CN110387598B - Antibacterial anti-ultraviolet multifunctional chemical fiber - Google Patents
Antibacterial anti-ultraviolet multifunctional chemical fiber Download PDFInfo
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- CN110387598B CN110387598B CN201810344876.6A CN201810344876A CN110387598B CN 110387598 B CN110387598 B CN 110387598B CN 201810344876 A CN201810344876 A CN 201810344876A CN 110387598 B CN110387598 B CN 110387598B
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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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- 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
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide 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
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses an antibacterial anti-ultraviolet multifunctional chemical fiber. Dissolving soluble metal salt and macromolecular complexing dispersant in water to prepare aqueous solution, adding the aqueous solution into a polymer monomer, reacting under the action of microwave or hydrothermal to obtain a polymer monomer containing multifunctional nano oxide, adding the polymer monomer, a polymer, a catalyst, an initiator, a stabilizer and the like into a polymerization reaction kettle, carrying out esterification, polycondensation or copolymerization to obtain a polymer melt, and carrying out spinning or casting tape granulation to obtain the antibacterial ultraviolet-proof multifunctional chemical fiber or master batch chip. The invention ensures small particle size and dispersibility of the nano metal oxide by generating the nano metal oxide in situ in the monomer before polymerization reaction, and does not influence subsequent spinning and weaving; the provided antibacterial ultraviolet-proof multifunctional chemical fiber has high-efficiency and lasting antibacterial ultraviolet-proof functions, is free of metal ion precipitation, effectively overcomes the problems of precipitation discoloration, single function and the like caused by silver ion usage in the prior art, and is safe and environment-friendly to use.
Description
Technical Field
The invention relates to an antibacterial ultraviolet-proof multifunctional chemical fiber obtained by in-situ polymerization, belonging to the technical field of special textile materials.
Background
Chemical fibers are widely used for their excellent physical and chemical properties. However, with the development of science and technology and the further improvement of the living standard of people, the development and application of functional chemical fiber textiles become a great direction for the research and development of the functional textiles in China at present. Due to the characteristics of chemical fibers, the production method of functional chemical fibers mainly adopts a blend spinning method to obtain a relatively durable functional effect. For example: the invention of Chinese patent CN104963028A provides a preparation method of an antibacterial polyester fiber, which is prepared by PET polyester chips and antibacterial polyester master batches through melt spinning, wherein the antibacterial polyester master batches are prepared by the PET polyester chips, a pretreated nano-silver antibacterial agent, an antioxidant, a lubricant and a dispersing agent through melt blending and extrusion, and the pretreated nano-silver antibacterial agent is a nano-silver antibacterial agent obtained through polyethylene wax coating treatment. Solves the problem of uniform distribution of small particle size of the nano-silver antibacterial agent in the PET matrix, and prepares the high-efficiency and long-acting antibacterial polyester fiber through melt spinning. The Chinese invention patent CN103184575A provides a production method of antibacterial chinlon, which comprises the following steps: (1) preparing an antibacterial polyamide master batch: mixing and granulating nylon-6 slices and nano-silver phosphate to obtain antibacterial nylon master batches; (2) spinning: and (2) blending the antibacterial chinlon prepared in the step (1) and the chinlon 6 slices for spinning, and performing oiling winding, balancing and stretching to obtain the antibacterial chinlon. According to the technical scheme, the nano silver phosphate is directly added into the chinlon, so that the physical property of the chinlon is reduced, and the service life of a product is influenced. For example, chinese patent CN102345179A discloses a method for preparing nano zinc oxide modified polyester fiber, in which metal oxides such as zinc oxide are directly dispersed in the polymer monomer and mixed, and chinese patent CN105962510A discloses a method for adding a nano mineral energy modifier from the polymerization end of the polymer monomer to obtain a nano mineral energy fiber. The nano material is not easy to be uniformly dispersed in the polymer monomer by the method, and the particle size of the oxide used is more than 20nm, thereby influencing the performance and causing the spinning blockage. The US patent 9527918B2 discloses a method for preparing a zinc-containing spinning solution by dissolving some zinc-containing salts into polymer monomers and then polymerizing the zinc-containing salts with other monomers, which has the disadvantages that the antibacterial property of the product still depends on the precipitation of zinc ions, so that the zinc ion precipitation is controlled to be a lower concentration as far as possible, the problem is not fundamentally solved, and the function is single.
