CN113463221A - POY sea-island fiber and preparation method thereof - Google Patents
POY sea-island fiber and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 58
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 31
- 229920000728 polyester Polymers 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 22
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 20
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 20
- 238000005507 spraying Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 238000001125 extrusion Methods 0.000 claims abstract description 4
- 238000004804 winding Methods 0.000 claims abstract description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims abstract description 3
- 239000007822 coupling agent Substances 0.000 claims description 21
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 20
- 239000002671 adjuvant Substances 0.000 claims description 20
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000005751 Copper oxide Substances 0.000 claims description 4
- 229910000431 copper oxide Inorganic materials 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000004599 antimicrobial Substances 0.000 claims 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 42
- 238000012360 testing method Methods 0.000 description 35
- 239000012071 phase Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 13
- 238000005406 washing Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 10
- 229920001817 Agar Polymers 0.000 description 7
- 239000008272 agar Substances 0.000 description 7
- 230000003385 bacteriostatic effect Effects 0.000 description 7
- 239000002609 medium Substances 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 description 4
- 229920002101 Chitin Polymers 0.000 description 3
- 241001122767 Theaceae Species 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 239000012074 organic phase Substances 0.000 description 3
- 150000008442 polyphenolic compounds Chemical class 0.000 description 3
- 235000013824 polyphenols Nutrition 0.000 description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 3
- FMNZBNCPTJEVDS-KVVVOXFISA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol;(z)-octadec-9-enoic acid Chemical compound CCC(CO)(CO)CO.CCCCCCCC\C=C/CCCCCCCC(O)=O FMNZBNCPTJEVDS-KVVVOXFISA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- 238000009499 grossing Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000011177 media preparation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000008041 oiling agent Substances 0.000 description 1
- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011218 seed culture Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance 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
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The application relates to the technical field of sea-island fibers, and particularly discloses a POY (polyester pre-oriented yarn) sea-island fiber and a preparation method thereof. The preparation method comprises the following steps: s1: pretreatment of raw materials: pre-crystallizing and drying polyethylene terephthalate and alkali-soluble polyester; s2: melt extrusion: respectively extruding polyethylene terephthalate and alkali-soluble polyester; s3: spinning: spinning polyethylene glycol terephthalate and alkali-soluble polyester by a composite spinning method to obtain POY sea-island protofilaments; s4: cooling and forming; s5: auxiliary agent spraying: uniformly spraying an auxiliary agent on the outer surface of the POY sea island precursor, wherein 100-200g of the auxiliary agent is correspondingly used for every 100tex of the POY sea island precursor; s6: bundling and oiling; s7: winding: obtaining POY sea-island fiber; the auxiliary agent comprises the following components in parts by weight: 100 parts of water; 2-6 parts of sodium hydroxide; 0.5-2.5 parts of antibacterial agent. The preparation method has the advantage of improving the antibacterial effect of the sea-island fiber.
Description
Technical Field
The application relates to the technical field of sea-island fibers, in particular to a POY (polyester pre-oriented yarn) sea-island fiber and a preparation method thereof.
Background
Sea-island fibers are formed by embedding one polymer in a very fine form (island phase) in another polymer (sea phase); the method is mainly obtained by two methods: the first is a composite spinning method, two polymers are melt-spun through a special spinning nozzle assembly, and island components are regularly distributed in sea components; the other is a blending spinning method, two polymers are blended and spun, and island components are randomly distributed in sea components.
The POY sea-island fiber commonly available in the market is obtained by a composite spinning method by taking polyethylene terephthalate (PET) as an island phase and alkali-soluble polyester (COPET) as a sea phase. For the antibacterial treatment of the fiber in the related technology, the antibacterial agent is generally mixed in the spinning raw material, but for the sea-island fiber, on one hand, the island phase is embedded in the sea phase, the sea phase accounts for 10-30% of the total weight, the sea phase proportion is small, and the antibacterial particles hardly have good antibacterial effect in the island phase or the sea phase.
Disclosure of Invention
In order to improve the antibacterial effect of the sea-island fiber, the present application provides a POY sea-island fiber and a preparation method thereof.
