CN111364115A - Antibacterial polyester fiber and fabric - Google Patents
Antibacterial polyester fiber and fabric Download PDFInfo
- Publication number
- CN111364115A CN111364115A CN202010204688.0A CN202010204688A CN111364115A CN 111364115 A CN111364115 A CN 111364115A CN 202010204688 A CN202010204688 A CN 202010204688A CN 111364115 A CN111364115 A CN 111364115A
- Authority
- CN
- China
- Prior art keywords
- polyester fiber
- antibacterial
- antibacterial polyester
- fabric
- stirring
- 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.)
- Withdrawn
Links
- 229920000728 polyester Polymers 0.000 title claims abstract description 105
- 239000000835 fiber Substances 0.000 title claims abstract description 78
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 76
- 239000004744 fabric Substances 0.000 title claims abstract description 72
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 21
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000004714 phosphonium salts Chemical group 0.000 claims abstract description 13
- 238000009987 spinning Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 8
- PAAZPARNPHGIKF-UHFFFAOYSA-N 1,2-dibromoethane Chemical compound BrCCBr PAAZPARNPHGIKF-UHFFFAOYSA-N 0.000 claims abstract description 6
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 6
- 150000001469 hydantoins Chemical class 0.000 claims abstract description 5
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 4
- 238000006467 substitution reaction Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 23
- 239000004627 regenerated cellulose Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 229920003043 Cellulose fiber Polymers 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 239000013067 intermediate product Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 9
- 239000000155 melt Substances 0.000 claims description 9
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical group CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical group CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003242 anti bacterial agent Substances 0.000 claims description 7
- 238000007493 shaping process Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 238000005098 hot rolling Methods 0.000 claims description 6
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000003115 biocidal effect Effects 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 230000032050 esterification Effects 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003063 flame retardant Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 8
- 230000007547 defect Effects 0.000 abstract description 6
- 244000005700 microbiome Species 0.000 abstract description 6
- 241000894006 Bacteria Species 0.000 abstract description 4
- 241000233866 Fungi Species 0.000 abstract description 4
- 238000004043 dyeing Methods 0.000 abstract description 4
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 abstract description 3
- 229940053195 antiepileptics hydantoin derivative Drugs 0.000 abstract description 3
- 238000003541 multi-stage reaction Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000009941 weaving Methods 0.000 abstract description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 28
- 229920004933 Terylene® Polymers 0.000 description 17
- 229920000139 polyethylene terephthalate Polymers 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 6
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 6
- 230000000845 anti-microbial effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000003466 anti-cipated effect Effects 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008034 disappearance Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- YIROYDNZEPTFOL-UHFFFAOYSA-N 5,5-Dimethylhydantoin Chemical compound CC1(C)NC(=O)NC1=O YIROYDNZEPTFOL-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- BLORRZQTHNGFTI-ZZMNMWMASA-L calcium-L-ascorbate Chemical compound [Ca+2].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] BLORRZQTHNGFTI-ZZMNMWMASA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
- D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/692—Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus
- C08G63/6924—Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6926—Dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/04—Blended or other yarns or threads containing components made from different materials
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/449—Yarns or threads with antibacterial properties
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/02—Setting
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
- D10B2201/20—Cellulose-derived artificial fibres
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/13—Physical properties anti-allergenic or anti-bacterial
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the field of new materials. The invention relates to an antibacterial polyester fiber and fabric, which are prepared from hydantoin derivatives (A), 1, 2-dibromoethane (B), triphenyl quaternary phosphonium salt (C), epichlorohydrin (D), terephthalic acid (E) and ethylene glycol (F) through substitution, polycondensation and other multi-step reactions, a spinning process and a weaving process. The antibacterial polyester fabric not only effectively overcomes the defect that the existing polyester is easy to breed bacteria, fungi and other microorganisms after dyeing and finishing processing, but also has high-efficiency flame retardant performance and antistatic performance, and foresees that the material can meet wide market space, and is particularly suitable for the fields of clothing and the like.
Description
Technical Field
The invention relates to an antibacterial polyester fiber and a fabric. The invention belongs to the field of new materials.
