CN113802207B - Nanometer antibacterial composite fiber for processing non-woven fabric and preparation method thereof - Google Patents
Nanometer antibacterial composite fiber for processing non-woven fabric and preparation method thereof Download PDFInfo
- Publication number
- CN113802207B CN113802207B CN202111121599.0A CN202111121599A CN113802207B CN 113802207 B CN113802207 B CN 113802207B CN 202111121599 A CN202111121599 A CN 202111121599A CN 113802207 B CN113802207 B CN 113802207B
- Authority
- CN
- China
- Prior art keywords
- nano
- composite fiber
- acid solution
- woven fabric
- antibacterial composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 71
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 65
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- 238000012545 processing Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 57
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 35
- 229920001661 Chitosan Polymers 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 27
- 239000011858 nanopowder Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 22
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 16
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000967 suction filtration Methods 0.000 claims abstract description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 10
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000009987 spinning Methods 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 18
- 238000007711 solidification Methods 0.000 description 18
- 230000008023 solidification Effects 0.000 description 18
- 238000000034 method Methods 0.000 description 13
- 238000000465 moulding Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 239000004744 fabric Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 229920002101 Chitin Polymers 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 244000005700 microbiome Species 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 2
- 241000238557 Decapoda Species 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000000644 propagated effect Effects 0.000 description 2
- 230000028327 secretion Effects 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229920002498 Beta-glucan Polymers 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000382353 Pupa Species 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/52—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated carboxylic acids or unsaturated esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of nano antibacterial composite fiber for processing non-woven fabrics, which comprises the following steps: adding nano titanium dioxide into water, performing ultrasonic dispersion for 5-10min, regulating the pH value of the system to 2.5-4, adding maleic anhydride, stirring at 60-80 ℃ for 2-5h under the protection of nitrogen, performing suction filtration, washing, drying at 40-50 ℃, and crushing to obtain grafted nano powder; adding chitosan into acetic acid solution, stirring uniformly, adding acrylic acid and grafted nano powder into the mixture under the protection of nitrogen, stirring uniformly, adding an initiator, and reacting at 40-60 ℃ for 5-10h to obtain a blending solution; extruding the blending solution from a spinning hole with the aperture of 0.65-0.75mm through a variable frequency stepper at the speed of 8-10mm/min, solidifying and forming in oxalic acid solution, and then sequentially washing, drafting and drying at room temperature to constant weight to obtain the nano antibacterial composite fiber for processing the non-woven fabric.
Description
Technical Field
The invention relates to the technical field of non-woven fabrics, in particular to a nano antibacterial composite fiber for processing non-woven fabrics and a preparation method thereof.
Background
Chitosan is a deacetylated product of chitin and is the most basic and important derivative of chitin. Chitin, also known as chitin, is chemically named (1, 4) -2-acetamide-2-deoxy-beta-D-glucan, and is mainly found in animal shells such as shrimps, crabs, pupas and insects, and cell walls of fungi and algae plants. The chitosan has the advantages of no toxicity, biodegradability, good biocompatibility and the like, so that the chitosan has wide research and application prospects in the fields of textiles, biological materials, drug carriers, medical use, environmental protection, health care products and the like, and is particularly widely applied to non-woven fabrics.
The non-woven fabric closely contacted with human body can be polluted with microorganisms inevitably in the use process, and the non-woven fabric can be a place for microorganism propagation, but the antimicrobial property of the chitosan non-woven fabric is general, so that the microbial balance on the skin surface of the human body can be destroyed, so that the microorganisms can be propagated on a large amount on the skin surface, bacteria on the textile are propagated by taking skin surface dander and textile fibers as nutrients, and various low-grade fatty acids, ammonia and other volatile matters with irritant odor are metabolized simultaneously, and the secretion of the microorganisms and the secretion of the human body are added, so that the textile is malodorous and the sanitation is affected.
Although the antibacterial finishing agent and the non-woven fabric fibers on the market can be mixed to ensure that the fabric has an antibacterial effect, the conventional antibacterial non-woven fabric is easy to dissolve out from the surface of the fabric, so that the antibacterial effect of the fabric is gradually deteriorated, particularly, the antibacterial effect of the fiber fabrics is quickly declined or failed along with the increase of the washing times, and meanwhile, the surface of the non-woven fabric fibers can form a groove structure along with the precipitation of the antibacterial finishing agent, so that the fibers are easy to break in the stress process. At present, the main reason for restricting the development of chitosan antibacterial fibers is that the mechanical strength of the chitosan fibers is not high, the breaking strength of the chitosan fibers obtained by conventional spinning is only 1.4-2.0cN/dtex, and the breaking strength of the chitosan fibers is seriously reduced by adding the precipitation of an antibacterial finishing agent.