In a first aspect, the present application provides the following technical solutions: a preparation method of POY sea-island fiber comprises the following steps:
s1: pretreatment of raw materials: pre-crystallizing and drying polyethylene terephthalate and alkali-soluble polyester;
s2: melt extrusion: respectively extruding polyethylene terephthalate and alkali-soluble polyester;
s3: spinning: spinning polyethylene glycol terephthalate and alkali-soluble polyester by a composite spinning method to obtain POY sea-island protofilaments;
s4: cooling and forming;
s5: auxiliary agent spraying: uniformly spraying an auxiliary agent on the outer surface of the POY sea island precursor, wherein 100-200g of the auxiliary agent is correspondingly used for every 100tex of the POY sea island precursor;
s6: bundling and oiling: bundling, oiling on the outer surface of the bundled fiber;
s7: winding: obtaining POY sea-island fiber;
the auxiliary agent comprises the following components in parts by weight:
100 parts of water;
2-6 parts of sodium hydroxide;
0.5-2.5 parts of antibacterial agent.
By adopting the technical scheme, after the POY sea-island fiber is obtained, the oil is applied through the auxiliary agent; attaching the antibacterial agent to the outer surface of sea to obtain the POY sea-island fiber with antibacterial effect. It is found from the test that the POY sea-island fiber obtained in this manner has a higher antibacterial effect than a POY sea-island fiber obtained by mixing the sea phase or island phase raw material with the same amount of the antibacterial agent.
Further, when the step S5 is performed, the temperature of the POY sea island filament is controlled at 103-130 ℃.
By adopting the technical scheme, experiments show that the antibacterial effect can be further improved.
Further, the adjuvant also comprises 0.05-0.2 part of coupling agent, and the antibacterial agent is an inorganic antibacterial agent.
By adopting the technical scheme, the coupling agent can connect an inorganic phase and an organic phase, the adhesive strength of the antibacterial agent outside the POY sea island protofilament can be improved, and tests show that the antibacterial effect and the water washing resistance can be further improved. On the other hand, the antibacterial agent and the POY sea-island precursor are connected by the coupling agent under the condition that the POY sea-island precursor is partially dissolved, so that the adhesion effect rate of the antibacterial agent can be improved, and the antibacterial effect is improved.
Further, the adjuvant also comprises 5-10 parts of polyvinyl alcohol.
By adopting the technical scheme, the polyvinyl alcohol has water solubility, film forming property and adhesiveness. As is clear from the test, the antibacterial effect can be further improved.
Further, the auxiliary agent comprises the following components in parts by weight:
100 parts of water;
2-2.5 parts of sodium hydroxide;
2-2.2 parts of inorganic antibacterial agent;
0.1-0.2 part of coupling agent;
6-8 parts of polyvinyl alcohol;
and is prepared by the following steps:
z1: dissolving sodium hydroxide in water, adding polyvinyl alcohol, and heating to 90-100 deg.C until the solution is completely dissolved;
z2: cooling to 20-60 deg.C, adding coupling agent and inorganic antibacterial agent, and mixing to obtain adjuvant.
By adopting the technical scheme, the auxiliary agents of the components in the compounding range are optimized, and tests show that the obtained POY sea island protofilament has better antibacterial effect. Further, the inorganic antibacterial agent comprises at least two of a nano silver ion antibacterial agent, nano zinc oxide and nano copper oxide.
By adopting the technical scheme, the small-particle antibacterial agent is adopted, so that the antibacterial agent is conveniently attached to the outer surface of the fiber, the particle feeling and the caking possibility are reduced, and the appearance performance of the POY sea-island fiber is improved.
Further, in the step S5, after spraying the auxiliary agent, an ethanol aqueous solution with a mass fraction of 60 to 75% is sprayed.
By adopting the technical scheme, the volatilization of water is accelerated by utilizing ethanol, so that the effect of instantaneous dissolution and instantaneous adsorption is achieved, the dissolution time of the outer surface of the POY sea-island fiber is reduced on one hand, and the preparation efficiency is improved on the other hand.
In a second aspect, the present application provides the following technical solutions: POY sea-island fiber obtained by the process according to any one of claims 1 to 7.
By adopting the technical scheme, the POY sea-island fiber with excellent antibacterial effect is obtained.
In summary, the present application has the following beneficial effects:
1. the auxiliary agent is sprayed after cooling and forming, bundling and oiling are carried out, and the antibacterial agent is attached to the surface of the POY sea-island fiber, so that the antibacterial agent has an excellent antibacterial effect.