Background
Terylene is also called polyester fiber, and is called PET fiber for short. The terylene is a synthetic fiber with low price and simple preparation process. The fabric has the advantages of high strength, good elasticity, easy washing and quick drying, and the like, is gradually popular in the market and is widely applied to the fields of clothing, industry, medical treatment and health care, and the like. The terylene has excellent physical and mechanical properties due to the fact that the structural units of the terylene contain rigid benzene rings and flexible aliphatic hydrocarbon groups, such as: high breaking strength and modulus, and good thermal and dimensional stability. However, the polyester fiber is a typical hydrophobic fiber, the moisture regain is only 0.4%, the wearing comfort is poor, charges are easy to accumulate to cause static electricity, the processing of the polyester fiber is difficult, dust is easy to adsorb, the anti-fouling capability is reduced, and the application of products in some fields is limited.
The chemical structure of the terylene leads to the extremely poor hydrophilicity of the terylene fibers, thus leading to the defects of hard handfeel, poor touch feeling, poor hygroscopicity and the like of the terylene fabric, and the terylene fabric has a certain antibacterial property due to the poor hygroscopicity of the terylene, but the terylene does not contain antibacterial active groups and can not maintain the long-term antibacterial and mildewproof performance. In the prior art, in the dyeing and finishing process of terylene, various additives and finishing agents can provide nutrient substances for microorganisms, and when the temperature and the humidity are suitable for growth, the microorganisms can grow and propagate on textiles in large quantities. This not only threatens the health of people, but also may cause significant medical accidents.
Therefore, the selection of the antibacterial agent and the antibacterial finishing technology play a key role in the development of the healthy and sanitary terylene. In recent years, the traditional antibacterial agent and finishing technology have the defects of low bonding degree with fibers, poor washing fastness and poor antibacterial durability. Therefore, it is more important to develop polyester fibers and fabrics which are antibacterial per se.
Disclosure of Invention
The invention aims to provide an antibacterial polyester fiber and fabric aiming at the defect that microorganisms such as bacteria and fungi are easy to breed after dyeing and finishing treatment is carried out on a polyester fabric in the prior art, the antibacterial polyester fiber and fabric are obtained by using hydantoin derivatives (A), 1, 2-dibromoethane (B), triphenyl quaternary phosphonium salt (C), epichlorohydrin (D), terephthalic acid (E) and ethylene glycol (F) as raw materials through multi-step reactions such as substitution, polycondensation and the like, a spinning process and a weaving process, the defect that microorganisms such as bacteria and fungi are easy to breed after dyeing and finishing treatment on the existing polyester is overcome, and the material has high-efficiency antibacterial property and a flame retardant property. It is anticipated that this material will appeal to a wide market space.
The technical scheme adopted by the invention for solving the technical problems is as follows:
an antibacterial polyester fiber has a structural formula as follows:
wherein, -R1：-CH3、-C5H9；-R2：-CH3、-C3H7、-C6H13、-C6H5or-C5H9。
A preparation method of antibacterial polyester fiber is characterized by comprising the following steps: comprises the following steps:
step (1): coupling reaction to obtain an intermediate product I;
step (2): coupling reaction to obtain an intermediate product II;
and (3): carrying out substitution reaction to obtain an intermediate product III;
and (4): performing polycondensation reaction to obtain polyester with an antibacterial function, namely a target product IV;
and (5): spinning the target product IV into the antibacterial polyester fiber.
Preferably, the step (1) is specifically:
adding 1mol of hydantoin derivative (A) and 1-1.2mol of 1, 2-dibromoethane (B) into 50mol of organic solvent a, heating to 70-85 ℃, strongly stirring for 1-6h, cooling, standing, and vacuum concentrating; slowly adding 50mol of water, stirring for 30min, adding 80mol of organic solvent b, stirring for 30min, standing for layering, taking an organic phase, drying with anhydrous sodium sulfate, filtering, and performing rotary evaporation to obtain an intermediate product I.
Preferably, the step (2) is specifically:
adding 1mol of I and 1-1.2mol of quaternary phosphonium salt (C) into 50mol of organic solvent a, heating to 75-85 ℃, stirring strongly for 4-8h, cooling, standing, rotary evaporating, purifying, and drying to obtain an intermediate product II.
