to-volume ratio of the nano-silver/graphene oxide composite to the dimethylformamide solution is 1:45-65g/ml, and the addition amount of the nano-silver/graphene oxide composite accounts for 2.5-8.0% of the finally obtained modified organic metal skeleton polybutylene succinate.
6. The composite garment fabric with efficient and durable antibacterial performance as claimed in claim 1, wherein in the preparation step 5), the mass ratio of the cotton fibers, the modified organic metal skeleton polybutylene succinate, the maleic anhydride, the silane coupling agent, the sodium hydroxide solution and the polyester fibers is 80-100:15-25:3-6:2-3:20-35:8-15, wherein the concentration of the sodium hydroxide solution is 2-6%; the melting temperature is 165-190 ℃, the spinning temperature of the spinning box is 235-255 ℃, and the spinning speed is 2800-3200 m/min; the warp density of the antibacterial composite garment fabric is 70-85 pieces/cm, and the weft density is 50-65 pieces/cm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112981662A (en) * | 2021-02-04 | 2021-06-18 | 江苏厚生新能源科技有限公司 | Antibacterial radiation-proof polyethylene composite fabric and preparation process thereof |
| CN113308876A (en) * | 2021-05-27 | 2021-08-27 | 宁波市富罗迷鞋业有限公司 | Children garment fabric and preparation method thereof |
| CN114717836A (en) * | 2022-04-28 | 2022-07-08 | 杭州萧山东达纺织有限公司 | Silver silk fabric and preparation method thereof |
| CN116121930A (en) * | 2023-02-27 | 2023-05-16 | 亿吉万(深圳)新材料科技有限公司 | Moisture-absorbing antibacterial textile |
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2019
- 2019-11-23 CN CN201911160247.9A patent/CN110863263A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112981662A (en) * | 2021-02-04 | 2021-06-18 | 江苏厚生新能源科技有限公司 | Antibacterial radiation-proof polyethylene composite fabric and preparation process thereof |
| CN113308876A (en) * | 2021-05-27 | 2021-08-27 | 宁波市富罗迷鞋业有限公司 | Children garment fabric and preparation method thereof |
| CN114717836A (en) * | 2022-04-28 | 2022-07-08 | 杭州萧山东达纺织有限公司 | Silver silk fabric and preparation method thereof |
| CN114717836B (en) * | 2022-04-28 | 2024-04-19 | 杭州萧山东达纺织有限公司 | Silver yarn fabric and preparation method thereof |
| CN116121930A (en) * | 2023-02-27 | 2023-05-16 | 亿吉万(深圳)新材料科技有限公司 | Moisture-absorbing antibacterial textile |
| CN116121930B (en) * | 2023-02-27 | 2023-11-03 | 亿吉万(深圳)新材料科技有限公司 | Moisture-absorbing antibacterial textile |
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