CN110565199A - Preparation method and application of fiber with warm-keeping and bacteriostatic functions - Google Patents
Preparation method and application of fiber with warm-keeping and bacteriostatic functions Download PDFInfo
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- CN110565199A CN110565199A CN201910849893.XA CN201910849893A CN110565199A CN 110565199 A CN110565199 A CN 110565199A CN 201910849893 A CN201910849893 A CN 201910849893A CN 110565199 A CN110565199 A CN 110565199A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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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
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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Abstract
The invention relates to the technical field of functional textile fibers, in particular to a preparation method and application of a warm-keeping bacteriostatic functional fiber, S1, preparing functional powder; s2, preparing functional polyester chips: putting functional powder, terephthalic acid and ethylene glycol into a container, adding a catalyst, an ether inhibitor and an antioxidant into the container, pulping to prepare pulping liquid, then carrying out pressurized esterification reaction on the pulping liquid to prepare esterified pulp, carrying out pre-polycondensation reaction and final polycondensation reaction on the esterified pulp, and carrying out melt granulation to prepare functional polyester chips; s3, preparing the fiber with the functions of heat preservation and bacteriostasis: and (3) performing high-pressure melting extrusion on the functional polyester chips, cooling by circular air blowing, bundling and oiling, drafting and heat setting, and winding to prepare the thermal-insulation antibacterial functional fiber. The invention improves the preparation efficiency and the heat-insulating and bacteriostatic performance of the heat-insulating and bacteriostatic functional fiber, overcomes the defects of low preparation efficiency and insufficient performance of the functional fiber in the prior art, and achieves the aim of efficiently preparing the heat-insulating and bacteriostatic functional fiber.
Description
Technical Field
The invention relates to the technical field of functional textile fibers, in particular to a preparation method and application of a thermal-insulation bacteriostatic functional fiber.
background
At present, many women have the conditions of cold womb and cold stomach, which cause many female diseases; the heat preservation is an important means for relieving the menstrual pain of the female and protecting the body health of the female at present. The existing warm-keeping functional fiber is mainly prepared by adopting fiber special-shaped section design and adding warm-keeping functional powder such as far infrared and the like to realize the warm-keeping function of the fiber; the hollow fibers, especially the hollow filaments, can enrich the fibers with a large amount of still air, thereby increasing thermal resistance and reducing heat loss through heat conduction. The fabric is also a novel fiber with moisture absorption and sweat releasing functions, has a special-shaped section, and can absorb moisture of sweat and moisture on the surface of skin and rapidly conduct the moisture to the surface of clothing, so that the evaporation of the moisture is accelerated. And because of the unique hollow section structure, the utility model has the characteristics of light weight, softness, comfort and the like, thereby being widely applied to underwear, sports clothes, curtains and the like. With the continuous and deep research, single hollow is also developed into three-hole, four-hole or even six-hole terylene fiber, and also hollow profiled fiber, and the corresponding heat preservation performance is also continuously improved with the development of technology. The far infrared powder has the problems of low fiber strength, easy generation of floating and broken ends in spinning and the like due to the fact that the far infrared powder is difficult to add and disperse in the spinning process, and the like, so that the production efficiency of the existing functional fiber containing the far infrared powder is low, the quality is not high, and the performance is not enough.
Disclosure of Invention
In view of the above, the invention provides a preparation method and application of a thermal-insulation bacteriostatic functional fiber, so as to solve the defects of low preparation efficiency and insufficient performance of the functional fiber in the prior art.
The invention discloses a preparation method of a fiber with warm-keeping and bacteriostatic functions, which comprises the following steps:
s1, preparing functional powder: s11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use; s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution; s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified; s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for several hours; s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for a plurality of hours, filtering, and washing with deionized water for a plurality of times to obtain filter residue; s16, calcining the filter residue in an aerobic environment at 450-750 ℃ for several hours, and then calcining in an aerobic environment at 800-1000 ℃ to prepare the functional powder.
s2, preparing functional polyester chips: putting functional powder, terephthalic acid and ethylene glycol into a container, adding a catalyst, an ether inhibitor and an antioxidant into the container, pulping to prepare pulping liquid, then carrying out pressurized esterification reaction on the pulping liquid to prepare esterified pulp, carrying out pre-polycondensation reaction and final polycondensation reaction on the esterified pulp, and carrying out melt granulation to prepare functional polyester chips;
S3, preparing the fiber with the functions of heat preservation and bacteriostasis: and (3) performing high-pressure melting extrusion on the functional polyester chips, cooling by circular air blowing, bundling and oiling, drafting and heat setting, and winding to prepare the thermal-insulation antibacterial functional fiber.
As a preferable scheme of the present invention, in the step S11, the mass fraction of bismuth nitrate in the bismuth nitrate solution is 5 to 15%; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 5-15%; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 5 to 15%.
In a preferred embodiment of the present invention, in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1:0.25 to 1: 0.50.