Preferably, the step (3) is specifically:
under the protection of nitrogen, dissolving 1mol of II, 1-1.2mol of epichlorohydrin (D) and 1-1.2mol of potassium iodide in 50mol of organic solvent a, heating to 85-110 ℃, strongly stirring for 20-28h, cooling, standing, vacuum concentrating, purifying and vacuum drying to obtain an intermediate product III.
Preferably, the step (4) is specifically:
stirring 1mol of terephthalic acid (E), 0.05-0.1mol of III, 1mol of ethylene glycol (F) and 0.05-1 wt% of catalyst, heating, and filling nitrogen to keep 0.15 MPa; the reaction temperature is controlled at 230 ℃ of 200-; recording the reaction temperature and pressure in the esterification process; the degree of polymerization reaction is judged by observing the current and torque change of a motor, and after the discharging condition is reached, nitrogen is introduced until the pressure is 0.17-0.20MPa, so that a PET product is obtained; opening a discharge valve to allow the melt to flow out of a casting strip head, cooling the casting strip through a cooling water tank, introducing the casting strip into a granulator, and granulating to obtain PET granules, namely a target product IV;
the catalyst is used in an amount based on parts by weight of terephthalic acid.
Preferably, the step (5) is specifically:
vacuum drying the PET granules IV at 80 ℃ for 5h, and vacuum drying at 120 ℃ for 24 h; stirring at high speed, mixing uniformly, putting into a double-screw extruder, performing melt extrusion to obtain a melt, outputting the melt into a spinning machine for spinning, drafting and cooling to obtain fibers, forming the fibers into a net by a net former, conveying the net-formed fibers into a hot rolling machine, and performing hot rolling at 90-95 ℃ and 3.2-3.7MPa to obtain the antibacterial polyester fibers.
Preferably, the organic solvent a is N, N-dimethylformamide or dimethyl sulfoxide.
Preferably, the organic solvent b is ethyl acetate, chloroform or dimethyl sulfoxide.
Preferably, the catalyst is 4-dimethylaminopyridine, zinc acetate or antimony trioxide.
Preferably, the diameter of the screw of the twin-screw extruder is 18-22mm, and the length-diameter ratio of the screw is 22.
Preferably, the spinning temperature is 200 ℃.
The utility model provides an antibiotic polyester fabric, is formed by antibiotic polyester fiber, polyester fiber and the blending of regenerated cellulose base fibre which characterized in that: comprises the following raw materials in parts by weight
20-40 parts of antibacterial polyester fiber;
40-60 parts of polyester fiber;
15-25 parts of regenerated cellulose fiber.
Preferably, the preparation method of the antibacterial polyester fabric comprises the following steps:
(1) the antibacterial polyester fiber, the polyester fiber and the regenerated cellulose fiber are blended into warp yarn and weft yarn according to a proportion, and the warp yarn and the weft yarn are mutually blended into grey cloth by right-angle staggered surfaces;
(2) raising the temperature to 200 ℃, and drying and shaping the grey cloth, wherein the drying speed is in the range of 24Y/min to 26Y/min; and obtaining the antibacterial polyester fabric.
The invention provides an antibacterial polyester fiber, which is prepared by the following steps:
the invention has the beneficial effects that:
(1) the invention provides an antibacterial polyester fiber, which is prepared by adopting hydantoin derivatives (A), 1, 2-dibromoethane (B), triphenyl quaternary phosphonium salt (C), epichlorohydrin (D), terephthalic acid (E) and ethylene glycol (F) as raw materials.
(2) The invention provides an antibacterial polyester fiber and fabric, and a target product contains a quaternary phosphonium salt and a quaternary ammonium salt structure. Firstly, N, P has excellent antibacterial property as the same main group element, and the quaternary phosphonium salt has larger atomic radius, stronger adsorbability and better antibacterial property; the quaternary ammonium salt has wide source and more selectivity; secondly, the presence of N, P gives the material better flame retardancy; and finally, the ionic forms of the quaternary ammonium salt and the quaternary phosphonium salt can increase the hydrophilicity of the polyester fiber and the fabric.