2. Since the coupling agent is used as a part of the adjuvant, the antibacterial effect and the water resistance can be further improved.
3. According to the preparation method, the polyvinyl alcohol, the coupling agent and the antibacterial agent are used as part of the auxiliary agent, and the preparation method of the auxiliary agent is matched, so that the inorganic antibacterial agent, the coupling agent and the polyvinyl alcohol have better connectivity, the possibility that effective components are possibly taken away by moisture is reduced, and the attachment rate of the antibacterial agent is further improved.
Detailed Description
Examples
Example 1: a preparation method of POY sea-island fiber comprises the following steps:
s1: pretreatment of raw materials:
polyethylene terephthalate (PET): putting PET into an incubator, pre-crystallizing at 165 ℃ for 30min, then putting into a drying oven, and drying at 165 ℃ for 4h to obtain dried PET;
alkali soluble polyester in (COPET): putting COPET into a heat preservation box, pre-crystallizing at 135 ℃ for 35min, then putting into a drying box, and drying at 165 ℃ for 4h to obtain dried COPET;
s2: melt extrusion:
PET: extruding the dried PET in an extruder, wherein the heating section temperature is 265 ℃, 275 ℃, 285 ℃ and 293 ℃ respectively;
COPET: extruding the dried COPET in an extruder, wherein the heating section temperatures are 230 ℃, 240 ℃, 280 ℃ and 285 ℃ respectively;
s3: spinning: enabling the molten PET and the molten COPET to pass through a metering pump, wherein the spinning dosage ratio of the PET to the COPET at the same time is 80: 20; the melted PET and COPET respectively enter two spinning boxes, and the spinning speed is 3000 m/min;
then introducing the raw materials in the spinning manifold into the composite assembly for spinning, wherein the number of island phase fibers is 36; the PET spinning temperature is 293 ℃, the COPET spinning temperature is 285 ℃ to obtain POY sea island precursor;
s4: and (3) cooling and forming: cooling by adopting cross air blow with the temperature of 22 +/-2 ℃ and the air speed of 0.3m/s until the fiber temperature is 150 ℃;
s5: auxiliary agent spraying: enabling the cooled POY sea island precursor to pass through an annular sprayer, enabling a nozzle to face the interior of the annular sprayer, and uniformly spraying an auxiliary agent on the outer surface of the POY sea island precursor, wherein 100g of the auxiliary agent is correspondingly used for every 100tex of the POY sea island precursor;
the components, compositions and qualities of the adjuvants are shown in table 1.1 and are obtained by the following preparation method: adding adjuvant raw materials into a stirrer, stirring at 95 deg.C and 80r/min for 20min, cooling to 40 deg.C, and dispersing at 1000r/min for 3min to obtain adjuvant;
s6: bundling and oiling: bundling by a bundling device, and oiling by using an oiling agent through an oil nozzle, wherein the oiling rate is 0.35%; the beam-focusing point is at 1000 m; the oil agent consists of 40kg of smoothing agent, 25kg of emulsifying agent and 1kg of bundling agent; wherein the smoothing agent consists of 25kg of white oil and 15kg of trimethylolpropane oleate; the emulsifier consists of 10kg of castor oil polyoxyethylene ether and 15kg of fatty alcohol polyoxyethylene ether; the bundling agent is glycerol;
s7: winding: POY sea-island fiber is obtained.
In the above embodiment, the industrial white oil was purchased from Nanjing Rongji chemical Co., Ltd, model 7 #; trimethylolpropane oleate was purchased from Wuhankangqiong biomedical science and technology Limited.
Castor oil polyoxyethylene ether is purchased from Jinan Hui Chuan chemical Co., Ltd., model EL-80, and fatty alcohol polyoxyethylene ether is purchased from Jinan Shuang Chen environmental protection technology Co., Ltd., model AEO-9.
Example 2: a method for preparing a POY sea-island fiber, which is different from example 1 in that:
in S4, the fiber was cooled to a temperature of 140 ℃.
In S5, 180g of auxiliary agent is used for every 100tex POY sea island protofilament; the components, compositions and masses of the adjuvants are referred to in table 1.1.