In a preferred embodiment of the present invention, in the step S15, the addition amount of the tungsten nitrate powder is 5 to 10% by mass of the functional powder precursor solution.
In a preferred embodiment of the present invention, in the step S2, the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.05 to 1.25; the mass ratio of the functional powder to the glycol is 1: 50-200; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the antioxidant was 0.05% by mass relative to terephthalic acid.
In a preferred embodiment of the present invention, in step S2, the catalyst is ethylene glycol antimony, the anti-ether agent is sodium acetate, and the antioxidant is triphenyl phosphate.
In the step S2, in the pressure esterification process, the pressure is 0.35 to 0.45MPa, the esterification temperature is 230 to 245 ℃, and the esterification time is 2.5 to 3.0 hours; the pre-polycondensation reaction is normal-pressure polycondensation, the pre-polycondensation temperature is 250-260 ℃, and the pre-polycondensation time is 0.5-1.5 h.
In a preferred embodiment of the present invention, in step S2, the final polycondensation reaction is a vacuum polycondensation, which is performed first by a low vacuum polycondensation and then by a high vacuum polycondensation; the vacuum degree of the low vacuum polycondensation is 500-5000 Pa, the low vacuum polycondensation time is 0.5-1.0 h, the vacuum degree of the high vacuum polycondensation is 50-100 Pa, and the high vacuum polycondensation time is 1.0-3.0 h.
The invention also discloses an application of the warm-keeping bacteriostatic functional fiber, and the prepared warm-keeping bacteriostatic functional fiber is applied to cloth.
the prepared heat-insulating bacteriostatic functional fiber has the bacteriostatic rate of 95-99% on staphylococcus aureus and the bacteriostatic rate of 95-98% on escherichia coli; the far infrared emissivity at the wavelength of 1.0-5.0 microns is 20-50%, the heat insulation performance of a fabric sample prepared by the heat-insulation and bacteriostatic functional fiber is subjected to heat radiation for 1min at the temperature of 100 ℃ (15cm), the surface temperature difference of the fabric sample before and after heating is 1.0-2.0 ℃, and the surface temperature of the fabric is higher than 100 ℃.
according to the technical scheme, the invention has the beneficial effects that: oxidizing bismuth nitrate by using potassium iodide to form bismuth oxyiodide particles which have high-efficiency antibacterial catalysis effect and hollow structure, and then passivating and coating the surfaces of the bismuth oxyiodide particles by using polyacrylic acid to form bismuth oxyiodide capsule particles with hollow microcapsule structures; then dissolving and adsorbing the tungsten nitrate powder particles into bismuth oxyiodide capsule particles, so that the prepared functional powder has the effects of keeping warm and far infrared emission and absorption; meanwhile, bismuth oxyiodide capsule particles with a hollow microcapsule structure are dispersed in a polyester matrix, and the bismuth oxyiodide capsule particles are not subjected to high shearing action in the polymerization process, so that the bismuth oxyiodide capsule particles can be uniformly dispersed in the polymerization matrix to form functional polyester chips; finally, bismuth oxyiodide capsule particles with hollow microcapsule structures are sheared at high pressure and high speed through spinneret orifices in a high-pressure melt spinning process to destroy the hollow structures, so that the antibacterial bismuth oxyiodide capsule particles are dispersed on fibers, and the spherical bismuth oxyiodide capsule particles with hollow structures are influenced by shearing action in a drafting shearing process and are favorably and quickly dispersed on the surfaces of functional fibers, so that the functional fibers are endowed with excellent antibacterial performance due to low addition, and the fiber with the functions of keeping warm and inhibiting bacteria is prepared; obviously, the bismuth oxyiodide capsule particles with efficient antibacterial catalysis effect and hollow structure are uniformly dispersed in the warm-keeping bacteriostatic functional fiber, so that the preparation efficiency of the warm-keeping bacteriostatic functional fiber is improved, the warm-keeping bacteriostatic performance of the functional fiber is improved, the defects of low preparation efficiency and insufficient performance of the functional fiber in the prior art are overcome, and the aim of efficiently preparing the warm-keeping bacteriostatic functional fiber is fulfilled.
Drawings
FIG. 1 is an XRD spectrum of a functional powder prepared by the present invention;
FIG. 2 is a scanning electron microscope image of the functional powder prepared by the present invention;
FIG. 3 is a sectional electron microscope atlas of the warm-keeping bacteriostatic functional fiber prepared by the invention.
Detailed Description
The following examples are intended to illustrate the invention in further detail, but are not intended to limit the invention in any way, and unless otherwise indicated, the reagents, methods and apparatus used in the invention are conventional in the art, and are not intended to limit the invention in any way.