(3) The invention provides an antibacterial polyester fiber and a fabric, and a target product contains a halamine structure. On one hand, the halamine has the characteristics of high sterilization speed, wide antimicrobial spectrum, reproducibility and no environmental pollution, and hardly generates drug resistance; on the other hand, the presence of quaternary ammonium salts, quaternary phosphonium salts, and haloamines provide synergistic antimicrobial effects.
(4) The invention provides an antibacterial polyester fiber and a fabric, on one hand, an antibacterial structure is added in a polyester polymerization stage through molecular design, so that the defect that microorganisms such as bacteria, fungi and the like are easy to breed after the existing polyester is treated is overcome, the material has high-efficiency antibacterial property and simultaneously has higher antistatic property and flame retardance; on the other hand, the antistatic effect of the fabric can be further improved by blending the regenerated cellulose fibers, and the fabric is more comfortable. It is anticipated that this material will appeal to a wide market space.
The specific implementation mode is as follows:
the present invention will be described in detail with reference to examples. It is to be understood, however, that the following examples are illustrative of embodiments of the present invention and are not to be construed as limiting the scope of the invention.
Example 1
The preparation method of the antibacterial polyester fiber comprises the following steps:
adding 1mol of 5, 5-dimethylhydantoin (A) and 1.2mol of 1, 2-dibromoethane (B) into 50mol of N, N-dimethylformamide, heating to 80 ℃, strongly stirring for 2h, cooling, standing, and vacuum concentrating; slowly adding 50mol water, stirring for 30min, adding 80mol chloroform, stirring for 30min, standing for layering, drying organic phase with anhydrous sodium sulfate, filtering, and rotary steaming to obtain intermediate product I (IR: 1051 cm)-1: tertiary amine-C-N-formation; 1672cm-1: amide-C ═ O is present; 644cm-1: -C-Br present).
Step (2) adding 1mol of the quaternary phosphonium salt (C) and 1.1mol of the quaternary phosphonium salt (I) into 50mol of N, N-dimethylformamide, heating to 80 ℃, stirring strongly for 6h, cooling, standing, rotary evaporating, purifying and drying to obtain an intermediate product II (IR: 644 cm)-1: -C-Br disappearance; 1074cm-1: -N-is present; 1673cm-1: amides of carboxylic acids-C ═ O is present; 3100cm-1、1489cm-1、1449cm-1、715cm-1: a benzene ring; 1097cm-1：P-Ph)。
Under the protection of nitrogen, dissolving 1mol of II, 1.2mol of epichlorohydrin (D) and 1.2mol of potassium iodide in 50mol of N, N-dimethylformamide, heating to 85 ℃, strongly stirring for 28h, cooling, standing, vacuum concentrating, purifying and vacuum drying to obtain an intermediate product III (IR: 1074 cm)-1: -N-is present; 1672cm-1: amide-C ═ O is present; 3100cm-1、1489cm-1、1449cm-1、715cm-1: a benzene ring; 1097cm-1：P-Ph；910cm-1: epoxy groups are present).
Step (4) stirring 1mol of terephthalic acid (E), 0.1mol of III, 1mol of ethylene glycol (F) and 1 wt% of 4-dimethylamino pyridine, heating, raising the temperature, and filling nitrogen to keep 0.15 MPa; controlling the reaction temperature at 200 ℃, supplementing 0.5mol of ethylene glycol (F), and keeping the pressure at 0.30 MPa; recording the reaction temperature and pressure in the esterification process; the polymerization degree is judged by observing the current and torque change of the motor, and after the discharge condition is reached, nitrogen is introduced until the pressure is 0.17MPa, so that a PET product is obtained; opening a discharge valve to allow the melt to flow out of a casting belt head, cooling the casting belt strip through a cooling water tank, introducing the casting belt strip into a granulator, and granulating to obtain PET granules, namely a target product IV (IR: 1074 cm)-1: -N-is present; 1672cm-1: amide-C ═ O is present; 1740cm-1: ester-C ═ O present; 3100cm-1、1489cm-1、1449cm-1、715cm-1: a benzene ring; 1097cm-1：P-Ph；910cm-1: disappearance of epoxy groups; 3532cm-1: -OH is present).