Therefore, it is needed to provide a preparation method of the antibacterial chitosan fiber, which has the advantages of simple process, low production cost, low energy consumption, improvement of the mechanical properties of the fiber, and excellent antibacterial effect.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a nano antibacterial composite fiber for processing non-woven fabrics and a preparation method thereof.
A preparation method of nano antibacterial composite fiber for processing non-woven fabrics comprises the following steps:
s1, adding nano titanium dioxide into water, performing ultrasonic dispersion for 5-10min, adjusting the pH value of a system to 2.5-4, adding maleic anhydride, stirring at 60-80 ℃ for 2-5h under the protection of nitrogen, performing suction filtration, washing, drying at 40-50 ℃, and crushing to obtain grafted nano powder;
S2, adding chitosan into an acetic acid solution, uniformly stirring, adding acrylic acid and grafted nano powder into the acetic acid solution under the protection of nitrogen, uniformly stirring, adding an initiator, and reacting at 40-60 ℃ for 5-10h to obtain a blending solution;
s3, extruding the blending solution from a spinneret orifice with the aperture of 0.65-0.75mm through a variable frequency stepper at the speed of 8-10mm/min, solidifying and forming in oxalic acid solution, and then sequentially washing, drafting and drying at room temperature to constant weight to obtain the nano antibacterial composite fiber for processing the non-woven fabric.
Preferably, in S1, the mass ratio of the nano titanium dioxide to the maleic anhydride is 2-6:1-3.
Preferably, in S1, concentrated sulfuric acid is used for regulating the pH value of the system to be 2.5-4.
Preferably, in S1, the filter is washed 1-4 times with methanol.
Preferably, in S2, the mass ratio of the chitosan, the acrylic acid, the grafted nano powder and the initiator is 5-15:1-4:3-6:0.1-1.
Preferably, in S2, the initiator is hydrogen peroxide or persulfate.
Preferably, in S2, the initiator is at least one of ammonium persulfate, potassium persulfate, sodium persulfate, and hydrogen peroxide.
Preferably, in S2, the concentration of the acetic acid solution is 0.5-1.2mol/L.
Preferably, in S3, the mass fraction of the oxalic acid solution is 2.5-3.5%.
The nano antibacterial composite fiber for processing the non-woven fabric is prepared by adopting the preparation method of the nano antibacterial composite fiber for processing the non-woven fabric.
The technical effects of the invention are as follows:
(1) According to the invention, chitosan is dissolved in acetic acid solution, then acrylic acid is added, and the temperature-rising polymerization is carried out under the protection of nitrogen, so that the chitosan and the acrylic acid are polymerized by free radicals, and the obtained macromolecular polymer forms an interpenetrating structure, so that the dimensional stability and mechanical property of the polymer can be effectively enhanced;
(2) The nano titanium dioxide is dispersed in water, reacts with maleic anhydride under an acidic condition, the maleic anhydride is grafted on the surface of the nano titanium dioxide, the grafted nano powder is added into a polymer, a double-network structure is taken as a core in an interpenetrating process, the grafted nano powder is fixed in the double-network structure through a surface hydrogen bond, a crosslinking point is formed in the double-network structure, interpenetrating macromolecules are forced to mutually hold, the hybridization degree is improved, double bonds on the grafted nano powder are initiated to polymerize in the double-network structure, energy loss can be realized when the interpenetrating nano powder is stressed, the dimensional stability is enhanced, meanwhile, nano antibacterial particles are combined in the interpenetrating network structure, the immobilization effect is extremely good, the interpenetrating nano titanium dioxide is not easy to slide off, and the antibacterial effect is long;
(3) According to the invention, maleic anhydride is grafted on nano titanium dioxide, and then the nano titanium dioxide is fixed in a double-network structure, the formed blending solution is solidified through oxalic acid solution, and the nano titanium dioxide can be tightly and firmly filled in the fiber, so that the separation and dissolution of the nano titanium dioxide from the fiber structure are effectively reduced, and the antibacterial effect and the antibacterial service life of the fiber fabric in use are effectively enhanced; meanwhile, the nano titanium dioxide has poor dispersibility, and can be more uniformly distributed in the fiber by grafting with maleic anhydride, so that the antibacterial effect of the antibacterial fiber fabric is further improved.