The invention discloses a preparation method of a fiber with warm-keeping and bacteriostatic functions, which comprises the following steps:
s1, preparing functional powder: s11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use; s12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution; s13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified; s14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for several hours; s15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for a plurality of hours, filtering, and washing with deionized water for a plurality of times to obtain filter residue; s16, calcining the filter residue in an aerobic environment at 450-750 ℃ for several hours, and then calcining in an aerobic environment at 800-1000 ℃ to prepare the functional powder. In the step S11, the mass fraction of the bismuth nitrate in the bismuth nitrate solution is 5-15%; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 5-15%; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 5 to 15%. In the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1:0.25 to 1: 0.50. In the step S15, the addition amount of the tungsten nitrate powder is 5 to 10% by mass of the functional powder precursor solution. In the invention, the steps are mainly that firstly, bismuth nitrate reacts with potassium iodide to generate bismuth oxyiodide, then tungsten ions are introduced to the bismuth oxyiodide, and the bismuth oxyiodide antibacterial agent is loaded with tungsten oxide powder through calcination in an aerobic environment, so that the functional powder has an antibacterial effect and a far infrared emission function. In the reaction process, polyacrylic acid is mainly dispersed into small balls through emulsification, an ammonium polyacrylate salt solution is formed on the surface of polyacrylic acid through the pH regulation of ammonia water, bismuth ions in bismuth nitrate in an alkaline environment are complexed with amino groups, then potassium iodide and the bismuth ions react to generate bismuth oxyiodide microspheres, tungsten hydroxide precipitate is loaded on the surfaces of the bismuth oxyiodide microspheres through complexation and precipitation, after the reaction is finished, the polyacrylic acid in a core layer can be removed through high-temperature calcination, and meanwhile, the loading of tungsten oxide with a far infrared emission function on the bismuth oxyiodide microspheres is realized through the regulation of a calcination process, so that the problems that conventional loaded microsphere particles are too large, the stability of tungsten oxide in the powder is poor, and the particle size of functional powder is large and the dispersibility is poor are solved. The aerobic environment set in step S16 is mainly for complete decomposition of polyacrylic acid, so as to avoid the residue of polyacrylic acid from affecting the color of the functional powder, and the distributed pyrolysis is mainly decomposition of polyacrylic acid at low temperature, and is mainly beneficial to formation of tungsten oxide at high temperature. In addition, the specific ratio of each product in step S1 is mainly to regulate the ratio of the core layer and the shell layer, the core layer contains polyacrylic acid with too much content and has too large particle size, which results in a thinner subsequent wall layer, which is easy to break the wall during calcination and difficult to form spherical complete functional powder, the core layer is too little and has thicker wall layer, which results in a particle size process of the wall layer, in the subsequent processing, the crushing pressure of the wall layer is increased, which results in difficulty in crushing and uniform dispersion in the melt spinning process, and the content of tungsten oxide powder is too low, which has poor far infrared effect, which results in too much bluing color and increased particle size of the powder.
S2, preparing functional polyester chips: putting functional powder, terephthalic acid and ethylene glycol into a container, adding a catalyst, an ether inhibitor and an antioxidant into the container, pulping to prepare pulping liquid, then carrying out pressurized esterification reaction on the pulping liquid to prepare esterified pulp, carrying out pre-polycondensation reaction and final polycondensation reaction on the esterified pulp, and carrying out melt granulation to prepare functional polyester chips; in the step S2, the molar ratio of the terephthalic acid to the ethylene glycol is 1: 1.05-1.25; the mass ratio of the functional powder to the glycol is 1: 50-200; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the antioxidant was 0.05% by mass relative to terephthalic acid. In the step S2, the catalyst is ethylene glycol antimony, the ether inhibitor is sodium acetate, and the antioxidant is triphenyl phosphate. In the step S2, in the pressure esterification process, the pressure is 0.35-0.45 MPa, the esterification temperature is 230-245 ℃, and the esterification time is 2.5-3.0 h; the pre-polycondensation reaction is normal-pressure polycondensation, the pre-polycondensation temperature is 250-260 ℃, and the pre-polycondensation time is 0.5-1.5 h. In the step S2, the final polycondensation reaction is vacuum polycondensation, and low vacuum polycondensation is performed first, and then high vacuum polycondensation is performed; the vacuum degree of the low vacuum polycondensation is 500-5000 Pa, the low vacuum polycondensation time is 0.5-1.0 h, the vacuum degree of the high vacuum polycondensation is 50-100 Pa, and the high vacuum polycondensation time is 1.0-3.0 h. In step S2, the functional powder is mainly prepared by a conventional polyester polymerization process, and the main purpose is to fully disperse and uniformly distribute the functional powder on the functional polyester chips.
S3, preparing the fiber with the functions of heat preservation and bacteriostasis: and (3) performing high-pressure melting extrusion on the functional polyester chips, cooling by circular air blowing, bundling and oiling, drafting and heat setting, and winding to prepare the thermal-insulation antibacterial functional fiber.
The invention also discloses an application of the warm-keeping bacteriostatic functional fiber, and the prepared warm-keeping bacteriostatic functional fiber is applied to cloth.