Disclosure of Invention
Aiming at the defects of the existing multifunctional chemical fiber technology, the invention provides the antibacterial and ultraviolet-proof multifunctional chemical fiber obtained by in-situ polymerization, which has high-efficiency and lasting antibacterial and ultraviolet-proof functions, no metal ions are separated out, and the use is safe and environment-friendly.
The technical scheme for realizing the aim of the invention is to provide an antibacterial ultraviolet-proof multifunctional chemical fiber which is prepared by the following steps:
(1) the preparation method comprises the following steps of (1): dissolving 0.02-0.5 of the metal salt in water to prepare an aqueous solution with the mass concentration of the metal soluble metal salt being 5-10%; adding the aqueous solution into a polymer monomer under vigorous stirring, reacting the soluble metal salt in the polymer monomer for 30-50 min under the microwave or hydrothermal condition at the temperature of 130-180 ℃ for 30-50 min, evaporating to remove water under a vacuum state, and controlling the water content to be below 2% to obtain the polymer monomer containing the nano oxide; the soluble metal salt comprises two or more of compounds of zinc, magnesium, calcium, titanium, copper, aluminum, zirconium, barium, strontium and silicon; the macromolecular complexing dispersant comprises polyacrylamide, polyacrylic acid, polyvinylpyrrolidone, polyvinyl alcohol, polymaleic anhydride, polyquaternary ammonium salt, polyethylene glycol, polyurethane, polyamide and amino acid; the polymer monomer comprises ethanol, acetone, ethylene glycol, propylene glycol, butanediol, glycerol, propylene glycol, ethylenediamine, caprolactam and amino acid;
(2) At the beginning or middle stage of polymerization reaction, adding the polymer monomer containing the nano oxide obtained in the step (1) into a conventional polymer monomer and other raw materials required by polymerization, fully mixing, and carrying out polymerization reaction according to the polymerization process conditions of the conventional polymer monomer to prepare an antibacterial ultraviolet-proof multifunctional polymer melt;
(3) spinning the polymer melt prepared in the step (2) to obtain the antibacterial and anti-ultraviolet multifunctional chemical fiber; or the polymer melt is granulated by a casting belt to obtain the antibacterial ultraviolet-proof multifunctional master batch slice.
In the above technical scheme, the other raw materials required for the polymerization include a catalyst and a stabilizer, and may also include other auxiliaries. The dosage of the polymer monomer containing the nano oxide and the conventional polymer monomer can be adjusted according to the product effect, for example, the ratio of the conventional polymer monomer to the polymer monomer containing the nano oxide is = 1-2: 1 in terms of molar ratio.
The conventional polymer comprises PET, PBT, PTT, PA, PTA, ABS, PP, PE, PVC and PU.
The present invention uses one of the monomers for chemical fiber polymerization as medium, and directly synthesizes nanometer oxide with the size less than 5nm in situ in the medium, and the nanometer oxide is a monomer containing multifunctional nanometer oxide, and then the monomer and other conventional polymer monomers are subjected to polymerization reaction, so that the high-efficiency multifunctional chemical fiber or master batch is obtained.
The antibacterial and ultraviolet-proof multifunctional chemical fiber obtained by the invention has the advantages of simple process, high efficiency, energy conservation and environmental protection, and the product has high-efficiency and lasting antibacterial and ultraviolet-proof functions, does not have metal ions to be separated out, is safe and environment-friendly to use, and effectively solves the problems of separation and color change, single function and the like caused by commonly used silver ions at present. The nanometer metal oxide is generated in situ in the monomer before polymerization reaction, so that the small particle size and the dispersity of the nanometer metal oxide are ensured, subsequent spinning and weaving are not influenced, and meanwhile, the polymerization speed of the monomer is accelerated by the semiconductor catalysis of the nanometer metal oxide, so that one third of time is saved compared with the conventional method, and the energy is saved.