Example 3: a method for preparing a POY sea-island fiber, which is different from example 1 in that:
in S4, the fiber was cooled to a temperature of 200 ℃.
In S5, 200g of auxiliary agent is used for every 100tex POY sea island protofilament; the components, compositions and masses of the adjuvants are referred to in table 1.1.
Example 4: a method for preparing a POY sea-island fiber, which is different from example 2 in that: in S4, the fiber was cooled to a fiber temperature of 103 ℃.
Example 5: a method for preparing a POY sea-island fiber, which is different from example 2 in that: in S4, the fiber was cooled to a fiber temperature of 121 ℃.
Example 6: a method for preparing a POY sea-island fiber, which is different from example 2 in that: in S4, the fiber was cooled to a temperature of 130 ℃.
Examples 7 to 10: a method for preparing a POY sea-island fiber, which is different from example 5 in that: the components, compositions and masses of the adjuvants are referred to in table 1.1.
Example 11: a method for preparing a POY sea-island fiber, which is different from example 5 in that: the components, compositions and masses of the adjuvants are referred to in table 1.2.
Example 12: a method for preparing a POY sea-island fiber, which is different from example 11 in that:
the auxiliary agent is obtained by the following preparation method:
z1: putting sodium hydroxide and water into a stirrer, stirring at 25 +/-2 ℃ and 30r/min for 10min to completely dissolve, putting polyvinyl alcohol into the stirrer, heating to 90 ℃, and stirring at 80r/min for 15 min;
z2: and (4) cooling the mixed solution obtained in the step Z1 to 20 ℃, adding the coupling agent and the antibacterial agent, and stirring for 3min at a stirring speed of 1000r/min to obtain the auxiliary agent.
Examples 13 to 15: a method for preparing a POY sea-island fiber, which is different from example 5 in that: the components, compositions and masses of the adjuvants are referred to in table 1.2.
And the auxiliary agent is obtained by the following preparation method:
z1: putting sodium hydroxide and water into a stirrer, stirring at the stirring speed of 30r/min at the temperature of 25 +/-2 ℃ for 10min to completely dissolve, then putting polyvinyl alcohol into the stirrer, heating to 100 ℃, and stirring at the stirring speed of 50r/min for 10 min;
z2: and (4) cooling the mixed solution obtained in the step Z1 to 60 ℃, adding the coupling agent and the antibacterial agent, and stirring for 3min at the stirring speed of 800r/min to obtain the auxiliary agent.
Example 16: a method for preparing a POY sea-island fiber, which is different from example 15 in that:
s5: auxiliary agent spraying: and uniformly spraying an auxiliary agent on the outer surface of the cooled POY sea island precursor, and spraying an ethanol water solution with the mass fraction of 60% on the outer surface of the POY sea island precursor.
Example 17: a method for preparing a POY sea-island fiber, which is different from example 15 in that:
s5: auxiliary agent spraying: after the auxiliary agent is uniformly sprayed on the outer surface of the cooled POY sea island precursor, an ethanol aqueous solution with the mass fraction of 75% is sprayed on the outer surface of the POY sea island precursor through an annular spray head (the nozzle faces the inside of the ring).
TABLE 1.1 examples 1-3, 7-10 adjuvant compositions, compositions and masses (kg)
TABLE 1.2 examples 11-15 adjuvant compositions, compositions and masses (kg)
In the above examples, the organosilicon quaternary ammonium salt was purchased from the armoring mildew-proof antibacterial science and technology limited, Huizhou, model KS 116; chitin was purchased from Zhengzhou Futai chemical products Co., Ltd; tea polyphenols are purchased from north Heibo Kelong Biotech limited; zinc oxide was purchased from Jingxian Longyuan chemical Co., Ltd; copper oxide was purchased from the industrial upgrading industries, ltd, wuhan gig.
The nano copper oxide is purchased from Hangzhou Hengge nano technology GmbH, and has a particle size of 20-30 nm; the nano zinc oxide is purchased from Shanghai Xiao Huan nano science and technology Limited company, and has an average particle size of 30 nm; the nano silver ion antibacterial agent is purchased from Lanfeng auxiliary agent Co., Ltd.
The polyvinyl alcohol designation is 1788.