The prepared heat-insulating bacteriostatic functional fiber has the bacteriostatic rate of 95-99% on staphylococcus aureus and the bacteriostatic rate of 95-98% on escherichia coli; the far infrared emissivity at the wavelength of 1.0-5.0 microns is 20-50%, the heat insulation performance of a fabric sample prepared by the heat-insulation and bacteriostatic functional fiber is subjected to heat radiation for 1min at the temperature of 100 ℃ (15cm), the surface temperature difference of the fabric sample before and after heating is 1.0-2.0 ℃, and the surface temperature of the fabric is higher than 100 ℃.
bismuth oxyiodide has excellent antibacterial and catalytic effects, is widely applied to preparation of antibacterial powder, and has large antibacterial activity, so that the bismuth oxyiodide is difficult to be added and dispersed in situ in a polymer, and is difficult to be applied to a polyester matrix; in the technical scheme disclosed by the invention, the antibacterial property of bismuth oxyiodide is utilized, the surface of the bismuth oxyiodide is passivated and coated by polyacrylic acid, in the process of coating bismuth oxyiodide, a hollow microcapsule structure is prepared, which can not only meet the requirement of dispersing bismuth oxyiodide in a polyester matrix, and the spherical antibacterial nano particles are not subjected to high shearing action in the polymerization process, so that the spherical antibacterial nano particles can be uniformly dispersed in a polymerization matrix, and the hollow structure can be destroyed by utilizing the high-pressure high-speed shearing of a spinneret orifice in the melt spinning process of the bismuth oxide with the hollow structure, thereby realizing the dispersion of the antibacterial bismuth oxyiodide on the fiber, and during the drafting and shearing process of the spherical hollow bismuth oxyiodide, the fiber surface is beneficial to fast dispersion under the influence of shearing action, so that the fiber is endowed with excellent antibacterial performance at low addition. Meanwhile, in the aspect of preparing functional powder, the excellent far infrared absorption and reflection effects are given to the powder by utilizing the far infrared emission function containing the tungsten nitrate structure, so that the functional powder has the warm-keeping effect and the far infrared emission and absorption effects, and the excellent warm-keeping function of the fiber is ensured on the fiber fabric through the design of the fiber hollow structure.
It is apparent that, more specifically, as shown in fig. 1 to 3, the present invention oxidizes bismuth nitrate with potassium iodide to form bismuth oxyiodide particles having a highly efficient antibacterial catalytic effect and a hollow structure, and then passivates and coats the surfaces of the bismuth oxyiodide particles with polyacrylic acid to form bismuth oxyiodide capsule particles having a hollow microcapsule structure; then dissolving and adsorbing the tungsten nitrate powder particles into bismuth oxyiodide capsule particles, so that the prepared functional powder has the effects of keeping warm and far infrared emission and absorption; meanwhile, bismuth oxyiodide capsule particles with a hollow microcapsule structure are dispersed in a polyester matrix, and the bismuth oxyiodide capsule particles are not subjected to high shearing action in the polymerization process, so that the bismuth oxyiodide capsule particles can be uniformly dispersed in the polymerization matrix to form functional polyester chips; finally, bismuth oxyiodide capsule particles with hollow microcapsule structures are sheared at high pressure and high speed through spinneret orifices in a high-pressure melt spinning process to destroy the hollow structures, so that the antibacterial bismuth oxyiodide capsule particles are dispersed on fibers, and the spherical bismuth oxyiodide capsule particles with hollow structures are influenced by shearing action in a drafting shearing process and are favorably and quickly dispersed on the surfaces of functional fibers, so that the functional fibers are endowed with excellent antibacterial performance due to low addition, and the fiber with the functions of keeping warm and inhibiting bacteria is prepared; obviously, the bismuth oxyiodide capsule particles with efficient antibacterial catalysis effect and hollow structure are uniformly dispersed in the warm-keeping bacteriostatic functional fiber, so that the preparation efficiency of the warm-keeping bacteriostatic functional fiber is improved, the warm-keeping bacteriostatic performance of the functional fiber is improved, and the aim of efficiently preparing the warm-keeping bacteriostatic functional fiber is fulfilled.