(4) According to the invention, even though the nano antibacterial particles are washed for a plurality of times, the nano antibacterial particles are not easy to separate out, and are combined in a network structure, so that the mechanical strength of the fiber can be effectively enhanced, the fiber is not easy to break in the stress process, and the use effect and the service life of the antibacterial fiber fabric are effectively enhanced.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
Example 1
A preparation method of nano antibacterial composite fiber for processing non-woven fabrics comprises the following steps:
S1, adding 2kg of nano titanium dioxide into 40kg of water, performing ultrasonic dispersion for 5min, adopting concentrated sulfuric acid to adjust the pH value of a system to 2.5-4, adding 3kg of maleic anhydride, stirring for 5h at 60 ℃ under the protection of nitrogen, performing suction filtration, adopting methanol for washing for 1 time, drying in a 50 ℃ oven, and crushing to obtain grafted nano powder;
s2, adding 5kg of chitosan into 70kg of acetic acid solution with the concentration of 0.5mol/L, uniformly stirring, adding 4kg of acrylic acid and 3kg of grafted nano powder into the mixture, uniformly stirring, adding 1kg of hydrogen peroxide, and reacting at 40 ℃ for 10 hours to obtain a blending solution;
S3, extruding the blending solution from a spinneret orifice with the aperture of 0.75mm through a variable frequency stepper at the speed of 8mm/min, performing solidification molding in an oxalic acid solution with the mass fraction of 2.5%, and sequentially performing water washing, drafting and room temperature drying to constant weight after 8min of solidification to obtain the nano antibacterial composite fiber for processing the non-woven fabric.
Example 2
A preparation method of nano antibacterial composite fiber for processing non-woven fabrics comprises the following steps:
s1, adding 6kg of nano titanium dioxide into 20kg of water, performing ultrasonic dispersion for 10min, adopting concentrated sulfuric acid to adjust the pH value of a system to 2.5-4, adding 1kg of maleic anhydride, stirring for 2h at 80 ℃ under the protection of nitrogen, performing suction filtration, adopting methanol to wash for 4 times, drying in a baking oven at 40 ℃, and crushing to obtain grafted nano powder;
s2, adding 15kg of chitosan into 50kg of acetic acid solution with the concentration of 1.2mol/L, uniformly stirring, adding 1kg of acrylic acid and 6kg of grafted nano powder into the mixture, uniformly stirring, adding 0.1kg of ammonium persulfate, and reacting at 60 ℃ for 5 hours to obtain a blending solution;
s3, extruding the blending solution from a spinning hole with the aperture of 0.65mm through a variable frequency stepper at the speed of 10mm/min, performing solidification molding in an oxalic acid solution with the mass fraction of 3.5%, and sequentially performing water washing, drafting and room temperature drying to constant weight after solidification for 4min to obtain the nano antibacterial composite fiber for processing the non-woven fabric.
Example 3
A preparation method of nano antibacterial composite fiber for processing non-woven fabrics comprises the following steps:
s1, adding 3kg of nano titanium dioxide into 35kg of water, performing ultrasonic dispersion for 6min, adopting concentrated sulfuric acid to adjust the pH value of a system to 2.5-4, adding 2.5kg of maleic anhydride, stirring for 4h at 65 ℃ under the protection of nitrogen, performing suction filtration, adopting methanol to wash for 2 times, drying in a drying oven at 47 ℃, and crushing to obtain grafted nano powder;
S2, adding 8kg of chitosan into 65kg of acetic acid solution with the concentration of 0.8mol/L, uniformly stirring, adding 3kg of acrylic acid and 4kg of grafted nano powder into the mixture, uniformly stirring, adding 0.8kg of potassium persulfate, and reacting at 45 ℃ for 8 hours to obtain a blending solution;
S3, extruding the blending solution from a spinneret orifice with the aperture of 0.7mm at the speed of 8.5mm/min through a variable frequency stepper, performing solidification molding in oxalic acid solution with the mass fraction of 3.2%, and sequentially performing water washing, drafting and room temperature drying to constant weight after solidification for 5min to obtain the nano antibacterial composite fiber for processing the non-woven fabric.