Comparative example
Comparative example 1: a method for preparing a POY sea-island fiber, which is different from example 1 in that the auxiliary agent does not contain sodium hydroxide.
Comparative example 2: a method for preparing POY sea-island fiber, which is different from the embodiment 1, is that in the step S2, PET and antibacterial agent are mixed and extruded, and 2.4g of antibacterial agent (0.96g of chitin, 0.96g of organosilicon quaternary ammonium salt and 0.48g of tea polyphenol) is added for every 100 tex.
Comparative example 3: a method for preparing POY sea-island fiber, which is different from the embodiment 1, is that in the step S2, COPET and antibacterial agent are mixed and extruded, and every 100tex corresponds to 2.4g of antibacterial agent (0.96g chitin, 0.96g organosilicon quaternary ammonium salt and 0.48g tea polyphenol).
Characterization test:
1. test for antibacterial Effect
Test subjects: POY islands-in-the-sea fibers prepared in examples 1-17 and comparative examples 1-3 were designated as examples 1-17 and comparative examples 1-2, and a blank set, for a total of 21 test samples.
The test method comprises the following steps: from the middle section of each test sample, a 10cm long fiber was taken. The blank group is the fiber obtained in example 1 except for step S5.
Staphylococcus aureus was selected as the test bacterium. The lower sterile medium was prepared first. 10mL of agar medium was poured into a sterile plate and allowed to clot. Then, the upper layer of the seed culture medium is prepared. 150mL of agar medium at 45 +/-2 ℃ is put into a flask, and 1mL of test bacterium liquid is added. The flasks were shaken to homogenize the bacteria, and 5mL of each plate was poured and allowed to coagulate. The inoculated agar culture medium is used within 1 h. The test samples were rounded end to end with sterile forceps and placed in the center of the plane and pressed evenly against the agar medium with sterile forceps until there was good contact between the test sample and the agar medium. Immediately after placing the test sample on the agar medium, the sample was placed in an incubator at 37 ℃. + -. 2 ℃ for 20 hours, ensuring that the sample and the agar medium remained in contact throughout the incubation period.
And measuring the middle section of each test sample, and calculating the ratio of the width of the out-of-circle bacteriostatic belt surrounded by the polyester yarns of the test sample to the width of the in-circle bacteriostatic belt surrounded by the polyester yarns to the diameter of the circle surrounded by the polyester yarns according to the following formula. And calculating the ratio of the width of the out-of-circle bacteriostatic strip surrounded by the polyester yarns of the parallel sample to the width of the in-circle bacteriostatic strip surrounded by the polyester yarns to the diameter of the circle surrounded by the polyester yarns according to the following formula.
H1＝(D1-d)/d*％；H2＝(D2-d)/d*％；
In the formula:
d, the diameter of a circle formed by the polyester yarn in millimeter (mm);
d1-the outer diameter of the circular outer antibacterial belt formed by the polyester yarns, and the unit is millimeter (mm);
d2-the outer diameter of the antibacterial belt in a circle formed by the polyester yarns, and the unit is millimeter (mm);
h1, the proportion of the width of the outer circle bacteriostatic zone surrounded by the polyester yarns to the diameter of the circle surrounded by the polyester yarns is in millimeter (mm);
h2, the ratio of the width of the bacteriostatic zone in the circle formed by the polyester yarns to the diameter of the circle formed by the polyester yarns is in millimeter (mm).
And (3) test results: the results of the antimicrobial efficacy tests are reported in table 2.
TABLE 2 antibacterial effectiveness test results
And (3) data analysis: the larger the inhibition zone is, the better the antibacterial effect is. Both the working and comparative samples showed antibacterial effects compared to the blank group. As is clear from the data in Table 2, the antibacterial effects were found to be good in the order of example 16-17, example 11-15, example 9-10, example 7-8, example 4-6, example 1-3 and comparative example 1-3.
Comparing the implementation sample 1 with the comparison samples 1-3, wherein the comparison sample 1 does not sample sodium hydroxide, the auxiliary agent is equivalent to an antibacterial agent and is directly sprayed on the outer surface of the POY sea island protofilament, the antibacterial agent is easily taken away by water, and the adhesive force is poor, so that the final antibacterial effect is poor. The comparison sample 2 is prepared by mixing the antibacterial agent into the PET raw material, and the comparison sample 3 is prepared by mixing the antibacterial agent into COPET to respectively prepare an island phase and a sea phase with the antibacterial agent; since the antibacterial agent is buried in the sea-island fiber, the antibacterial effect is hardly exhibited, and the comparative sample 3 in which the antibacterial agent is provided in the sea phase closer to the outer surface of the fiber has a better antibacterial effect than the comparative sample 2.