The following are specific examples:
Example 1
The embodiment of the invention discloses a preparation method of a warm-keeping bacteriostatic functional fiber, which comprises the following steps:
S1, preparation of functional powder: firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use. Then, the polyacrylic acid resin is dispersed in the ethylene glycol solution, and the polyacrylic acid resin is dissolved in the ethylene glycol solution by stirring with ammonia water to prepare a polyacrylic acid mixed solution. Then adding potassium iodide into a polyacrylic acid mixed solution, dissolving, obtaining a functional powder precursor solution after the solution is clarified, dropwise adding a bismuth nitrate glycol solution into the functional powder precursor solution under ultrasonic and rapid stirring, carrying out ultrasonic stirring reaction for 4 hours, then adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for 4 hours, then filtering, washing filter residues with deionized water for 3 times, calcining the filter residues in an aerobic environment at 650 ℃ for 2 hours, and then calcining at 900 ℃ for 15 minutes to obtain the functional powder. The mass fraction of bismuth nitrate in the diethylene alcohol solution of bismuth nitrate is 15 percent; the mass fraction of the polyacrylic acid mixed solution is 15%; the mass fraction of potassium iodide in the functional powder precursor solution is 15%; the volume ratio of the functional powder precursor to the ethylene glycol solution of bismuth nitrate is 1: 0.50; the addition amount of the tungsten nitrate is 10 percent of the mass fraction of the functional powder precursor. The specific internal structure of the functional powder is shown in fig. 1-2.
S2, preparation of functional polyester chips: adopting an in-situ copolymerization method, firstly pulping the functional powder obtained in the step S1, terephthalic acid and ethylene glycol, simultaneously adding a catalyst of ethylene glycol antimony, an ether inhibitor of sodium acetate and an antioxidant of triphenyl phosphate, pulping for 15min at the temperature of 80 ℃ to prepare a pulping liquid, then carrying out pressurized esterification reaction on the pulping liquid to prepare an esterification slurry, then carrying out pre-polycondensation reaction and final polycondensation reaction, and carrying out melt granulation to prepare the functional polyester chip. The molar ratio of the terephthalic acid to the ethylene glycol is 1: 1.25; the mass ratio of the functional powder to the glycol is 1: 50; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; in the pressure esterification process, the pressure is 0.35-0.45 MPa, the esterification temperature is 230-245 ℃, and the esterification time is 3.0 h; the pre-polycondensation reaction is normal-pressure polycondensation, the pre-polycondensation temperature is 250-260 ℃, and the pre-polycondensation time is 1.5 h; the final polycondensation reaction is vacuum polycondensation, and low vacuum polycondensation is firstly carried out, and then high vacuum polycondensation is carried out; the low vacuum degree of vacuum polycondensation is 500-5000 Pa, the low vacuum time of polycondensation is 1.0h, the high vacuum degree of vacuum polycondensation is 50-100 Pa, and the high vacuum time of polycondensation is 3.0 h.
s3, preparing the heat-preservation and bacteriostatic functional fiber: and (4) taking the functional polyester chip prepared in the step S2 as a raw material, carrying out melt spinning by using a special-shaped spinneret plate, carrying out high-pressure extrusion on a melt, cooling by circular blowing, bundling and oiling, drafting and heat setting, and winding to prepare the thermal-insulation antibacterial functional fiber. The special-shaped spinneret plate is formed by 3 'C' shapes, the radian of the C-shaped angle of the spinneret plate is 105 degrees, and the radian between adjacent C-shaped angles is 15 degrees. The melt spinning process is the same as the conventional melt spinning process. The specific structure of the interior of the warm-keeping bacteriostatic functional fiber is shown in figure 3
The embodiment of the invention also discloses application of the warm-keeping bacteriostatic functional fiber, and the prepared warm-keeping bacteriostatic functional fiber is applied to cloth.
Example 2
The embodiment of the invention discloses a preparation method of a warm-keeping bacteriostatic functional fiber, which comprises the following steps:
S1, preparation of functional powder: firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use. Then, the polyacrylic acid resin is dispersed in the ethylene glycol solution, and the polyacrylic acid resin is dissolved in the ethylene glycol solution by stirring with ammonia water to prepare a polyacrylic acid mixed solution. Then adding potassium iodide into a polyacrylic acid mixed solution, dissolving, obtaining a functional powder precursor solution after the solution is clarified, dropwise adding a bismuth nitrate glycol solution into the functional powder precursor solution under ultrasonic and rapid stirring, carrying out ultrasonic stirring reaction for 4 hours, then adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for 4 hours, then filtering, washing filter residues with deionized water for 3 times, calcining the filter residues in an aerobic environment at 650 ℃ for 2 hours, and then calcining at 900 ℃ for 15 minutes to obtain the functional powder. The mass fraction of bismuth nitrate in the diethylene alcohol solution of bismuth nitrate is 5 percent; the mass fraction of the polyacrylic acid mixed solution is 5%; the mass fraction of potassium iodide in the functional powder precursor solution is 5%; the volume ratio of the functional powder precursor to the ethylene glycol solution of bismuth nitrate is 1: 0.25; the addition amount of the tungsten nitrate is 5% of the mass fraction of the functional powder precursor.
