CN112899815A - Method for preparing nanofiber antibacterial non-woven fabric by adopting chitin - Google Patents
Method for preparing nanofiber antibacterial non-woven fabric by adopting chitin Download PDFInfo
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- CN112899815A CN112899815A CN202110058367.9A CN202110058367A CN112899815A CN 112899815 A CN112899815 A CN 112899815A CN 202110058367 A CN202110058367 A CN 202110058367A CN 112899815 A CN112899815 A CN 112899815A
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- woven fabric
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- 229920002101 Chitin Polymers 0.000 title claims abstract description 67
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 61
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 54
- 239000002121 nanofiber Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 74
- 238000002156 mixing Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- -1 polypropylene Polymers 0.000 claims abstract description 26
- 239000002086 nanomaterial Substances 0.000 claims abstract description 25
- JXTHNDFMNIQAHM-UHFFFAOYSA-N dichloroacetic acid Chemical compound OC(=O)C(Cl)Cl JXTHNDFMNIQAHM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008187 granular material Substances 0.000 claims abstract description 24
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 24
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004743 Polypropylene Substances 0.000 claims abstract description 17
- 229920001155 polypropylene Polymers 0.000 claims abstract description 17
- 229920001661 Chitosan Polymers 0.000 claims abstract description 15
- 229960004494 calcium gluconate Drugs 0.000 claims abstract description 14
- 239000004227 calcium gluconate Substances 0.000 claims abstract description 14
- 235000013927 calcium gluconate Nutrition 0.000 claims abstract description 14
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims abstract description 14
- 235000013539 calcium stearate Nutrition 0.000 claims abstract description 14
- 239000008116 calcium stearate Substances 0.000 claims abstract description 14
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims abstract description 14
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000002787 reinforcement Effects 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 13
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 229960005215 dichloroacetic acid Drugs 0.000 claims abstract description 12
- 238000001125 extrusion Methods 0.000 claims abstract description 12
- 235000019253 formic acid Nutrition 0.000 claims abstract description 12
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000007935 neutral effect Effects 0.000 claims abstract description 12
- 238000007711 solidification Methods 0.000 claims abstract description 12
- 230000008023 solidification Effects 0.000 claims abstract description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 11
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002667 nucleating agent Substances 0.000 claims abstract description 9
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- FQUNFJULCYSSOP-UHFFFAOYSA-N bisoctrizole Chemical compound N1=C2C=CC=CC2=NN1C1=CC(C(C)(C)CC(C)(C)C)=CC(CC=2C(=C(C=C(C=2)C(C)(C)CC(C)(C)C)N2N=C3C=CC=CC3=N2)O)=C1O FQUNFJULCYSSOP-UHFFFAOYSA-N 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 7
- 239000010452 phosphate Substances 0.000 claims description 7
- SNAQARSCIHDMGI-UHFFFAOYSA-M sodium;bis(4-tert-butylphenyl) phosphate Chemical compound [Na+].C1=CC(C(C)(C)C)=CC=C1OP([O-])(=O)OC1=CC=C(C(C)(C)C)C=C1 SNAQARSCIHDMGI-UHFFFAOYSA-M 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- ZHROMWXOTYBIMF-UHFFFAOYSA-M sodium;1,3,7,9-tetratert-butyl-11-oxido-5h-benzo[d][1,3,2]benzodioxaphosphocine 11-oxide Chemical compound [Na+].C1C2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2OP([O-])(=O)OC2=C1C=C(C(C)(C)C)C=C2C(C)(C)C ZHROMWXOTYBIMF-UHFFFAOYSA-M 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005469 granulation Methods 0.000 description 9
- 230000003179 granulation Effects 0.000 description 9
- 239000000835 fiber Substances 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 5
- 230000005923 long-lasting effect Effects 0.000 description 5
- 238000005452 bending Methods 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002759 woven fabric Substances 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
- 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
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- 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
-
- 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
-
- 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
- D01F6/46—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 polyolefins
-
- 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
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/007—Addition polymers
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin, which comprises the following steps: adding calcium gluconate and ammonium hydrogen phosphate into water, adjusting the temperature to 105-115 ℃, stirring, filtering, washing to be neutral, drying and crushing to obtain a prefabricated nano material; uniformly mixing formic acid, dichloroacetic acid and water, adding chitin, chitosan and N-isopropylacrylamide, uniformly stirring, adding N, N-methylenebisacrylamide during stirring, continuously stirring, adding ammonium persulfate and ethylenediamine under a stirring state, stirring, adding a prefabricated nano material, and continuously stirring at the stirring temperature of 80-90 ℃ to obtain pretreated chitin; uniformly mixing polypropylene, pretreated chitin, a nucleating agent and calcium stearate, and then extruding and granulating by a double screw to obtain granules; and adding the granules into a single-screw extruder, and performing melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Description
Technical Field
The invention relates to the technical field of non-woven fabrics, in particular to a method for preparing a nano-fiber antibacterial non-woven fabric by adopting chitin.