The 4-dimethylaminopyridine is used in an amount based on parts by weight of terephthalic acid.
Step (5), drying the PET granules IV in vacuum at 80 ℃ for 5h, and drying in vacuum at 120 ℃ for 24 h; stirring at a high speed, uniformly mixing, placing in a double-screw extruder, selecting the diameter of a screw of the double-screw extruder to be 20mm and the length-diameter ratio of the screw to be 22, carrying out melt extrusion to obtain a melt, outputting the melt to a spinning machine for spinning at 200 ℃, drafting and cooling to obtain fibers, forming the fibers into a net by a net former, conveying the net-formed fibers to a hot rolling mill, and carrying out hot rolling at 90 ℃ and 3.2MPa to obtain the antibacterial polyester fibers.
The antibacterial polyester fabric blending composition and the process are as follows:
an antibacterial polyester fabric is formed by blending antibacterial polyester fibers, polyester fibers and regenerated cellulose fibers and comprises the following raw materials in parts by weight
20 parts of antibacterial polyester fiber;
60 parts of polyester fiber;
20 parts of regenerated cellulose fiber.
The preparation method of the antibacterial polyester fabric comprises the following steps:
(1) the antibacterial polyester fiber, the polyester fiber and the regenerated cellulose fiber are blended into warp yarn and weft yarn according to the proportion, and the warp yarn and the weft yarn are mutually blended into grey cloth by right-angle staggered surfaces;
(2) raising the temperature to 200 ℃, and drying and shaping the grey cloth, wherein the drying speed is 24Y/min; and obtaining the antibacterial polyester fabric.
The preparation of the antibacterial polyester fiber and the fabric is as in the specific examples 2-6, and the other steps are as in the specific example 1, except that:
comparative examples 1-4 are all compared to the antimicrobial polyester face fabric of example 1, with the antimicrobial structure content of example 1 amounting to about 2.6 wt%.
Comparative example 1
The terylene fabric is blended by terylene fibers and regenerated cellulose fibers and comprises the following raw materials in parts by weight
80 parts of polyester fiber; 20 parts of regenerated cellulose fiber.
The preparation method of the polyester fabric comprises the following steps:
(1) blending the polyester fiber and the regenerated cellulose fiber into warp yarn and weft yarn according to the proportion, and blending the warp yarn and the weft yarn mutually at right angles in a staggered manner to form grey cloth;
(2) raising the temperature to 200 ℃, and drying and shaping the grey cloth, wherein the drying speed is 24Y/min; and obtaining the antibacterial polyester fabric.
Comparative example 2
The polyester fabric comprises the following components in parts by weight:
an antibacterial polyester fabric is formed by blending antibacterial polyester fibers, polyester fibers and regenerated cellulose fibers and comprises the following raw materials in parts by weight
2.6 parts of an antibacterial agent; 77.4 parts of polyester fiber; 20 parts of regenerated cellulose fiber.
The preparation method of the antibacterial polyester fabric comprises the following steps:
(1) after the antibacterial agent and the PET slices are blended, extruded and melt spun, the antibacterial agent and the regenerated cellulose fiber are blended into warp yarns and weft yarns according to the proportion, and the warp yarns and the weft yarns are mutually blended into grey cloth in a right-angle staggered mode;
(2) raising the temperature to 200 ℃, and drying and shaping the grey cloth, wherein the drying speed is 24Y/min; and obtaining the antibacterial polyester fabric.
Comparative example 3
The polyester fabric comprises the following components in parts by weight:
the flame-retardant polyester fabric is formed by blending flame-retardant polyester fibers, polyester fibers and regenerated cellulose fibers and comprises the following raw materials in parts by weight
2.6 parts of a flame retardant; 77.4 parts of polyester fiber; 20 parts of regenerated cellulose fiber.
The preparation method of the flame-retardant polyester fabric comprises the following steps:
(1) after the flame retardant and the PET slices are blended, extruded and melt spun, the flame retardant and the regenerated cellulose fiber are blended into warp yarns and weft yarns according to the proportion, and the warp yarns and the weft yarns are mutually blended into grey cloth in a right-angle staggered mode;
(2) raising the temperature to 200 ℃, and drying and shaping the grey cloth, wherein the drying speed is 24Y/min; and obtaining the antibacterial polyester fabric.