S2, preparation of functional polyester chips: adopting an in-situ copolymerization method, firstly pulping the functional powder obtained in the step S1, terephthalic acid and ethylene glycol, simultaneously adding a catalyst of ethylene glycol antimony, an ether inhibitor of sodium acetate and an antioxidant of triphenyl phosphate, pulping for 15min at the temperature of 80 ℃ to prepare a pulping liquid, then carrying out pressurized esterification reaction on the pulping liquid to prepare an esterification slurry, then carrying out pre-polycondensation reaction and final polycondensation reaction, and carrying out melt granulation to prepare the functional polyester chip. The molar ratio of the terephthalic acid to the ethylene glycol is 1: 1.05; the mass ratio of the functional powder to the glycol is 1: 50; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; in the pressure esterification process, the pressure is 0.35-0.45 MPa, the esterification temperature is 230-245 ℃, and the esterification time is 3.0 h; the pre-polycondensation reaction is normal-pressure polycondensation, the pre-polycondensation temperature is 250-260 ℃, and the pre-polycondensation time is 1.5 h; the final polycondensation reaction is vacuum polycondensation, and low vacuum polycondensation is firstly carried out, and then high vacuum polycondensation is carried out; the low vacuum degree of vacuum polycondensation is 500-5000 Pa, the low vacuum time of polycondensation is 1.0h, the high vacuum degree of vacuum polycondensation is 50-100 Pa, and the high vacuum time of polycondensation is 3.0 h.
s3, preparing the heat-preservation and bacteriostatic functional fiber: and (4) taking the functional polyester chip prepared in the step S2 as a raw material, carrying out melt spinning by using a special-shaped spinneret plate, carrying out high-pressure extrusion on a melt, cooling by circular blowing, bundling and oiling, drafting and heat setting, and winding to prepare the thermal-insulation antibacterial functional fiber. The special-shaped spinneret plate is formed by 3 'C' shapes, the radian of the C-shaped angle of the spinneret plate is 105 degrees, and the radian between adjacent C-shaped angles is 15 degrees. The melt spinning process is the same as the conventional melt spinning process. The specific structure of the interior of the warm-keeping bacteriostatic functional fiber is shown in figure 3
The embodiment of the invention also discloses application of the warm-keeping bacteriostatic functional fiber, and the prepared warm-keeping bacteriostatic functional fiber is applied to cloth.
Example 3
The embodiment of the invention discloses a preparation method of a warm-keeping bacteriostatic functional fiber, which comprises the following steps:
s1, preparation of functional powder: firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use. Then, the polyacrylic acid resin is dispersed in the ethylene glycol solution, and the polyacrylic acid resin is dissolved in the ethylene glycol solution by stirring with ammonia water to prepare a polyacrylic acid mixed solution. Then adding potassium iodide into a polyacrylic acid mixed solution, dissolving, obtaining a functional powder precursor solution after the solution is clarified, dropwise adding a bismuth nitrate glycol solution into the functional powder precursor solution under ultrasonic and rapid stirring, carrying out ultrasonic stirring reaction for 4 hours, then adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for 4 hours, then filtering, washing filter residues with deionized water for 3 times, calcining the filter residues in an aerobic environment at 650 ℃ for 2 hours, and then calcining at 900 ℃ for 15 minutes to obtain the functional powder. The mass fraction of bismuth nitrate in the diethylene alcohol solution of bismuth nitrate is 12%; the mass fraction of the polyacrylic acid mixed solution is 15%; the mass fraction of potassium iodide in the functional powder precursor solution is 12%; the volume ratio of the functional powder precursor to the ethylene glycol solution of bismuth nitrate is 1: 0.35; the addition amount of the tungsten nitrate is 8 percent of the mass fraction of the functional powder precursor.
S2, preparation of functional polyester chips: adopting an in-situ copolymerization method, firstly pulping the functional powder obtained in the step S1, terephthalic acid and ethylene glycol, simultaneously adding a catalyst of ethylene glycol antimony, an ether inhibitor of sodium acetate and an antioxidant of triphenyl phosphate, pulping for 15min at the temperature of 80 ℃ to prepare a pulping liquid, then carrying out pressurized esterification reaction on the pulping liquid to prepare an esterification slurry, then carrying out pre-polycondensation reaction and final polycondensation reaction, and carrying out melt granulation to prepare the functional polyester chip. The molar ratio of the terephthalic acid to the ethylene glycol is 1: 1.15; the mass ratio of the functional powder to the glycol is 1: 120; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the mass fraction of the antioxidant relative to the terephthalic acid is 0.05 percent; in the pressure esterification process, the pressure is 0.35-0.45 MPa, the esterification temperature is 230-245 ℃, and the esterification time is 3.0 h; the pre-polycondensation reaction is normal-pressure polycondensation, the pre-polycondensation temperature is 250-260 ℃, and the pre-polycondensation time is 1.5 h; the final polycondensation reaction is vacuum polycondensation, and low vacuum polycondensation is firstly carried out, and then high vacuum polycondensation is carried out; the low vacuum degree of vacuum polycondensation is 500-5000 Pa, the low vacuum time of polycondensation is 1.0h, the high vacuum degree of vacuum polycondensation is 50-100 Pa, and the high vacuum time of polycondensation is 3.0 h.