Example 4
A preparation method of nano antibacterial composite fiber for processing non-woven fabrics comprises the following steps:
S1, adding 5kg of nano titanium dioxide into 25kg of water, performing ultrasonic dispersion for 8min, adopting concentrated sulfuric acid to adjust the pH value of a system to 2.5-4, adding 1.5kg of maleic anhydride, stirring for 3h at 75 ℃ under the protection of nitrogen, performing suction filtration, adopting methanol to wash for 3 times, drying in a baking oven at 43 ℃, and crushing to obtain grafted nano powder;
S2, adding 12kg of chitosan into 55kg of acetic acid solution with the concentration of 1mol/L, uniformly stirring, adding 2kg of acrylic acid and 5kg of grafted nano powder into the mixture under the protection of nitrogen, uniformly stirring, adding 0.2kg of sodium persulfate, and reacting at 55 ℃ for 6 hours to obtain a blending solution;
S3, extruding the blending solution from a spinneret orifice with the aperture of 0.7mm at the speed of 9.5mm/min through a variable frequency stepper, performing solidification molding in an oxalic acid solution with the mass fraction of 2.8%, and sequentially performing water washing, drafting and room temperature drying to constant weight after 7min of solidification to obtain the nano antibacterial composite fiber for processing the non-woven fabric.
Example 5
A preparation method of nano antibacterial composite fiber for processing non-woven fabrics comprises the following steps:
S1, adding 4kg of nano titanium dioxide into 30kg of water, performing ultrasonic dispersion for 7min, adopting concentrated sulfuric acid to adjust the pH value of a system to 2.5-4, adding 2kg of maleic anhydride, stirring for 3.5h at 70 ℃ under the protection of nitrogen, performing suction filtration, adopting methanol to wash for 4 times, drying in a drying oven at 45 ℃, and crushing to obtain grafted nano powder;
S2, adding 10kg of chitosan into 60kg of acetic acid solution with the concentration of 0.9mol/L, uniformly stirring, adding 2.5kg of acrylic acid and 4.5kg of grafted nano powder into the mixture under the protection of nitrogen, uniformly stirring, adding 0.5kg of ammonium persulfate, and reacting for 7 hours at 50 ℃ to obtain a blending solution;
S3, extruding the blending solution from a spinneret orifice with the aperture of 0.7mm at the speed of 9mm/min through a variable frequency stepper, performing solidification molding in an oxalic acid solution with the mass fraction of 3%, and after 6min of solidification, sequentially performing water washing, drafting and room temperature drying to constant weight to obtain the nano antibacterial composite fiber for processing the non-woven fabric.
Comparative example 1
A method for preparing antibacterial fiber, comprising the following steps:
S1, adding 10kg of chitosan into 60kg of acetic acid solution with the concentration of 0.9mol/L, uniformly stirring, and filtering and defoaming to obtain spinning solution;
S2, extruding the spinning solution from a spinning hole with the aperture of 0.7mm through a variable frequency stepper at the speed of 9mm/min, solidifying and forming in oxalic acid solution with the mass fraction of 3%, solidifying for 6min, and sequentially washing, drafting, and drying at room temperature to constant weight to obtain the antibacterial fiber.
Comparative example 2
A method for preparing antibacterial fiber, comprising the following steps:
S1, adding 10kg of chitosan into 60kg of acetic acid solution with the concentration of 0.9mol/L, uniformly stirring, adding 2.5kg of acrylic acid and 4.5kg of nano titanium dioxide into the mixture, uniformly stirring, adding 0.5kg of ammonium persulfate, and reacting at 50 ℃ for 7 hours to obtain a blending solution;
s2, extruding the blending solution from a spinneret orifice with the aperture of 0.7mm at the speed of 9mm/min through a variable frequency stepper, performing solidification molding in oxalic acid solution with the mass fraction of 3%, and performing water washing, drafting and room temperature drying to constant weight after 6min of solidification to obtain the antibacterial fiber.