Background
The non-woven fabric is a non-woven fabric, which is made from chemical fibers, plant fibers and the like by using water or air as a suspension medium on a wet or dry paper machine and then is formed by needling or hot rolling reinforcement. The non-woven fabric product has the advantages of rich color, brightness, fashion, environmental protection, wide application, elegant appearance, various patterns and styles, light weight, environmental protection and recycling, and is internationally recognized as an environmental protection product for protecting the earth ecology. Compared with common woven fabrics, the non-woven fabrics have the advantages of moisture resistance, air permeability, flexibility, light weight, convenient processing and the like, and are widely applied to various fields.
The non-woven fabric is a material processing technology originated from spinning but superior to spinning, and the main types of non-woven fabric products at home and abroad at present are pure cotton non-woven fabric, polyester/cotton blended non-woven fabric, viscose/cotton blended non-woven fabric, polyester/viscose blended non-woven fabric, wood pulp non-woven fabric and the like.
The non-woven fabric adopting the nano fibers is mainly characterized in that the diameter of the obtained fibers is very small, and the non-woven fabric formed by the fibers is a porous material with nano micropores and has a very large specific surface area, thereby showing specificity in the aspects of physical and chemical properties, having multiple potential applications and being widely used as antibacterial daily sanitary textiles. The existing nanofiber antibacterial non-woven fabric is mostly a nano silver-loaded antibacterial non-woven fabric, so that the antibacterial components are easy to fall off, the antibacterial aging is short, the fibers are easy to break, the mechanical property is poor, the actual production and life requirements are difficult to meet, and the problem is urgently needed to be solved.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for preparing a nanofiber antibacterial non-woven fabric by using chitin.
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding calcium gluconate and ammonium hydrogen phosphate into water, adjusting the temperature to 105-115 ℃, stirring, filtering, washing to be neutral, drying, and crushing to obtain a prefabricated nano material;
s2, uniformly mixing formic acid, dichloroacetic acid and water, adding chitin, chitosan and N-isopropylacrylamide, uniformly stirring, adding N, N-methylenebisacrylamide during stirring, continuously stirring, adding ammonium persulfate and ethylenediamine under a stirring state, stirring, adding a prefabricated nano material, and continuously stirring at the stirring temperature of 80-90 ℃ to obtain pretreated chitin;
s3, uniformly mixing polypropylene, pretreated chitin, a nucleating agent and calcium stearate, and then extruding and granulating by a double screw to obtain granules;
and S4, adding the granules into a single-screw extruder, and performing melt mixing, extrusion, air flow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Preferably, in S1, the mass ratio of calcium gluconate to ammonium hydrogen phosphate is 4-10: 15-25.
Preferably, in S1, the washing with clean water is neutral.
Preferably, in S2, the mass ratio of formic acid, dichloroacetic acid, chitin and chitosan is 10-15: 1-5: 10-20: 2-4.