In example 1, the antibacterial agent is attached to the outer surface of the POY sea island precursor by the auxiliary agent, so that a good antibacterial effect is obtained, which may be caused by: since the sea phase is alkali soluble polyester, after POY sea island precursor is obtained, the alkali auxiliary agent is sprayed on the surface of the POY sea island precursor, and partial outer surface of the POY sea island precursor is dissolved, so that the antibacterial agent is attached. When the auxiliary agent is sprayed, the sea island protofilament has a certain temperature, water can be evaporated, on one hand, the alkalinity is improved to realize the dissolution of the outer surface, on the other hand, the possibility of the water flowing on the fiber surface is reduced, the loss of the antibacterial agent and sodium hydroxide is reduced, the dissolution of the outer surface of the sea island protofilament and the adhesion of the antibacterial agent are ensured, and the antibacterial effect is realized. Compared with the comparative example, the antibacterial agent is more beneficial to the effect of the antibacterial agent because the antibacterial agent is attached to the surface of the sea island protofilament.
Examples 4 to 6 define the temperature of the sea island precursor before the auxiliary agent is sprayed on the basis of example 2, and the bacteriostatic effect is improved by a small margin. The reasons may be: at the moment, the water evaporation speed and the concentration change of the sodium hydroxide reach balance, and the adhesion rate of the antibacterial agent in the auxiliary agent can be further improved, so that the antibacterial effect is improved.
Examples 7 to 8 were prepared by adding a coupling agent to example 5, and the antibacterial effect was further improved. The coupling agent can connect an inorganic phase and an organic phase, and can improve the adhesion strength of the antibacterial agent outside the POY sea island protofilament; on the other hand, the antibacterial agent and the POY sea-island precursor are connected by the coupling agent under the condition that the POY sea-island precursor is partially dissolved, so that the adhesion effect rate of the antibacterial agent can be improved, and the antibacterial effect is improved.
In examples 9 to 10, the use of polyvinyl alcohol was added to example 8, and the antibacterial effect was further improved. The reasons may be: in the process of water evaporation, the fluidity of the polyvinyl alcohol is gradually reduced, and the adhesiveness is improved, so that the effect of adhering the antibacterial agent to the outer surface of the POY is achieved.
Examples 11 to 13 the amounts of the respective components in the adjuvant were limited based on example 10, and the antibacterial effect was further improved. In addition, examples 12-13 further define a method for preparing the adjuvant, and the antibacterial effect can be further improved by mixing the polyvinyl alcohol with sodium hydroxide and water, and then uniformly mixing the polyvinyl alcohol with the antibacterial agent and the coupling agent, as compared with example 11. The reasons may be: the coupling agent and the inorganic antibacterial agent are put into the polyvinyl alcohol alkaline water and dissolved, so that the inorganic antibacterial agent, the coupling agent and the polyvinyl alcohol three phases have better connectivity, the possibility that the effective components are possibly taken away by water is reduced, and the attachment rate of the antibacterial agent is further improved.
In examples 16 to 17, the use of ethanol was added to example 15, and the antibacterial effect was improved to a small extent. The ethanol is utilized to accelerate the volatilization of water, so that the effect of instantaneous dissolution and instantaneous adsorption is achieved, the dissolution time of the outer surface of the POY sea-island fiber is reduced, the adhesion efficiency is improved, and the preparation efficiency is improved.
2. Water washing resistance test
Test subjects: example 5, examples 7-10 and blank groups for a total of 6 test samples.
The test method comprises the following steps: from the middle section of each test sample, 10cm long polyester yarn was cut.
Staphylococcus aureus was selected as the test bacterium. The culture medium preparation was the same as in test "1, antibacterial effect test".
The measurement point of each test sample is the midpoint in the length direction thereof, and H1 before water washing was calculated in the manner of calculation in test "1, antibacterial effect test". And then, carrying out water washing on the test sample for 3 times, carrying out the antibacterial effect test again, recording H1 after water washing, and calculating the difference value between H1 before water washing and H1 after water washing.
And (3) water washing operation: heating 50kg of water to 35 ℃, adding 80g of the bluish moon-brightening laundry detergent (natural faint scent), and uniformly mixing to obtain the water washing liquid. And (3) soaking the test sample in a water washing solution for 30h, taking out and naturally drying.
And (3) test results: the water wash resistance test results are reported in table 3.
TABLE 3 Water resistance test results
And (3) data analysis: as is clear from the data in Table 3, the antibacterial effect stability after washing was from good to poor in the order of example 9-10, example 7-8, example 5 and comparative example 1.
Compared with the comparative sample 1, the embodiment 5 adopts sodium hydroxide, so that the outer surface of the POY sea-island fiber is partially dissolved, the antibacterial agent is attached to the outer surface of the fiber, and after the water is dried, the COPET is recrystallized and attached with the antibacterial agent, so that better washing resistance is obtained.
In examples 7 to 8, the use of a coupling agent was added to example 5, and the water resistance of the antibacterial effect was improved. The coupling agent can connect inorganic phase and organic phase, and can improve the adhesion strength of the antibacterial agent outside the POY sea island protofilament, thereby reducing the possibility that the antibacterial component is washed away.
In examples 9 to 10, the use of polyvinyl alcohol was further increased in addition to example 8, and the water resistance of the antibacterial effect was further improved. The reasons may be: the film forming property and the adhesiveness of the polyvinyl alcohol improve the adhesiveness of the antibacterial agent on the surface of the sea-island fiber.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. A preparation method of POY sea-island fiber is characterized by comprising the following steps:
s1: pretreatment of raw materials: pre-crystallizing and drying polyethylene terephthalate and alkali-soluble polyester;
s2: melt extrusion: respectively extruding polyethylene terephthalate and alkali-soluble polyester;
s3: spinning: spinning polyethylene glycol terephthalate and alkali-soluble polyester by a composite spinning method to obtain POY sea-island protofilaments;
s4: cooling and forming;
s5: auxiliary agent spraying: uniformly spraying an auxiliary agent on the outer surface of the POY sea island precursor, wherein 100-200g of the auxiliary agent is correspondingly used for every 100tex of the POY sea island precursor;
s6: bundling and oiling;
s7: winding: obtaining POY sea-island fiber;
the auxiliary agent comprises the following components in parts by weight:
100 parts of water;
2-6 parts of sodium hydroxide;
0.5-2.5 parts of antibacterial agent.
2. The method as claimed in claim 1, wherein the POY island fiber is prepared by controlling the temperature of the POY island fiber at 103-130 ℃ while the step S5 is performed.
3. The method of claim 1 or 2, wherein the adjuvant further comprises 0.05-0.2 parts of a coupling agent, and the antimicrobial agent is an inorganic antimicrobial agent.
4. The method of claim 3, wherein the adjuvant further comprises 5-10 parts of polyvinyl alcohol.
5. The method of claim 4, wherein the adjuvant comprises the following components in parts by weight:
100 parts of water;
2-2.5 parts of sodium hydroxide;
2-2.2 parts of inorganic antibacterial agent;
0.1-0.2 part of coupling agent;
6-8 parts of polyvinyl alcohol;
and is prepared by the following steps:
z1: dissolving sodium hydroxide in water, adding polyvinyl alcohol, and heating to 90-100 deg.C until the solution is completely dissolved;
z2: cooling to 20-60 deg.C, adding coupling agent and inorganic antibacterial agent, and mixing to obtain adjuvant.
6. The method of claim 4, wherein the inorganic antimicrobial agent comprises at least two of nano silver ion antimicrobial agent, nano zinc oxide, and nano copper oxide.
7. The method of claim 1, wherein the step S5, after spraying the auxiliary agent, is spraying an ethanol aqueous solution with a mass fraction of 60-75%.
8. POY sea-island fiber obtained by the production process according to any one of claims 1 to 7.
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| CN114318589A (en) * | 2022-02-25 | 2022-04-12 | 杭州惠丰化纤有限公司 | High-flame-retardant superfine sea island filament and preparation process thereof |
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Application publication date: 20211001 |