Comparative example 4
The polyester fabric comprises the following components in parts by weight:
the antistatic polyester fabric is formed by blending antistatic polyester fibers, polyester fibers and regenerated cellulose fibers and comprises the following raw materials in parts by weight
2.6 parts of an antistatic agent; 77.4 parts of polyester fiber; 20 parts of regenerated cellulose fiber.
The preparation method of the antistatic polyester fabric comprises the following steps:
(1) after the antistatic agent is blended with PET slices and extruded for melt spinning, the PET slices and regenerated cellulose fibers are blended into warp yarns and weft yarns according to the proportion, and the warp yarns and the weft yarns are mutually blended into grey cloth by right-angle staggered surfaces;
(2) raising the temperature to 200 ℃, and drying and shaping the grey cloth, wherein the drying speed is 24Y/min; and obtaining the antibacterial polyester fabric.
The physical properties, including antistatic property, antibacterial property and flame retardant property, of the antibacterial polyester fabrics prepared in application examples 1-6 and comparative examples 1-4 of the present invention were measured, respectively, and the results are shown in table 1.
Table 1 physical test properties of the examples
Firstly, as can be seen from table 1, compared with the conventional polyester fabric, the antibacterial polyester fabric of the invention has the advantages that the quaternary phosphonium salt and the quaternary ammonium salt exist in the form of ions, so that the antibacterial polyester fabric is beneficial to the transmission and dispersion of static electricity and has a higher antistatic effect;
secondly, compared with the conventional common polyester fabric, the antibacterial polyester fabric has the advantages of obvious flame retardant property due to the compounding of N, P;
thirdly, compared with the prior common polyester fabric, the antibacterial polyester fabric has better initial antibacterial property and durability due to the synergistic effect of the halamine structure and the quaternary phosphonium salt and the quaternary ammonium salt in the structure.
In sum, compared with the existing antibacterial polyester fabric, the antibacterial polyester fabric disclosed by the invention has obvious advantages in antibacterial property and has efficient flame retardance and antistatic property. The functional structure exists in the terylene fabric in the form of chemical bonds, so the terylene fabric has excellent effect after being washed by water for many times and has excellent function durability. The product has wide market prospect and can be applied to the fields of clothing and the like.
The test method comprises the following steps:
(1) antistatic property: tested with reference to GB/T14342-.
(2) Flame retardancy: the flame retardant effect was observed visually on open fire. Flame retardancy expression method: 5 is optimal and 1 is worst.
(3) The antibacterial performance test of the terylene fabric adopts an AATCC 100-2004 standard method, and the selected strains are gram negative-escherichia coli and gram positive bacteria-staphylococcus aureus. The test specifically comprises the following operation steps: firstly, cutting a test sample into square samples to be tested with the side length of 2.54cm, then inoculating 25 mu L of bacterial suspension with a certain concentration at the center of one square sample to be tested, covering the other square sample to be tested, and pressing the square sample to be tested by using a sterile weight. Culturing at 37 deg.C for 24h in a constant temperature and humidity chamber. After the culture was completed, the number of colonies and the antibacterial ratio were counted.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. The antibacterial polyester fiber is characterized by having a structural formula as follows:
wherein, -R1：-CH3、-C5H9；-R2：-CH3、-C3H7、-C6H13、-C6H5or-C5H9。
2. A preparation method of antibacterial polyester fiber is characterized by comprising the following steps: comprises the following steps:
step (1): coupling reaction to obtain an intermediate product I;
step (2): coupling reaction to obtain an intermediate product II;
and (3): carrying out substitution reaction to obtain an intermediate product III;
and (4): performing polycondensation reaction to obtain polyester with an antibacterial function, namely a target product IV;
and (5): spinning the target product IV into the antibacterial polyester fiber.