Preferably, in S2, the mass ratio of chitin, N-isopropylacrylamide, N-methylenebisacrylamide, ammonium persulfate, ethylenediamine and the prefabricated nano-material is 10-20: 2-5: 0.1-0.18: 0.1-0.12: 1-2: 2-6.
Preferably, in S3, the mass ratio of the polypropylene, the pretreated chitin, the nucleating agent and the calcium stearate is 100: 10-20: 1-2: 1-2.
Preferably, in S3, the polypropylene has a melt mass flow rate of 2.4 to 3.7g/min, M, at 230 ℃ under a 2.16kg loadz/MwIs 2.5-2.95.
Wherein M iszIs an average molecular weight, MwIs the weight average molecular weight.
Preferably, in S3, the nucleating agent is an organophosphate nucleating agent, preferably one of sodium bis (4-tert-butylphenyl) phosphate, sodium 2,2 '-methylene-bis (4, 6-di-tert-butylphenyl) phosphate, and aluminum bis [2,2' -methylene-bis (4, 6-di-tert-butylphenyl) phosphate ] hydroxy.
Preferably, in S3, the temperature of the twin-screw extruder is as follows: the temperature of the 1 region is 150-.
Preferably, in S4, the single screw extruder temperature is 190-230 ℃.
The technical effects of the invention are as follows:
although chitin is a natural antibacterial agent, the heat resistance is poor, chitin and chitosan are dissolved in a mixed solvent of formic acid and dichloroacetic acid to react with N-isopropylacrylamide and N, N-methylenebisacrylamide to form a network hydrogel structure, so that the pretreated chitin has excellent antibacterial property, is not influenced by external environments such as temperature and the like, and can effectively ensure a lasting antibacterial effect.
According to the invention, calcium gluconate reacts with ammonium hydrogen phosphate at high temperature to form a two-dimensional nano network structure with negative charges on the surface, the two-dimensional nano network structure can be effectively coated and firmly combined on the surface of the product grafted with chitosan with positive charges, the formed strong hydrogen bond network can effectively improve the tensile strength of pretreated chitin, the phenomenon of agglomeration caused by the addition of the two-dimensional nano network structure can be avoided, the product has good dispersibility, and meanwhile, the non-woven fabric is formed by crosswise and crosswise stacking a large number of nano fibers, so that the antibacterial effect is long-lasting, the fibers are not easy to break, and the mechanical property is excellent.
The non-woven fabric obtained by the invention not only has remarkable antibacterial performance, but also has stable antibacterial performance, long antibacterial aging and high mechanical strength.
Compared with the prior art, the invention has good antibacterial and temperature-resistant effects on the premise of maintaining good mechanical properties, and long antibacterial aging,
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
The melt mass flow rate of the polypropylene used is 2.4-3.7g/min at 230 ℃ under a load of 2.16kg, Mz/MwIs 2.5-2.95.
Example 1
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding 4kg of calcium gluconate, 25kg of ammonium hydrogen phosphate and 100kg of water into a reaction kettle, stirring for 30 hours at the temperature of 105 ℃, filtering, washing with water to be neutral, drying and crushing to obtain a prefabricated nano material;
s2, uniformly mixing 10kg of formic acid, 5kg of dichloroacetic acid and 40kg of water, adding 20kg of chitin, 2kg of chitosan and 5kg of N-isopropylacrylamide, uniformly stirring, adding 0.1kg of N, N-methylene bisacrylamide in the stirring process, continuously stirring for 20min, continuously adding 0.1kg of ammonium persulfate and 2kg of ethylenediamine in the stirring state, stirring for 1h, adding 6kg of prefabricated nano material, continuously stirring for 15min, wherein the stirring temperature is 90 ℃, and obtaining pretreated chitin;
s3, adding 100kg of polypropylene, 10kg of pretreated chitin, 2kg of sodium bis (4-tert-butylphenyl) phosphate and 1kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the zone 1 is 160 ℃, the temperature of the zone 2 is 165 ℃, the temperature of the zone 3 is 200 ℃, the temperature of the zone 4 is 200 ℃, the temperature of the zone 5 is 240 ℃, and the temperature of the zone 6 is 200 ℃;