Compared with the traditional functional chemical fiber, the nano-oxide is synthesized in situ in the monomer in advance, so that the fiber has small particle size and good dispersibility, does not influence subsequent spinning and weaving, has excellent functions, does not precipitate metal ions, and is very safe and environment-friendly. Compared with the traditional chemical fiber synthesis, the method greatly shortens the polymerization time, improves the efficiency and saves the energy by utilizing the catalytic effect of the nano metal oxide.
The nano oxide is synthesized in situ in the polymer monomer, so that the particle size is small, the dispersibility is good, the subsequent spinning and weaving are not influenced, the function is excellent, no metal ion is separated out, and the preparation method is very safe and environment-friendly. Compared with the traditional chemical fiber synthesis, the method greatly shortens the polymerization time, improves the efficiency and saves the energy by utilizing the catalytic effect of the nano metal oxide.
Compared with the prior art, the invention has the outstanding advantages that:
1. one of monomers used for chemical fiber polymerization is taken as a medium, and the nano oxide with the grain diameter less than 5nm is directly synthesized in situ, does not need to be dispersed again, and has good compatibility with other polymerization monomers;
2. the catalytic effect of the nano metal oxide is utilized, so that the polymerization time is greatly shortened, the efficiency is improved, and the energy is saved;
3. the antibacterial and ultraviolet-proof multifunctional fiber provided by the invention has extremely strong and durable antibacterial and ultraviolet-proof functions, does not precipitate metal ions, and is safe and environment-friendly to use.
Drawings
Fig. 1 is a diagram of the ultraviolet protection effect of the nano antibacterial ultraviolet-proof multifunctional polyester provided in embodiment 1 of the present invention.
Fig. 2 is an antibacterial effect diagram of the nano antibacterial ultraviolet-proof multifunctional polyester fiber provided in embodiment 1 of the present invention.
Detailed Description
The technical solution of the present invention is further explained below with reference to the embodiments and the accompanying drawings.
Example 1:
titanium sulfate, zinc acetate and polyethylene glycol are mixed according to the weight ratio of 0.5: 0.5: dissolving the mixture in water in a mass ratio of 0.1 to prepare a 6% aqueous solution; gradually adding the aqueous solution into 5000 ml of ethylene glycol under vigorous stirring, placing into a microwave oven, reacting at 150 ℃ for 40min, and cooling to obtain ethylene glycol monomer with particle size below 5nm and containing nano metal oxide; evaporating the water content in the vacuum state until the content is below 2%; adding the ethylene glycol monomer containing the nano metal oxide and terephthalic acid into an esterification polymerization reaction kettle according to the molar ratio of 1.2:1, adding 0.05 percent of antimony trioxide serving as a catalyst and 0.02 percent of triethyl phosphate serving as a stabilizer according to the mass percent, and carrying out esterification reaction for 1 hour under the conditions that the kettle pressure is 2.0MPa and the temperature is 200 ℃; starting a vacuum system, heating to 270 ℃, and carrying out polycondensation reaction for 2.5 h; after the reaction is finished, the product is subjected to spinning, cooling and forming to obtain the polyester fiber with the antibacterial and ultraviolet-proof functions.
Referring to the attached drawing 1, which is a comparison graph of the ultraviolet protection effect of the functional polyester fabric and the common polyester product provided by the embodiment, it can be seen from the curve in the graph that the ultraviolet protection index of the nano antibacterial ultraviolet-proof multifunctional polyester provided by the embodiment is obviously higher than that of the common polyester.
Referring to the attached figure 2, it is a comparison graph of the antibacterial effect of the nano antibacterial ultraviolet-proof multifunctional polyester fiber provided by the embodiment of the invention and the common polyester; wherein, a picture A is common terylene, a picture B is the antibacterial anti-ultraviolet multifunctional terylene provided by the embodiment, and a picture C is the antibacterial anti-ultraviolet multifunctional terylene washed for 50 times.
Example 2:
copper acetate, zinc acetate, titanium sulfate and polyvinylpyrrolidone are mixed according to the weight ratio of 0.4: 0.3: 0.3: dissolving the mixture in water in a mass ratio of 0.2 to prepare a 7% aqueous solution; gradually adding the aqueous solution to 5000 ml of 1, 3-propanediol under vigorous stirring; placing into a microwave oven, reacting at 170 deg.C for 30min, and cooling to obtain 1, 3-propylene glycol monomer containing nanometer metal oxide with particle size below 5 nm; evaporating water in the mixture under vacuum until the content is below 2%, adding 1, 3-propanediol monomer containing nano metal oxide and dimethyl terephthalate into a reaction kettle according to the mol ratio of 1.5:1, catalyst tetrabutyl titanate of 0.05% and stabilizer triethyl phosphate of 0.03%, esterifying for 1h under the protection of nitrogen and at the pressure of 0.1MPa and the temperature of 210 ℃, then sending the mixture into a polycondensation reaction kettle, heating to 250 ℃ under high vacuum to start polycondensation for 4.5h, and spinning, cooling and slicing the product after the reaction is finished to obtain the antibacterial ultraviolet-resistant PTT chemical fiber master batch.
Example 3:
titanium sulfate, zinc nitrate, zirconium oxychloride and polyethylene glycol are mixed according to the proportion of 0.3: 0.4: 0.3: dissolving the mixture in water in a mass ratio of 0.5 to prepare a 6% aqueous solution; gradually adding the aqueous solution to 5000 ml of adipic acid under vigorous stirring; putting into a hydrothermal reaction kettle, reacting for 40min at 160 ℃, and cooling to obtain an adipic acid monomer containing nano metal oxide with the particle size of less than 5 nm; adding caprolactam monomer and a small amount of water, cobalt acetate, nylon monomer salt and other substances into a reaction kettle, and reacting for 4 hours under the atmosphere of nitrogen and at the kettle pressure of 2.0MPa and the temperature of 235 ℃; and then adding an adipic acid monomer containing nano metal oxide, continuing to react for 2 hours, adding a polyethylene glycol soft segment and a tetrabutyl titanate catalyst, heating to 247 ℃, continuing to react for 2 hours to obtain an antibacterial and ultraviolet-proof PA6 molten mass, and performing spinning, cooling and slicing on a product after the reaction is finished to obtain the antibacterial and ultraviolet-proof far-infrared PA6 nylon master batch.
Claims (1)
1. An antibacterial ultraviolet-proof multifunctional chemical fiber is characterized in that the preparation method comprises the following steps:
(1) soluble metal salt and a macromolecular complexing dispersant are mixed according to the mass ratio of 1: 0.02-0.5, dissolving in water to prepare an aqueous solution with the mass concentration of the soluble metal salt of 5-10%; adding an aqueous solution of soluble metal salt into a polymer monomer under vigorous stirring, wherein the molar concentration of the soluble metal salt in the polymer monomer is 0.01-0.5M, reacting for 30-50 min under a microwave or hydrothermal condition at the temperature of 130-180 ℃, evaporating to remove water under a vacuum state, and controlling the water content to be below 2% to obtain a polymer monomer containing nano oxide; the soluble metal salt is one or more of compounds of zinc and titanium and compounds of magnesium, calcium, copper, aluminum, zirconium, barium, strontium and silicon; the macromolecular complexing dispersant is one or more of polyacrylamide, polyacrylic acid, polyvinylpyrrolidone, polyvinyl alcohol, polymaleic anhydride, polyquaternium, polyethylene glycol, polyurethane and polyamide; the polymer monomer is one or more of ethylene glycol, propylene glycol, butanediol, ethylenediamine, caprolactam and amino acid;
(2) At the beginning or middle stage of polymerization reaction, adding the polymer monomer containing the nano oxide obtained in the step (1) into a monomer required by the polymer and other raw materials required by polymerization, fully mixing, and carrying out polymerization reaction according to the polymerization process conditions of the polymer to prepare an antibacterial ultraviolet-proof multifunctional polymer melt; the polymer is selected from PET, PBT, PTT or PA;
(3) and (3) spinning the polymer melt prepared in the step (2) to obtain the antibacterial ultraviolet-proof multifunctional chemical fiber.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810344876.6A CN110387598B (en) | 2018-04-17 | 2018-04-17 | Antibacterial anti-ultraviolet multifunctional chemical fiber |
| US16/647,398 US11319647B2 (en) | 2018-01-29 | 2018-06-27 | Anti-bacterial and anti-ultraviolet multifunctional chemical fiber |
| EP18902844.2A EP3748048A4 (en) | 2018-01-29 | 2018-06-27 | Antibacterial anti-ultraviolet multifunctional chemical fiber |
| JP2020562805A JP7197607B2 (en) | 2018-01-29 | 2018-06-27 | Antibacterial/ultraviolet shielding multifunctional chemical fiber |
| PCT/CN2018/093197 WO2019144567A1 (en) | 2018-01-29 | 2018-06-27 | Antibacterial anti-ultraviolet multifunctional chemical fiber |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810344876.6A CN110387598B (en) | 2018-04-17 | 2018-04-17 | Antibacterial anti-ultraviolet multifunctional chemical fiber |
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| CN110387598A CN110387598A (en) | 2019-10-29 |
| CN110387598B true CN110387598B (en) | 2022-06-14 |
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| CN112695408B (en) * | 2020-12-31 | 2023-01-24 | 江苏纳盾科技有限公司 | Efficient quick-acting non-dissolution antibacterial composite fiber and preparation method thereof |
| CN113150267B (en) * | 2021-04-21 | 2023-01-13 | 中鼎凯瑞科技成都有限公司 | Amino acid-based polymer with antiviral and antibacterial functions and preparation method thereof |
| CN113831517A (en) * | 2021-09-09 | 2021-12-24 | 万凯新材料股份有限公司 | Preparation method of antibacterial and uvioresistant polyester |
| CN115232302B (en) * | 2022-08-30 | 2024-01-05 | 杭州聚合顺新材料股份有限公司 | Method for simply, conveniently and rapidly preparing nylon 66 nanocomposite |
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| CN101134815A (en) * | 2007-10-17 | 2008-03-05 | 东华大学 | Method for preparing ultraviolet-resistant polyphenylene sulfide resin by in situ Polymerization |
| CN101550657B (en) * | 2009-05-14 | 2011-12-14 | 苏州大学 | Method for preparing functional textile of nano materials |
| CN102020762B (en) * | 2010-10-20 | 2012-07-25 | 东华大学 | Novel silver-containing PET (polyethylene terephthalate)-based composite and in-situ assembly preparation method and application thereof |
| CN101993527B (en) * | 2010-10-20 | 2012-11-07 | 东华大学 | Preparation method and application of silver-containing PET based composite resin material |
| EP2660268B1 (en) * | 2010-12-28 | 2019-08-07 | Shanghai Genius Advanced Material (Group) Co. Ltd | Nano particle/polyamide composite material, preparation method therefor, and use thereof |
| CN103599779B (en) * | 2013-11-13 | 2015-12-02 | 福州大学 | A kind of CuO/ZrO 2water gas converting catalyst and preparation method thereof |
| CN104963028B (en) * | 2015-07-01 | 2017-04-26 | 义乌市惠航化纤科技有限公司 | Antibacterial polyester fibers and preparation method for same |
| CN107459685B (en) * | 2017-09-11 | 2020-11-27 | 苏州美纳福健康科技有限公司 | Latex with precipitation-free sterilization function, preparation method and application |
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