Comparative example 3
A method for preparing antibacterial fiber, comprising the following steps:
S1, adding 4kg of nano titanium dioxide into 30kg of water, performing ultrasonic dispersion for 7min, adopting concentrated sulfuric acid to adjust the pH value of a system to 2.5-4, adding 2kg of maleic anhydride, stirring for 3.5h at 70 ℃ under the protection of nitrogen, performing suction filtration, adopting methanol to wash for 4 times, drying in a drying oven at 45 ℃, and crushing to obtain grafted nano powder;
s2, adding 10kg of chitosan into 60kg of acetic acid solution with the concentration of 0.9mol/L, stirring uniformly, adding 4.5kg of grafted nano powder into the solution under the protection of nitrogen, stirring uniformly, adding 0.5kg of ammonium persulfate, and reacting at 50 ℃ for 7 hours to obtain a blending solution;
s3, extruding the blending solution from a spinneret orifice with the aperture of 0.7mm at the speed of 9mm/min through a variable frequency stepper, performing solidification molding in oxalic acid solution with the mass fraction of 3%, and performing water washing, drafting and room temperature drying to constant weight after 6min of solidification to obtain the antibacterial fiber.
Comparative example 4
A method for preparing antibacterial fiber, comprising the following steps:
S1, adding 4kg of nano silver particles into 30kg of water, performing ultrasonic dispersion for 7min, adopting concentrated sulfuric acid to adjust the pH value of a system to 2.5-4, adding 2kg of maleic anhydride, stirring at 70 ℃ for 3.5h under the protection of nitrogen, performing suction filtration, adopting methanol to wash for 4 times, drying in a drying oven at 45 ℃, and crushing to obtain grafted nano powder;
S2, adding 10kg of chitosan into 60kg of acetic acid solution with the concentration of 0.9mol/L, uniformly stirring, adding 2.5kg of acrylic acid and 4.5kg of grafted nano powder into the mixture under the protection of nitrogen, uniformly stirring, adding 0.5kg of ammonium persulfate, and reacting for 7 hours at 50 ℃ to obtain a blending solution;
s3, extruding the blending solution from a spinneret orifice with the aperture of 0.7mm at the speed of 9mm/min through a variable frequency stepper, performing solidification molding in oxalic acid solution with the mass fraction of 3%, and performing water washing, drafting and room temperature drying to constant weight after 6min of solidification to obtain the antibacterial fiber.
Comparative example 5
A method for preparing antibacterial fiber, comprising the following steps:
S1, adding 10kg of chitosan into 60kg of acetic acid solution with the concentration of 0.9mol/L, stirring uniformly, adding 2.5kg of acrylic acid into the acetic acid solution under the protection of nitrogen, stirring uniformly, adding 0.5kg of ammonium persulfate, and reacting at 50 ℃ for 7 hours to obtain a blending solution;
s2, extruding the blending solution from a spinneret orifice with the aperture of 0.7mm at the speed of 9mm/min through a variable frequency stepper, performing solidification molding in oxalic acid solution with the mass fraction of 3%, and performing water washing, drafting and room temperature drying to constant weight after 6min of solidification to obtain the antibacterial fiber.
Test example 1
The nano antibacterial composite fiber for processing the non-woven fabric obtained in example 5 and the antibacterial fibers obtained in comparative examples 1 to 5 were characterized in terms of orientation degree and crystallinity, each group of orientation degree was detected by a birefringence method, and each group of crystallinity was detected by an X-ray diffraction method.
The degree of change in the orientation and crystallinity of each group was calculated using the antibacterial fiber obtained in comparative example 1 as a control, and the results were as follows:
| Orientation degree change rate% | Rate of change of crystallinity% | |
| Example 5 | 41.25 | 28.71 |
| Comparative example 2 | -4.93 | -3.14 |
| Comparative example 3 | 28.57 | 20.50 |
| Comparative example 4 | 37.62 | 24.56 |
| Comparative example 5 | 30.46 | 21.37 |
Test example 2
The nano antibacterial composite fiber for processing the non-woven fabric obtained in the example 5 and the antibacterial fibers obtained in the comparative examples 1 to 5 were subjected to mechanical property test, and specifically the following are adopted:
The fiber to be measured is measured by an LLY-06 type electronic single fiber strength tester: clamping a fiber sample to be tested on a single-fiber electronic strength tester, wherein the pre-tension is 0.3cN, the clamping length is 10mm, and stretching the fiber sample to be tested until the fiber is broken, and the stretching speed is 10mm/min; the results are shown below:
From the results of test examples 1 and 2, it can be seen that: according to the invention, through modifying the chitosan fiber, the fiber orientation degree and the crystallinity are improved, so that the difference of the connecting chain lengths between the crystal sections is small, and when the connecting chain is subjected to the action of external force, the difference of the tension applied to each connecting chain is also small, so that the external force bearable by the fiber is increased, and the mechanical property of the fiber is improved.