S3, preparing the heat-preservation and bacteriostatic functional fiber: and (4) taking the functional polyester chip prepared in the step S2 as a raw material, carrying out melt spinning by using a special-shaped spinneret plate, carrying out high-pressure extrusion on a melt, cooling by circular blowing, bundling and oiling, drafting and heat setting, and winding to prepare the thermal-insulation antibacterial functional fiber. The special-shaped spinneret plate is formed by 3 'C' shapes, the radian of the C-shaped angle of the spinneret plate is 105 degrees, and the radian between adjacent C-shaped angles is 15 degrees. The melt spinning process is the same as the conventional melt spinning process. The specific structure of the interior of the warm-keeping bacteriostatic functional fiber is shown in figure 3
the embodiment of the invention also discloses application of the warm-keeping bacteriostatic functional fiber, and the prepared warm-keeping bacteriostatic functional fiber is applied to cloth.
Comparative example 1
And directly spinning the PET fiber to obtain the finished product.
Comparative example 2
Comparative example 2 is basically the same as example 1, except that the functional powder prepared by blending bismuth oxyiodide powder and tungsten oxide powder with the same mass fraction as that of example 1 is adopted;
The fiber finished products prepared in examples 1 to 3 were subjected to the following test:
And (3) antibacterial testing: the method for measuring the absorbance is adopted to carry out an antibacterial experiment, and the adopted strains are escherichia coli and staphylococcus aureus. 5mg of each of the finished fiber products prepared in examples 1 to 3 and comparative examples 1 to 2 were placed in a conical flask, 100 times of the same volume of culture solution was added, the pH of the culture solution was adjusted to 6.8 to 5.2, and autoclaving was carried out at 125 ℃. 105CFU of escherichia coli and staphylococcus aureus are respectively inoculated in each conical flask, shake culture is carried out for 0min, 60min, 120min, 240min, 480min and 520min, 10 mu L of bacterial suspension is removed by using a liquid-removing gun to measure the absorbance value, and the result is shown in table 1.
TABLE 1 antimicrobial testing
in addition, 5mg of water is respectively placed in conical flasks, 105CFU of escherichia coli and staphylococcus aureus are respectively inoculated in each conical flask, shaking culture is carried out for 0min, 60min, 120min, 240min, 480min and 520min, 10 mu L of bacterial suspension is transferred by using a liquid transfer gun, and the absorbance value is measured to serve as a negative control group. The results show that there is a significant increase in absorbance values over this time range. From the test, it is shown that the smaller the absorbance value, the smaller the number of the strain, and the better the bacteriostatic effect. Obviously, the bacteriostatic effect obtained in examples 1-3 is much greater than that of comparative examples 1-2.
And (3) testing the heat retention property: the method for measuring the surface temperature difference before and after the heating of the fiber cloth is adopted to carry out the thermal insulation performance experiment, the thermal insulation performance of the fiber cloth is obtained by comparing the surface temperature difference before and after the heating of the fiber cloth, the smaller the surface temperature difference before and after the heating of the fiber cloth is, the higher the far infrared emissivity of the fiber cloth is, and the better the thermal insulation performance is. The fiber cloth prepared in examples 1 to 3 and comparative examples 1 to 2, which had the same size, was thermally radiated at 100 ℃ (15cm) for 1min, and then the surface temperature difference before and after heating of the comparative fiber cloth was measured. The results are shown in Table 2:
TABLE 2 test of warmth retention
and (4) conclusion: as can be seen from table 2, by comparing the surface temperature difference before and after heating of the fiber cloth, the surface temperature difference before and after heating of the fiber cloth prepared in examples 1 to 3 is much smaller than the surface temperature difference before and after heating of the fiber cloth prepared in comparative example 1 to 2, which indicates that the far infrared emissivity of the fiber cloth prepared in examples 1 to 3 is much larger than that of the fiber cloth prepared in comparative example 1 to 2, and obviously, the thermal insulation performance of the fiber cloth prepared in examples 1 to 3 is much better than that of the fiber cloth prepared in comparative example 1 to 2. In summary, the prepared heat-insulation bacteriostatic functional fiber has excellent heat-insulation and antibacterial effects; because the tungsten oxide powder is loaded on the surface of the bismuth oxyiodide, the antibacterial performance of the bismuth oxyiodide powder is further improved, and because the tungsten oxide has excellent far infrared emission effect, although the two powder blending methods adopted in the comparative example 2 are added into the polyester, the polyester has a certain far infrared emission function, the powder content is the same as that of the comparative example 1, and because the bismuth oxyiodide and the tungsten oxide have the synergistic modification effect after being loaded, the far infrared emission rate of the examples 1 and 2 is far greater than that of the comparative example 2, and the antibacterial performance of the examples 1 and 2 is further improved after the bismuth oxyiodide is loaded with the tungsten oxide, the simple functional powder blending method has poor dispersion uniformity and poor antibacterial effect of the powder, and therefore the antibacterial performance of the powder is far less than that of the examples 1 and 2.
the technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments can be referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. a preparation method of a warm-keeping bacteriostatic functional fiber is characterized by comprising the following steps:
s1, preparing functional powder;
S2, preparing functional polyester chips: putting functional powder, terephthalic acid and ethylene glycol into a container, adding a catalyst, an ether inhibitor and an antioxidant into the container, pulping to prepare pulping liquid, then carrying out pressurized esterification reaction on the pulping liquid to prepare esterified pulp, carrying out pre-polycondensation reaction and final polycondensation reaction on the esterified pulp, and carrying out melt granulation to prepare functional polyester chips;
S3, preparing the fiber with the functions of heat preservation and bacteriostasis: and (3) performing high-pressure melting extrusion on the functional polyester chips, cooling by circular air blowing, bundling and oiling, drafting and heat setting, and winding to prepare the thermal-insulation antibacterial functional fiber.
2. The method for preparing the warm-keeping bacteriostatic functional fiber according to claim 1, wherein the specific contents of the step S1 include:
S11, firstly, dissolving bismuth nitrate powder in an ethylene glycol solution to prepare a bismuth nitrate solution for later use;
S12, dispersing polyacrylic resin in an ethylene glycol solution, and stirring with ammonia water to dissolve the polyacrylic resin in the ethylene glycol solution to prepare a polyacrylic acid mixed solution;
S13, adding potassium iodide into the polyacrylic acid mixed solution, dissolving, and obtaining a functional powder precursor solution after the solution is clarified;
S14, dropwise adding the bismuth nitrate solution prepared in the step S1 into the functional powder precursor solution under ultrasonic and rapid stirring to perform ultrasonic stirring reaction for several hours;
S15, adding tungsten nitrate powder, carrying out dissolving and adsorption reaction, continuously carrying out ultrasonic stirring reaction for a plurality of hours, filtering, and washing with deionized water for a plurality of times to obtain filter residue;
S16, calcining the filter residue in an aerobic environment at 450-750 ℃ for several hours, and then calcining in an aerobic environment at 800-1000 ℃ to prepare the functional powder.
3. The method for preparing the warm-keeping bacteriostatic functional fiber according to claim 2, characterized in that in the step S11, the mass fraction of bismuth nitrate in the bismuth nitrate solution is 5-15%; in the step S12, the mass fraction of polyacrylic acid in the polyacrylic acid mixed solution is 5-15%; in the step S13, the mass fraction of potassium iodide in the functional powder precursor solution is 5 to 15%.
4. The method for preparing the warm-keeping bacteriostatic functional fiber according to claim 2, wherein in the step S14, the volume ratio of the functional powder precursor solution to the bismuth nitrate solution is 1: 0.25-1: 0.50.
5. The method for preparing the warm-keeping bacteriostatic functional fiber according to claim 2, wherein in the step S15, the addition amount of the tungsten nitrate powder is 5-10% of the mass fraction of the functional powder precursor solution.
6. the method for preparing the warm-keeping bacteriostatic functional fiber according to claim 1, wherein in the step S2, the molar ratio of the terephthalic acid to the ethylene glycol is 1: 1.05-1.25; the mass ratio of the functional powder to the glycol is 1: 50-200; the mass fraction of the catalyst relative to the terephthalic acid is 0.05 percent; the mass fraction of the ether inhibitor relative to the terephthalic acid is 0.05 percent; the antioxidant was 0.05% by mass relative to terephthalic acid.
7. The method for preparing the heat-insulating bacteriostatic functional fiber according to claim 1, wherein in the step S2, the catalyst is ethylene glycol antimony, the ether inhibitor is sodium acetate, and the antioxidant is triphenyl phosphate.
8. The method for preparing the heat-insulating bacteriostatic functional fiber according to claim 1, wherein in the step S2, in the pressure esterification process, the pressure is 0.35-0.45 MPa, the esterification temperature is 230-245 ℃, and the esterification time is 2.5-3.0 h; the pre-polycondensation reaction is normal-pressure polycondensation, the pre-polycondensation temperature is 250-260 ℃, and the pre-polycondensation time is 0.5-1.5 h.
9. the method for preparing the heat-insulating bacteriostatic functional fiber according to the claim 8, wherein in the step S2, the final polycondensation reaction is vacuum polycondensation, and the low vacuum polycondensation is performed firstly, and then the high vacuum polycondensation is performed; the vacuum degree of the low vacuum polycondensation is 500-5000 Pa, the low vacuum polycondensation time is 0.5-1.0 h, the vacuum degree of the high vacuum polycondensation is 50-100 Pa, and the high vacuum polycondensation time is 1.0-3.0 h.
10. The application of the warm-keeping bacteriostatic functional fiber prepared according to any one of claims 1 to 9 in cloth.
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