3. The preparation method of the antibacterial polyester fiber according to claim 2, characterized in that: the step (1) is specifically as follows:
adding 1mol of hydantoin derivative (A) and 1-1.2mol of 1, 2-dibromoethane (B) into 50mol of organic solvent a, heating to 70-85 ℃, strongly stirring for 1-6h, cooling, standing, and vacuum concentrating; slowly adding 50mol of water, stirring for 30min, adding 80mol of organic solvent b, stirring for 30min, standing for layering, taking an organic phase, drying with anhydrous sodium sulfate, filtering, and performing rotary evaporation to obtain an intermediate product I;
the organic solvent b is ethyl acetate, chloroform or dimethyl sulfoxide.
4. The preparation method of the antibacterial polyester fiber according to claim 2, characterized in that: the step (2) is specifically as follows:
adding 1mol of I and 1-1.2mol of quaternary phosphonium salt (C) into 50mol of organic solvent a, heating to 75-85 ℃, stirring strongly for 4-8h, cooling, standing, rotary evaporating, purifying, and drying to obtain an intermediate product II.
5. The preparation method of the antibacterial polyester fiber according to claim 2, characterized in that: the step (3) is specifically as follows:
under the protection of nitrogen, dissolving 1mol of II, 1-1.2mol of epichlorohydrin (D) and 1-1.2mol of potassium iodide in 50mol of organic solvent a, heating to 85-110 ℃, strongly stirring for 20-28h, cooling, standing, vacuum concentrating, purifying and vacuum drying to obtain an intermediate product III.
6. The preparation method of the antibacterial polyester fiber according to claim 2, characterized in that: the step (4) is specifically as follows:
stirring 1mol of terephthalic acid (E), 0.05-0.1mol of III, 1mol of ethylene glycol (F) and 0.05-1 wt% of catalyst, heating, and filling nitrogen to keep 0.15 MPa; the reaction temperature is controlled at 230 ℃ of 200-; recording the reaction temperature and pressure in the esterification process; the degree of polymerization reaction is judged by observing the current and torque change of a motor, and after the discharging condition is reached, nitrogen is introduced until the pressure is 0.17-0.20MPa, so that a PET product is obtained; opening a discharge valve to allow the melt to flow out of a casting strip head, cooling the casting strip through a cooling water tank, introducing the casting strip into a granulator, and granulating to obtain PET granules, namely a target product IV;
the catalyst is used based on the weight part of terephthalic acid;
the catalyst is 4-dimethylamino pyridine, zinc acetate or antimony trioxide.
7. The preparation method of the antibacterial polyester fiber according to claim 2, characterized in that: the step (5) is specifically as follows:
vacuum drying the PET granules IV at 80 ℃ for 5h, and vacuum drying at 120 ℃ for 24 h; stirring at a high speed, uniformly mixing, putting into a double-screw extruder, performing melt extrusion to obtain a melt, outputting the melt into a spinning machine for spinning, drafting and cooling to obtain fibers, forming the fibers into a net by a net former, conveying the net-formed fibers into a hot rolling machine, and performing hot rolling at 90-95 ℃ and 3.2-3.7MPa to obtain antibacterial polyester fibers;
the diameter of a screw of the double-screw extruder is 18-22mm, and the length-diameter ratio of the screw is 22;
the spinning temperature was 200 ℃.
8. The method for preparing antibacterial polyester fiber according to claims 3, 4 and 5, characterized in that: the organic solvent a is N, N-dimethylformamide or dimethyl sulfoxide.
9. The utility model provides an antibiotic polyester fabric, is formed by antibiotic polyester fiber, polyester fiber and the blending of regenerated cellulose base fibre which characterized in that: comprises the following raw materials in parts by weight
20-40 parts of antibacterial polyester fiber;
40-60 parts of polyester fiber;
15-25 parts of regenerated cellulose fiber.