and S4, adding the granules into a single-screw extruder, wherein the screw temperature is 230 ℃, and carrying out melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Example 2
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding 10kg of calcium gluconate, 15kg of ammonium hydrogen phosphate and 100kg of water into a reaction kettle, stirring for 20 hours at the temperature of 115 ℃, filtering, washing with water to be neutral, drying and crushing to obtain a prefabricated nano material;
s2, mixing 15kg of formic acid, 1kg of dichloroacetic acid and 60kg of water uniformly, adding 10kg of chitin, 4kg of chitosan and 2kg of N-isopropylacrylamide, stirring uniformly, adding 0.18kg of N, N-methylene bisacrylamide during stirring, continuing to stir for 10min, continuing to add 0.12kg of ammonium persulfate and 1kg of ethylenediamine under stirring, stirring for 2h, adding 2kg of prefabricated nano material, continuing to stir for 35min, wherein the stirring temperature is 80 ℃, and obtaining pretreated chitin;
s3, adding 100kg of polypropylene, 20kg of pretreated chitin, 1kg of sodium bis (4-tert-butylphenyl) phosphate and 2kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 150 ℃, the temperature of the 2 area is 175 ℃, the temperature of the 3 area is 180 ℃, the temperature of the 4 area is 230 ℃, the temperature of the 5 area is 210 ℃ and the temperature of the 6 area is 220 ℃;
and S4, adding the granules into a single-screw extruder, wherein the screw temperature is 190 ℃, and carrying out melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Example 3
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding 6kg of calcium gluconate, 22kg of ammonium hydrogen phosphate and 100kg of water into a reaction kettle, stirring for 27 hours at the temperature of 108 ℃, filtering, washing with water to be neutral, drying and crushing to obtain a prefabricated nano material;
s2, uniformly mixing 12kg of formic acid, 4kg of dichloroacetic acid and 45kg of water, adding 18kg of chitin, 2.5kg of chitosan and 4kg of N-isopropylacrylamide, uniformly stirring, adding 0.12kg of N, N-methylene bisacrylamide in the stirring process, continuously stirring for 18min, continuously adding 0.105kg of ammonium persulfate and 1.7kg of ethylenediamine in the stirring state, stirring for 1.2h, adding 5kg of prefabricated nano material, continuously stirring for 20min, wherein the stirring temperature is 88 ℃, and thus obtaining pretreated chitin;
s3, adding 100kg of polypropylene, 13kg of pretreated chitin, 1.7kg of 2,2' -methylene-bis (4, 6-di-tert-butylphenyl) sodium phosphate and 1.2kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 158 ℃, the temperature of the 2 area is 168 ℃, the temperature of the 3 area is 195 ℃, the temperature of the 4 area is 210 ℃, the temperature of the 5 area is 230 ℃, and the temperature of the 6 area is 205 ℃;
and S4, adding the granules into a single-screw extruder, wherein the screw temperature is 220 ℃, and carrying out melt mixing, extrusion, air flow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Example 4
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding 8kg of calcium gluconate, 18kg of ammonium hydrogen phosphate and 100kg of water into a reaction kettle, stirring for 23 hours at the temperature of 112 ℃, filtering, washing with water to be neutral, drying and crushing to obtain a prefabricated nano material;
s2, uniformly mixing 14kg of formic acid, 2kg of dichloroacetic acid and 55kg of water, adding 12kg of chitin, 3.5kg of chitosan and 3kg of N-isopropylacrylamide, uniformly stirring, adding 0.16kg of N, N-methylene bisacrylamide in the stirring process, continuously stirring for 12min, continuously adding 0.115kg of ammonium persulfate and 1.3kg of ethylenediamine in the stirring state, stirring for 1.8h, adding 3kg of prefabricated nano material, continuously stirring for 30min at the stirring temperature of 82 ℃ to obtain pretreated chitin;
s3, adding 100kg of polypropylene, 17kg of pretreated chitin, 1.3kg of 2,2' -methylene-bis (4, 6-di-tert-butylphenyl) sodium phosphate and 1.8kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 152 ℃, the temperature of the 2 area is 172 ℃, the temperature of the 3 area is 185 ℃, the temperature of the 4 area is 220 ℃, the temperature of the 5 area is 220 ℃, and the temperature of the 6 area is 215 ℃;