Test example 3
Evaluation of antimicrobial Properties of textiles according to GB/T20944.3-2008 part 3: the antibacterial ability of the nano antibacterial composite fiber for processing nonwoven fabric obtained in example 5 and the antibacterial fibers obtained in comparative examples 1 to 5 was tested in the vibration method test.
And (3) using gram-negative bacteria escherichia coli as a test strain, and testing the bacteriostasis rate after washing for 0 th, 1 st, 3 th, 5 th and 10 th times respectively. The results are as follows:
| The 0 th time | 1 St time | 3 Rd time | 5 Th time | 10 Th time | |
| Example 5 | 99.96 | 99.95 | 99.93 | 99.91 | 98.88 |
| Comparative example 1 | 73.25 | 72.51 | 72.03 | 71.26 | 70.57 |
| Comparative example 2 | 79.36 | 75.51 | 72.22 | 70.24 | 69.03 |
| Comparative example 3 | 99.87 | 99.80 | 99.71 | 99.57 | 98.33 |
| Comparative example 4 | 99.91 | 93.24 | 84.42 | 76.57 | 67.33 |
| Comparative example 5 | 76.32 | 74.47 | 73.03 | 72.51 | 71.30 |
From the above table, it can be seen that: after multiple times of washing, the nano antibacterial composite fiber for processing the non-woven fabric has little change of antibacterial performance, high stability, no damage to antibacterial property after washing, and good antibacterial effect.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (2)
1. The preparation method of the nano antibacterial composite fiber for processing the non-woven fabric is characterized by comprising the following steps of:
s1, adding nano titanium dioxide into water, performing ultrasonic dispersion for 5-10min, adjusting the pH value of a system to 2.5-4, adding maleic anhydride, stirring at 60-80 ℃ for 2-5h under the protection of nitrogen, performing suction filtration, washing, drying at 40-50 ℃, and crushing to obtain grafted nano powder;
S2, adding chitosan into an acetic acid solution, uniformly stirring, adding acrylic acid and grafted nano powder into the acetic acid solution under the protection of nitrogen, uniformly stirring, adding an initiator, and reacting at 40-60 ℃ for 5-10h to obtain a blending solution;
S3, extruding the blending solution from a spinneret orifice with the aperture of 0.65-0.75mm through a variable frequency stepper at the speed of 8-10mm/min, solidifying and forming in oxalic acid solution, and then sequentially washing, drafting and drying at room temperature to constant weight to obtain the nano antibacterial composite fiber for processing the non-woven fabric;
In S1, the mass ratio of the nano titanium dioxide to the maleic anhydride is 2-6:1-3;
In S1, the pH value of the system is regulated to be 2.5-4 by adopting concentrated sulfuric acid;
in S1, washing 1-4 times by adopting methanol after suction filtration;
In S2, the mass ratio of chitosan, acrylic acid, grafted nano powder and initiator is 5-15:1-4:3-6:0.1-1;
In S2, the initiator is hydrogen peroxide or persulfate;
In S2, the initiator is at least one of ammonium persulfate, potassium persulfate, sodium persulfate and hydrogen peroxide;
In S2, the concentration of the acetic acid solution is 0.5-1.2mol/L;
in S3, the mass fraction of the oxalic acid solution is 2.5-3.5%.