10. The antibacterial polyester fabric according to claim 9, characterized in that: the preparation steps are as follows:
(1) the antibacterial polyester fiber, the polyester fiber and the regenerated cellulose fiber are blended into warp yarn and weft yarn according to a proportion, and the warp yarn and the weft yarn are mutually blended into grey cloth by right-angle staggered surfaces;
(2) raising the temperature to 200 ℃, and drying and shaping the grey cloth, wherein the drying speed is in the range of 24Y/min to 26Y/min; and obtaining the antibacterial polyester fabric.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010204688.0A CN111364115A (en) | 2020-03-22 | 2020-03-22 | Antibacterial polyester fiber and fabric |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010204688.0A CN111364115A (en) | 2020-03-22 | 2020-03-22 | Antibacterial polyester fiber and fabric |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111364115A true CN111364115A (en) | 2020-07-03 |
Family
ID=71205812
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010204688.0A Withdrawn CN111364115A (en) | 2020-03-22 | 2020-03-22 | Antibacterial polyester fiber and fabric |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111364115A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111728837A (en) * | 2020-07-22 | 2020-10-02 | 万贤能 | A kind of sports massage belt capable of rubbing abdomen and chest and throwing butterfly sleeves and preparation method thereof |
| CN117431680A (en) * | 2023-11-27 | 2024-01-23 | 潮州市苏菲亚时装有限公司 | A kind of preparation method of light and breathable fabric |
| CN118489679A (en) * | 2024-05-27 | 2024-08-16 | 胜利油田海发环保化工有限责任公司 | High-penetration broad-spectrum fungicide for offshore oil fields and preparation method thereof |
-
2020
- 2020-03-22 CN CN202010204688.0A patent/CN111364115A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111728837A (en) * | 2020-07-22 | 2020-10-02 | 万贤能 | A kind of sports massage belt capable of rubbing abdomen and chest and throwing butterfly sleeves and preparation method thereof |
| CN117431680A (en) * | 2023-11-27 | 2024-01-23 | 潮州市苏菲亚时装有限公司 | A kind of preparation method of light and breathable fabric |
| CN118489679A (en) * | 2024-05-27 | 2024-08-16 | 胜利油田海发环保化工有限责任公司 | High-penetration broad-spectrum fungicide for offshore oil fields and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111364115A (en) | Antibacterial polyester fiber and fabric | |
| CN102747450B (en) | Production method of chitin antibacterial mouldproof polypropylene BCF (bulk continuous filament) filament | |
| CN112981707A (en) | Preparation method of antibacterial, antiviral and mildewproof polyester spunlace nonwoven fabric containing PHBV material | |
| CN118109955A (en) | Efficient antibacterial polyester fabric and preparation method thereof | |
| CN112144293B (en) | High-barrier antibacterial barrier coating for non-woven fabric and preparation method thereof | |
| CN106987944A (en) | Sun-proof anti-bacterial fibre mixed yarn | |
| CN113981563A (en) | Antibacterial polyester high stretch yarn and preparation method thereof | |
| CN113584725A (en) | Preparation process of PHBV and PLA biodegradable antibacterial deodorizing spunbonded nonwoven fabric | |
| CN105239204A (en) | Novel polylactic acid fiber fabric | |
| CN113122957A (en) | Preparation method of antibacterial and antiviral polyester filament containing PHBV material | |
| CN115679547B (en) | Antibacterial non-woven fabric for preparing protective clothing | |
| CN116240645A (en) | Regenerated polyamide fiber and method for producing same | |
| CN111345649A (en) | Blanket for infant care and preparation method thereof | |
| CN112160049A (en) | Sun-proof antibacterial textile fabric and preparation method thereof | |
| CN1180140C (en) | Making process of polypropylene fiber with mosquito repelling function | |
| CN110983469A (en) | Polylactic acid BCF bulked yarn, and preparation method and application thereof | |
| CN112609294A (en) | Environment-friendly antibacterial and anti-mite fiber fabric for home textiles | |
| CN104805521B (en) | Preparation method of polyester fiber with antibacterial function | |
| CN112981610A (en) | Environment-friendly hydrophilic low-melting-point PET composite short fiber and preparation method thereof | |
| CN119686110A (en) | Negative ion antibacterial polyester fiber composite fabric and production process thereof | |
| CN110144650B (en) | Multifunctional pearl polylactic acid blended yarn and preparation method thereof | |
| CN118422397A (en) | Polyester yarn and preparation method thereof | |
| CN1468983A (en) | Polypropylene fiber with mosquito repelling function | |
| CN106012098A (en) | Preparing method of high-water-absorption antibacterial acrylic fiber | |
| CN1468984A (en) | Making process of polypropylene fiber with mosquito repelling function |
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 | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200703 |