and S4, adding the granules into a single-screw extruder, controlling the screw temperature at 200 ℃, and performing melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Example 5
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding 7kg of calcium gluconate, 20kg of ammonium hydrogen phosphate and 100kg of water into a reaction kettle, stirring for 25 hours at the temperature of 110 ℃, filtering, washing with water to be neutral, drying and crushing to obtain a prefabricated nano material;
s2, uniformly mixing 13kg of formic acid, 3kg of dichloroacetic acid and 50kg of water, adding 15kg of chitin, 3kg of chitosan and 3.5kg of N-isopropylacrylamide, uniformly stirring, adding 0.14kg of N, N-methylene bisacrylamide in the stirring process, continuously stirring for 15min, continuously adding 0.11kg of ammonium persulfate and 1.5kg of ethylenediamine in the stirring state, stirring for 1.5h, adding 4kg of prefabricated nano material, continuously stirring for 25min, wherein the stirring temperature is 85 ℃, and obtaining pretreated chitin;
s3, adding 100kg of polypropylene, 15kg of pretreated chitin, 1.5kg of bis [2,2' -methylene-bis (4, 6-di-tert-butylphenyl) phosphate ] aluminum hydroxide and 1.5kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 155 ℃, the temperature of the 2 area is 170 ℃, the temperature of the 3 area is 190 ℃, the temperature of the 4 area is 215 ℃, the temperature of the 5 area is 225 ℃ and the temperature of the 6 area is 210 ℃;
and S4, adding the granules into a single-screw extruder, wherein the screw temperature is 210 ℃, and carrying out melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Comparative example 1
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, uniformly mixing 13kg of formic acid, 3kg of dichloroacetic acid and 50kg of water, adding 15kg of chitin, 3kg of chitosan and 3.5kg of N-isopropylacrylamide, uniformly stirring, adding 0.14kg of N, N-methylene bisacrylamide in the stirring process, continuously stirring for 15min, continuously adding 0.11kg of ammonium persulfate and 1.5kg of ethylenediamine in the stirring state, stirring for 1.5h, and stirring at the temperature of 85 ℃ to obtain pretreated chitin;
s2, adding 100kg of polypropylene, 15kg of pretreated chitin, 1.5kg of bis [2,2' -methylene-bis (4, 6-di-tert-butylphenyl) phosphate ] aluminum hydroxide and 1.5kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 155 ℃, the temperature of the 2 area is 170 ℃, the temperature of the 3 area is 190 ℃, the temperature of the 4 area is 215 ℃, the temperature of the 5 area is 225 ℃ and the temperature of the 6 area is 210 ℃;
and S3, adding the granules into a single-screw extruder, wherein the screw temperature is 210 ℃, and carrying out melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Comparative example 2
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding 7kg of calcium gluconate, 20kg of ammonium hydrogen phosphate and 100kg of water into a reaction kettle, stirring for 25 hours at the temperature of 110 ℃, filtering, washing with water to be neutral, drying and crushing to obtain a prefabricated nano material;
s2, stirring 15kg of chitin and 4kg of prefabricated nano material for 25min at the stirring temperature of 85 ℃ to obtain pretreated chitin;
s3, adding 100kg of polypropylene, 15kg of pretreated chitin, 1.5kg of bis [2,2' -methylene-bis (4, 6-di-tert-butylphenyl) phosphate ] aluminum hydroxide and 1.5kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 155 ℃, the temperature of the 2 area is 170 ℃, the temperature of the 3 area is 190 ℃, the temperature of the 4 area is 215 ℃, the temperature of the 5 area is 225 ℃ and the temperature of the 6 area is 210 ℃;
and S4, adding the granules into a single-screw extruder, wherein the screw temperature is 210 ℃, and carrying out melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Comparative example 3
A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin comprises the following steps:
s1, adding 100kg of polypropylene, 15kg of chitin, 1.5kg of bis [2,2' -methylene-bis (4, 6-di-tert-butylphenyl) phosphate ] aluminum hydroxide and 1.5kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 155 ℃, the temperature of the 2 area is 170 ℃, the temperature of the 3 area is 190 ℃, the temperature of the 4 area is 215 ℃, the temperature of the 5 area is 225 ℃ and the temperature of the 6 area is 210 ℃;
and S2, adding the granules into a single-screw extruder, wherein the screw temperature is 210 ℃, and carrying out melt mixing, extrusion, airflow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
Comparative example 4
A preparation method of nanofiber non-woven fabric comprises the following steps:
s1, adding 7kg of calcium gluconate, 20kg of ammonium hydrogen phosphate and 100kg of water into a reaction kettle, stirring for 25 hours at the temperature of 110 ℃, filtering, washing with water to be neutral, drying and crushing to obtain a prefabricated nano material;
s2, adding 100kg of polypropylene, 4kg of prefabricated nano material, 1.5kg of bis [2,2' -methylene-bis (4, 6-di-tert-butylphenyl) phosphate ] aluminum hydroxide and 1.5kg of calcium stearate into a stirrer, uniformly mixing, and then feeding into a double-screw extruder for granulation to obtain granules; the temperature of each part of the double-screw extruder is as follows:
the temperature of the 1 area is 155 ℃, the temperature of the 2 area is 170 ℃, the temperature of the 3 area is 190 ℃, the temperature of the 4 area is 215 ℃, the temperature of the 5 area is 225 ℃ and the temperature of the 6 area is 210 ℃;
and S3, adding the granules into a single-screw extruder, wherein the screw temperature is 210 ℃, and carrying out melt mixing, extrusion, air flow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber non-woven fabric.
The nonwoven fabrics obtained in example 5 and comparative examples 1 to 4 were subjected to the following mechanical property tests: the bending length and the bending rigidity are measured according to GB/T18318.1-2009, and the sample size is 25mm multiplied by 200 mm; the breaking strength and breaking elongation are tested according to GB/T3923.1-2013.
The results are as follows:
the shorter the bending length, the lower the bending rigidity, indicating that the softness of the nonwoven fabric is better.
From the above table, it can be seen that: the softness of the non-woven fabric is moderate, the breaking strength and the breaking elongation of the non-woven fabric are superior to those of a comparative example, and the non-woven fabric is soft and high in mechanical performance.
According to the invention, calcium gluconate reacts with ammonium hydrogen phosphate at high temperature to form a two-dimensional nano network structure with negative charges on the surface, and the two-dimensional nano network structure can be effectively coated and firmly combined on the surface of the product grafted with chitosan with positive charges, so that the strong hydrogen bond network can effectively improve the tensile strength of the product.
The nonwoven fabrics obtained in example 5 and comparative examples 1 to 4 were subjected to the antibacterial property test as follows: respectively adopting ATCC6538 staphylococcus aureus, ATCC25922 escherichia coli and ATCC27853 pseudomonas aeruginosa, wherein the number of the bacteria is 1.12 multiplied by 107And (3) drop-dyeing each group of non-woven fabrics by cfu/mL, washing a bacterial colony by distilled water after the drop-dyeing is carried out for different time, culturing the washed solution in a constant-temperature water bath at 37 ℃ for 24 hours, measuring the number of bacteria contained in the solution, and calculating the sterilization rate.
The results are shown below:
from the above table, it can be seen that: the non-woven fabric obtained by the invention has excellent antibacterial and sterilization performance, and the antibacterial effect is long-lasting and long-lasting as time goes on, because the non-woven fabric is formed by criss-cross lamination of a large number of nano fibers, the pretreated chitin is wrapped by the nano fibers, and the pretreated chitin gradually migrates to the surface as time goes on, so that the antibacterial effect is long-lasting and long-lasting.
In contrast, comparative example 1, no preformed nanomaterial was added, but the effect on antibacterial performance was small; comparative example 2 the chitin and the prefabricated nano material are directly mixed, so that the prefabricated nano material is not uniformly dispersed, and the antibacterial effect is gradually deteriorated along with the time; comparative example 3 only adopts chitin, which causes poor antibacterial effect, chitin gradually migrates to the surface along with the passage of time, and the antibacterial effect is gradually improved; in comparative example 4, the antibacterial effect was poor due to no addition of chitin/chitosan, and the antibacterial effect was increasingly poor with the passage of time.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method for preparing nano-fiber antibacterial non-woven fabric by adopting chitin is characterized by comprising the following steps:
s1, adding calcium gluconate and ammonium hydrogen phosphate into water, adjusting the temperature to 105-115 ℃, stirring, filtering, washing to be neutral, drying, and crushing to obtain a prefabricated nano material;
s2, uniformly mixing formic acid, dichloroacetic acid and water, adding chitin, chitosan and N-isopropylacrylamide, uniformly stirring, adding N, N-methylenebisacrylamide during stirring, continuously stirring, adding ammonium persulfate and ethylenediamine under a stirring state, stirring, adding a prefabricated nano material, and continuously stirring at the stirring temperature of 80-90 ℃ to obtain pretreated chitin;
s3, uniformly mixing polypropylene, pretreated chitin, a nucleating agent and calcium stearate, and then extruding and granulating by a double screw to obtain granules;
and S4, adding the granules into a single-screw extruder, and performing melt mixing, extrusion, air flow stretching, cooling solidification, paving and reinforcement to obtain the nanofiber antibacterial non-woven fabric.
2. The method for preparing nanofiber antibacterial non-woven fabric by using chitin according to claim 1, wherein in S1, the mass ratio of calcium gluconate to ammonium hydrogen phosphate is 4-10: 15-25.
3. The method of claim 1, wherein the step of washing the nanofiber nonwoven fabric with clear water to be neutral in S1.
4. The method for preparing nanofiber antibacterial non-woven fabric by using chitin according to claim 1, wherein in S2, the mass ratio of formic acid, dichloroacetic acid, chitin and chitosan is 10-15: 1-5: 10-20: 2-4.
5. The method for preparing nanofiber antibacterial non-woven fabric by using chitin according to claim 1, wherein in S2, the mass ratio of chitin, N-isopropylacrylamide, N-methylenebisacrylamide, ammonium persulfate, ethylenediamine and the prefabricated nano-material is 10-20: 2-5: 0.1-0.18: 0.1-0.12: 1-2: 2-6.
6. The method for preparing nanofiber antibacterial non-woven fabric by using chitin according to claim 1, wherein in S3, the mass ratio of polypropylene, pretreated chitin, nucleating agent and calcium stearate is 100: 10-20: 1-2: 1-2.
7. The method of claim 1, wherein in S3, the melt mass flow rate of polypropylene under a load of 2.16kg at 230 ℃ is 2.4-3.7g/min, M is Mz/MwIs 2.5-2.95.
8. The method of claim 1, wherein the nucleating agent in S3 is an organophosphate nucleating agent, preferably one of sodium bis (4-tert-butylphenyl) phosphate, sodium 2,2 '-methylene-bis (4, 6-di-tert-butylphenyl) phosphate, and aluminum bis [2,2' -methylene-bis (4, 6-di-tert-butylphenyl) phosphate ] hydroxy.
9. The method of preparing nanofiber antibacterial nonwoven fabric using chitin according to claim 1, wherein in S3, the temperature of the twin-screw extruder is as follows: the temperature of the 1 region is 150-.
10. The method of claim 1, wherein the temperature of the single screw extruder in S4 is 190-230 ℃.
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