2. The nano antibacterial composite fiber for processing the non-woven fabric is characterized by being prepared by the preparation method of the nano antibacterial composite fiber for processing the non-woven fabric according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111121599.0A CN113802207B (en) | 2021-09-24 | 2021-09-24 | Nanometer antibacterial composite fiber for processing non-woven fabric and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111121599.0A CN113802207B (en) | 2021-09-24 | 2021-09-24 | Nanometer antibacterial composite fiber for processing non-woven fabric and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113802207A CN113802207A (en) | 2021-12-17 |
| CN113802207B true CN113802207B (en) | 2024-06-14 |
Family
ID=78896744
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111121599.0A Active CN113802207B (en) | 2021-09-24 | 2021-09-24 | Nanometer antibacterial composite fiber for processing non-woven fabric and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113802207B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115637522A (en) * | 2022-09-21 | 2023-01-24 | 南通东典纺织品有限公司 | Antibacterial fiber composite fabric and preparation process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206567A (en) * | 2018-07-18 | 2019-01-15 | 安徽工程大学 | A kind of preparation method of the inorganic nano-particle of surface grafting polyvinyl |
| CN113089131A (en) * | 2021-04-07 | 2021-07-09 | 大连工业大学 | Preparation method of inorganic nanoparticle dynamic cross-linking double-network modified natural polymer material |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273509C (en) * | 2003-10-29 | 2006-09-06 | 中山大学 | Method for modifying inorganic particles through grafting in situ by ball milling method |
| CN102552966B (en) * | 2012-01-31 | 2014-10-01 | 李育强 | Alginate antibacterial dressing and its preparation method |
| CN108505143A (en) * | 2018-04-10 | 2018-09-07 | 郑州智锦电子科技有限公司 | A kind of nanofiber and preparation method thereof |
-
2021
- 2021-09-24 CN CN202111121599.0A patent/CN113802207B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109206567A (en) * | 2018-07-18 | 2019-01-15 | 安徽工程大学 | A kind of preparation method of the inorganic nano-particle of surface grafting polyvinyl |
| CN113089131A (en) * | 2021-04-07 | 2021-07-09 | 大连工业大学 | Preparation method of inorganic nanoparticle dynamic cross-linking double-network modified natural polymer material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113802207A (en) | 2021-12-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20230080314A1 (en) | Deacetylation and crosslinking of chitin and chitosan in fungal materials and their composites for tunable properties | |
| CN110894642B (en) | Chitin modified PP spunbonded non-woven fabric | |
| CN113802207B (en) | Nanometer antibacterial composite fiber for processing non-woven fabric and preparation method thereof | |
| CN109369948B (en) | Bacterial cellulose/polyvinyl alcohol antibacterial hydrogel and preparation method and application thereof | |
| WO1998012369A1 (en) | Chitosan-containing acrylic fibers and process for preparing the same | |
| CN1940153A (en) | Chitose graft alginate fibre, its production and use | |
| CN112900088B (en) | Biological modified fabric and preparation method thereof | |
| CN108048933B (en) | Copper-containing antibacterial viscose fiber and preparation method thereof | |
| BE1028623B1 (en) | METHOD OF SYNTHETING A FUNCTIONAL GEL FOR SURFACE MODIFICATION OF ARTIFICIAL GRASS FIBERS | |
| CN101210354A (en) | Method for preparing health care fibre and health care fibre produced by the same method | |
| EP0860522A1 (en) | Process for producing moulded articles from polysaccharide mixtures | |
| CN102373514A (en) | Glucomannan fiber and preparation method thereof | |
| CN111364139A (en) | Antibacterial polyester fiber blended yarn and preparation method thereof | |
| CN101314650B (en) | Nano-scale chitosan and latex coblended antibiont and preparation method thereof | |
| CN112609294B (en) | Environment-friendly antibacterial anti-mite fiber fabric for home textiles | |
| CN113699786A (en) | Cotton fiber-based lasting antibacterial fiber fabric and preparation method thereof | |
| EP2819711B1 (en) | Antiseptic wound dressing | |
| CN105920655B (en) | A kind of degradable compound operation suture | |
| AU2018102134A4 (en) | Preparation method of chitosan-allantoin regenerated cellulose fiber | |
| CN117265684B (en) | Preparation method and application of gentian viscose fiber with relieving effect | |
| CN113981610A (en) | Antibacterial keratin nanofiber membrane and preparation method thereof | |
| CN112899815A (en) | Method for preparing nanofiber antibacterial non-woven fabric by adopting chitin | |
| CN1552962A (en) | Producing method for antimite terylene hollow fibre | |
| WO2021074319A1 (en) | Process for producing a cellulosic functional fibre with high ion exchange capacity, cellulosic functional fibre, textile product comprising cellulosic functional fibre, and garment or piece of furniture comprising said cellulosic functional fibre or textile product | |
| JPS61239018A (en) | Continuous production of fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20240517 Address after: 276000 efficient and intensive demonstration park in Linyi Economic and Technological Development Zone, Shandong Province Applicant after: Shandong Xuhui non woven products Co.,Ltd. Country or region after: China Address before: No. 218, Jinlu 1st Road, management committee of Wuhou e-commerce industrial functional zone, Wuhou District, Chengdu, Sichuan 610000 Applicant before: Sun Dawei Country or region before: China |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |