CN111733480A - Sea-island fiber with PA6 as island component, preparation method thereof and superfine fiber formed by same - Google Patents
Sea-island fiber with PA6 as island component, preparation method thereof and superfine fiber formed by same Download PDFInfo
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- CN111733480A CN111733480A CN202010644747.6A CN202010644747A CN111733480A CN 111733480 A CN111733480 A CN 111733480A CN 202010644747 A CN202010644747 A CN 202010644747A CN 111733480 A CN111733480 A CN 111733480A
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- sea
- island
- fiber
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- modified copolyester
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- 239000000835 fiber Substances 0.000 title claims abstract description 128
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 229920001634 Copolyester Polymers 0.000 claims abstract description 46
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 28
- 238000009987 spinning Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000002131 composite material Substances 0.000 claims description 24
- 239000000155 melt Substances 0.000 claims description 22
- 238000001125 extrusion Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 229910052700 potassium Inorganic materials 0.000 claims description 10
- 239000011591 potassium Substances 0.000 claims description 10
- 239000011734 sodium Chemical group 0.000 claims description 10
- 229910052708 sodium Chemical group 0.000 claims description 10
- 230000008961 swelling Effects 0.000 claims description 10
- 239000006184 cosolvent Substances 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 5
- 229920001410 Microfiber Polymers 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000009998 heat setting Methods 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004804 winding Methods 0.000 claims description 2
- 238000002788 crimping Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 14
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 22
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 9
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- QWGRWMMWNDWRQN-UHFFFAOYSA-N 2-methylpropane-1,3-diol Chemical compound OCC(C)CO QWGRWMMWNDWRQN-UHFFFAOYSA-N 0.000 description 7
- 239000003513 alkali Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000005886 esterification reaction Methods 0.000 description 6
- 150000002148 esters Chemical group 0.000 description 6
- 239000012760 heat stabilizer Substances 0.000 description 6
- 238000006068 polycondensation reaction Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 5
- 229940035437 1,3-propanediol Drugs 0.000 description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 5
- 229920001684 low density polyethylene Polymers 0.000 description 5
- 239000004702 low-density polyethylene Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical group O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000011045 prefiltration Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000000237 capillary viscometry Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical group COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical group C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 description 1
- 229920003081 Povidone K 30 Polymers 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical group OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- VIQSRHWJEKERKR-UHFFFAOYSA-L disodium;terephthalate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=C(C([O-])=O)C=C1 VIQSRHWJEKERKR-UHFFFAOYSA-L 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 230000004580 weight loss Effects 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
-
- 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
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
- C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6886—Dicarboxylic acids and dihydroxy compounds
-
- 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
- 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
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Multicomponent Fibers (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention provides a sea-island fiber with PA6 as an island component, a preparation method thereof and a superfine fiber formed by the same, wherein the sea-island fiber with PA6 as the island component uses modified copolyester as a sea component. The modified copolyester is adopted as the sea material of the sea-island fiber, and the PA6 is adopted as the island material, so that the formed sea-island fiber has good spinnability, and the sea-island fiber can be opened under very mild conditions due to the characteristics of the modified copolyester, and the physicochemical property of the island component PA6 cannot be influenced by the mild opening condition, so that the property of the PA6 superfine fiber formed by the island component is not damaged.
Description
Technical Field
The invention relates to the technical field of superfine fibers, in particular to a sea-island fiber taking PA6 as an island component and a preparation method thereof.
Background
Sea-island fibers are fibers in which one polymer is dispersed in another polymer, the dispersed phase being in the form of "islands" in the cross section of the fiber, and the matrix corresponding to "sea" in which one component is surrounded by another component in a finely dispersed state as viewed in the cross section of the fiber, as if there were many islands in the sea.
The sea-island fiber is prepared through melt spinning 2 kinds of fiber forming polymer as island component and sea component in different compounding ratio, and the superfine fiber is prepared through eliminating sea component and leaving island component with the solubility or decomposition of the 2 kinds of components in some chemical solvent. The sea-island fiber is classified into a hydrolysis-peeling type (alkali weight reduction method), a solvent-dissolving type (benzene weight reduction method), and a hot-water dissolving type (hot-water dissolving method) according to the type of sea-phase polymer and the opening process.
The hydrolysis stripping type (alkali reduction method) adopts alkali soluble polyester (COPET) as a sea component of sea-island fibers, adopts the conditions of high temperature and strong alkali (the temperature is more than or equal to 95 ℃ and the pH value is more than or equal to 13) to degrade the sea-phase COPET into sodium terephthalate and ethylene glycol, has various problems of recycling of hydrolysate, treatment of waste alkali liquor and the like, has difficult treatment of alkali reduction waste liquor with strong alkalinity, and has high pollution discharge cost.
The solvent sea-dissolving type (benzene reduction method) adopts low-density polyethylene (LDPE) as a sea component of sea-island fibers, and adopts organic solvents such as toluene or xylene to dissolve the sea-phase LDPE at a higher temperature (the temperature is more than or equal to 85 ℃), so that the leakage risk of toxic harmful solvents and the residue problem of trace toxic harmful solvents on superfine fibers exist, the recovered LDPE has toxic harmful organic solvents such as toluene or xylene, and the use value is reduced.
A hot water dissolving type (hot water dissolving method) is disclosed in CN108589028A, CN108589028A, CN108505190A, CN108589028A, CN108486683A and CN108424601A, polyvinyl alcohol (PVA) is used as a sea phase of a sea-island fiber, if an island component is PA6, the problem that the spinning temperature difference of the two phases of the sea-island is large (the temperature difference is more than 80 ℃) and the spinning on common sea-island spinning equipment is difficult exists, and the existence of water needs to be avoided in the drawing post-processing and application processes before fiber opening, otherwise, the fiber can generate a bonding phenomenon, and the service performance of the fiber is seriously influenced. The polyvinyl alcohol aqueous solution after opening is low in recycling value, and if the polyvinyl alcohol aqueous solution is directly discharged, the waste of resources is caused. In addition, the PVA sea component disclosed in the above patent contains additives such as a polyol or salt compound modifier, an antioxidant, a lubricant, and the like (the total content of which accounts for at least 15% of the sea component), which all increase the difficulty and cost of the treatment of the opening waste water.
In summary, the methods for opening sea-island fibers available in the market in mass production all have certain defects and are accompanied with irreversible environmental pollution. At present, no sea component exists, which can realize value retention or high added value recycling, has no toxicity or zero emission in the recycling process, and can be well matched with various spinning sea components such as high polymer PET, PA6, PP and the like.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, it is an object of the present invention to provide an island-in-sea fiber having PA6 as an island component, a method for preparing the same, and an ultrafine fiber formed therefrom, which are useful for solving the problems of the prior art.
To achieve the above objects and other related objects, the present invention is achieved by the following technical solutions.
The invention provides a sea-island fiber taking PA6 as an island component, wherein the sea-island fiber taking PA6 as the island component takes modified copolyester as the sea component, and the structural formula of the modified copolyester is shown as the following formula:
wherein,
repeating unit
Is randomly selected from
M is potassium or sodium, and n is more than or equal to 95.
According to the sea-island fiber with PA6 as the island component, the mass ratio of the sea component to the island component is 1: (1-9).
According to the sea-island fiber with PA6 as the island component, the island component PA6 is a conventional spinning slice.
According to the sea-island fiber with PA6 as island component, in the modified copolyester,
the number of repetitions of the structure is less than 3. Otherwise, the resulting modified copolyester may have an enhanced appearance in the molten state due to ionic aggregation effectsThe viscosity increases and the spinnability decreases.
The sea-island fiber taking PA6 as island component has the structure in the modified copolyester
In a molar ratio of 1: (1.1-2.4): (0.015 to 0.07): (0.04-0.20): (0.02-0.10), preferably, the molar ratio is 1: (1.1-2.4): (0.015 to 0.05): (0.05-0.20): (0.025 to 0.10), more preferably in a molar ratio of 1: (1.1-2.4): (0.02-0.05): (0.05-0.15): (0.025 to 0.075), most preferably in a molar ratio of 1: (1.1-2.4): (0.03-0.04): (0.05-0.10): (0.025 to 0.05).
According to the sea-island fiber with PA6 as an island component, the intrinsic viscosity of the modified copolyester is (0.4-0.7) dL/g. Intrinsic viscosity in this application is measured by capillary viscometry.
According to the sea-island fiber taking PA6 as an island component, the melting point of the modified copolyester is 200-240 ℃.
The sea-island fiber with PA6 as island component is prepared by the method comprising the following steps:
1) carrying out esterification reaction on ethylene glycol and terephthalic acid;
2) adding m-benzene dibasic acid dibasic ester-5-sodium sulfonate or m-benzene dibasic acid dibasic ester-5-potassium sulfonate, and adding 2-methyl-1, 3-propylene glycol and 1, 3-propylene glycol for ester exchange;
3) adding catalyst and heat stabilizer to perform polycondensation reaction.
According to the sea-island fiber with PA6 as the island component, in the step 1), the temperature of the esterification reaction is 240-270 ℃.
According to the sea-island fiber with PA6 as the island component, in the step 1), the esterification reaction time is 2-4 h.
According to the sea-island fiber with PA6 as the island component, in the step 2), the temperature of the ester exchange reaction is 240-270 ℃.
According to the sea-island fiber with PA6 as the island component, in the step 2), the time of the ester exchange reaction is 1-3 h.
According to the sea-island fiber with PA6 as the island component, in the step 3), the temperature of the polycondensation reaction is 270-300 ℃.
According to the sea-island fiber with PA6 as the island component, in the step 3), the time of polycondensation reaction is 2-4 h.
According to the sea-island fiber with PA6 as the island component, in the step 3), the catalyst is one or more of Zn, Sb, Mn, Ca or Co-containing compounds. More preferably, the catalyst is antimony trioxide.
According to the sea-island fiber taking PA6 as an island component, the adding amount of the catalyst is not more than 0.08 percent of the mass of the terephthalic acid, and the adding amount of the catalyst is preferably 0.01 to 0.08 percent.
According to the sea-island fiber with PA6 as the island component, in the step 3), the heat stabilizer is trimethyl phosphate or triphenyl phosphate.
According to the sea-island fiber taking PA6 as an island component, the addition amount of the heat stabilizer is 0.02-0.06% of the mass of the terephthalic acid.
According to the sea-island fiber taking PA6 as an island component, the molar ratio of terephthalic acid, ethylene glycol, m-phthalic acid dibasic ester-5-sodium sulfonate or potassium, 2-methyl-1, 3-propanediol and 1, 3-propanediol is 1: (1.1-2.4): (0.015 to 0.07): (0.04-0.20): (0.02-0.10).
The invention also discloses a preparation method of the sea-island fiber with PA6 as an island component, which comprises the following steps:
by adopting a melt composite spinning technology, the island component PA6 is fed into a first screw extruder for melt extrusion, and meanwhile, the sea component modified copolyester is fed into a second screw extruder for extrusion;
the two melts after melt extrusion enter a composite spinning box body, are metered by a metering pump, are sprayed out by a composite spinning spinneret to obtain nascent fiber, and then are subjected to post-treatment to obtain the sea-island fiber taking PA6 as an island component.
According to the above production method, the post-treatment is selected from one or more of stretching, heat setting, winding, texturing, bundling, curling and cutting.
According to the preparation method, the primary fiber is subjected to bundle drawing, heat setting, curling and cutting to obtain the sea-island short fiber taking PA6 as an island component.
According to the preparation method, the primary fiber is stretched, heat-set and wound to obtain the sea-island fully drawn yarn with PA6 as islands.
According to the preparation method, the primary fiber is stretched and wound to obtain the island-in-sea pre-oriented yarn with PA6 as an island component.
According to the preparation method, the primary fiber is stretched, heat-set, elasticated and wound to obtain the sea-island tensile deformation filament with PA6 as an island component.
According to the preparation method, the temperature of the fifth area in the first screw extruder is 265-270 ℃, 270-275 ℃, 275-280 ℃ and 270-275 ℃; the temperature of the fifth zone in the second screw extruder is 250-265 ℃, 265-275 ℃, 260-270 ℃ and 260-280 ℃.
According to the preparation method, the temperature of the composite spinning manifold is 265-280 ℃.
The invention also discloses PA6 superfine fiber, wherein the PA6 superfine fiber is obtained by removing sea components from the sea-island fiber which takes PA6 as island components.
According to the PA6 superfine fiber, the method for removing the sea component comprises the following steps: and (3) opening the sea-island fiber taking PA6 as an island component in water containing a swelling agent and a cosolvent.
According to the PA6 superfine fiber, when the fiber is opened, the mass ratio of the sea-island fiber taking PA6 as an island component to water is 1: (10-100).
According to the PA6 superfine fiber, the temperature of water is 60-70 ℃ during fiber opening. The dissolution of the sea material can be better promoted at this lower temperature.
According to the PA6 superfine fiber, the fiber opening treatment time is 30-120 min.
The sea material in the application can be removed under the coordination of the swelling agent and the cosolvent, and the damage of the island material caused by fiber splitting under the condition of adopting a high-temperature strong alkali condition or matching with other organic solvents at high temperature in the prior art is avoided.
According to the PA6 superfine fiber, the weight of the swelling agent in water is 5-25 wt% during fiber opening. Preferably, the mass of the swelling agent in water is 8 wt% to 15 wt%.
According to the PA6 superfine fiber, the mass of the cosolvent in water is 2-20 wt% during fiber opening. Preferably, the mass of the cosolvent in the water is 5-10 wt%.
The PA6 superfine fiber is prepared from sulfolane, urea, isopropanol, glycol, polyoxyethylene and polyvinylpyrrolidone. Preferably, the polyoxyethylene is PEG 200. Preferably, the polyvinylpyrrolidone is PVP-K30.
The PA6 superfine fiber is prepared from the PA6 superfine fiber, and the cosolvent is selected from NH-containing4 +、K+And Na+Is one or more of the soluble salts of (A), the anion of the soluble salt is selected from SO4 2-、CO3 2-、NO3 -、Ac-And Cl-One or more of (a).
The modified copolyester in the technical scheme of the application has almost no structural change in water or hot water at 70 ℃ when used as a sea material, but can be dissolved in a shorter time when a certain amount of swelling agent and cosolvent are present in the hot water, which can be theoretically attributed to-CH2-CH(CH3)-CH2Steric effect of monomethyl side chains in the unitsThe aggregation structure is looser, and the swelling agent can enter more easily; -CH2-CH2-CH2The freely rotating helical conformation of the units, making the macromolecular structure more mobile under the action of the swelling agent; the ionizing effect of the m-benzenesulfonate group causes the macromolecule to eventually dissolve in the aqueous solution. Since this modified copolyester is insoluble in boiling water but soluble in a low-temperature near-neutral aqueous solution under specific conditions, when used as a sea material for sea-island fibers, it can be effectively removed by a mild process and means, and damage to the island component in the sea-island fibers is better avoided, thereby forming PA6 ultrafine fibers having only the island component.
Compared with the prior art, the technical scheme in the application has the following beneficial effects:
the modified copolyester is adopted as the sea material of the sea-island fiber, and the PA6 is adopted as the island material, so that the formed sea-island fiber has good spinnability, and the sea-island fiber can be opened under very mild conditions due to the characteristics of the modified copolyester, and the physicochemical property of the island component PA6 cannot be influenced by the mild opening condition, so that the PA6 superfine fiber formed by the island component is not damaged, and the PA6 superfine fiber with excellent performance is very easily formed.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
The structural formula of the modified copolyester used in the examples of the present application is shown as follows:
wherein,
repeating unit
Is randomly selected from
M is potassium or sodium, and n is more than or equal to 95.
More specifically, in the modified copolyester,
the number of repetitions of the structure is less than 3. Otherwise, the formed modified copolyester is intensified due to the ionic aggregation effect, the apparent viscosity is increased in a molten state, and the spinnability is reduced.
More specifically, the intrinsic viscosity of the modified copolyester is (0.4-0.7) dL/g. Intrinsic viscosity in this application is measured by capillary viscometry.
More specifically, the melting point of the modified copolyester is 200-240 ℃.
More specifically, the preparation method of the modified polyester comprises the following steps:
1) carrying out esterification reaction on ethylene glycol and terephthalic acid; the temperature of the esterification reaction is 240-270 ℃; the esterification reaction time is 2-4 h;
2) adding m-benzene dibasic acid dibasic ester-5-sodium sulfonate or m-benzene dibasic acid dibasic ester-5-potassium sulfonate, and adding 2-methyl-1, 3-propylene glycol and 1, 3-propylene glycol for ester exchange; the temperature of the ester exchange reaction is 240-270 ℃; the time of the ester exchange reaction is 1-3 h;
3) adding a catalyst and a heat stabilizer to perform polycondensation reaction; the temperature of the polycondensation reaction is 270-300 ℃; the time of the polycondensation reaction is 2-4 h; wherein the catalyst is antimony trioxide; the heat stabilizer is trimethyl phosphate or triphenyl phosphate; the addition amount of the heat stabilizer is 0.02-0.06 percent of the mass of the terephthalic acid; the addition amount of the catalyst is not more than 0.08 percent of the mass of the terephthalic acid.
And discharging the modified copolyester obtained through the reaction, granulating and drying to obtain the modified copolyester slice.
The modified copolyester according to the present application can be formed into the structure as described above by the molar ratio of the raw materials and the reaction temperature. Specifically, the molar ratio of terephthalic acid, ethylene glycol, m-phthalic acid dibasic ester-5-sodium sulfonate or potassium, 2-methyl-1, 3-propanediol and 1, 3-propanediol is 1: (1.1-2.4): (0.015 to 0.07): (0.04-0.20): (0.02-0.10).
Example 1
In this example, the molar ratio of terephthalic acid, ethylene glycol, m-phthalic acid dibasic ester-5-sodium sulfonate or potassium, 2-methyl-1, 3-propanediol, and 1, 3-propanediol is 1: 2.0: 0.05: 0.10: 0.08, forming a modified copolyester by the method described above.
The sea component of the sea-island fiber in this embodiment is the modified copolyester as described above, the island component is PA6, and the mass ratio of the sea component to the island component in this embodiment is 1: 7.
by adopting a melt composite spinning technology, the island component PA6 is fed into a first screw extruder for melt extrusion, and meanwhile, the sea component modified copolyester is fed into a second screw extruder for extrusion; the temperature of the fifth zone in the first screw extruder is 265-270 ℃, 270-275 ℃, 275-280 ℃ and 270-275 ℃; the temperature of the fifth area in the second screw extruder is 250-265 ℃, 265-275 ℃, 260-270 ℃ and 260-280 ℃;
filtering the two melts after melt extrusion through a prefilter respectively, conveying the two melts into a composite spinning manifold, metering the two melts through a metering pump, and conveying the two melts into a composite spinning assembly, wherein the temperature of the composite spinning manifold is 265-280 ℃, the two melts are sprayed out through a composite spinning spinneret to obtain nascent fibers, and the nascent fibers are stretched, heat-set and wound to obtain 150dtex 16-island fully-stretched sea-island filaments taking PA6 as islands.
The sea-island fully drawn yarn in this example was treated in a 60 ℃ aqueous solution of 10 wt% sulfolane and 8 wt% potassium nitrate for 40min, and the sea component modified copolyester of the sea-island fully drawn yarn was completely dissolved to form an ultrafine fiber filament containing only PA6, wherein the mass ratio of the modified copolyester to water was 1: 10.
Example 2
In this example, the molar ratio of terephthalic acid, ethylene glycol, m-phthalic acid dibasic ester-5-sodium sulfonate or potassium, 2-methyl-1, 3-propanediol, and 1, 3-propanediol is 1: 1.5: 0.03: 0.05: 0.10, forming the modified copolyester by the method as described above.
In this embodiment, the sea component in the sea island fiber is the modified copolyester, the island component is half-dull PA6 and black PA6 masterbatch, and the mass ratio of the sea component to the island component in this embodiment is 1: 5.
by adopting a melt composite spinning technology, island component semi-dull PA6 and black PA6 master batches are blended by a dispersing agent, the blending ratio is 7:3, the mixture is uniformly mixed and then fed into a first screw extruder for melt extrusion, and simultaneously sea component modified copolyester is fed into a second screw extruder for extrusion; the temperature of the fifth zone in the first screw extruder is 265-270 ℃, 270-275 ℃, 275-280 ℃ and 270-275 ℃; the temperature of the fifth area in the second screw extruder is 250-265 ℃, 265-275 ℃, 260-270 ℃ and 260-280 ℃;
filtering the two melts after melt extrusion through a prefilter respectively, conveying the two melts into a composite spinning manifold, metering the two melts through a metering pump, and conveying the two melts into a composite spinning assembly, wherein the temperature of the composite spinning manifold is 265-280 ℃, the two melts are sprayed out through a composite spinning spinneret to obtain nascent fibers, and the nascent fibers are subjected to bundling, stretching, heat setting, curling and cutting to obtain the 3.0dtex 37-island black sea-island short fibers taking PA6 as islands.
The sea-island short fiber in the embodiment is treated in 60 ℃ water solution of 10 wt% of isopropanol and 8 wt% of sodium nitrate for 40min, the sea component modified copolyester of the sea-island short fiber is completely dissolved, and black superfine fiber only containing PA6 is formed, wherein the mass ratio of the modified copolyester to water is 1: 10.
Example 3
In this example, the molar ratio of terephthalic acid, ethylene glycol, m-phthalic acid dibasic ester-5-sodium sulfonate or potassium, 2-methyl-1, 3-propanediol, and 1, 3-propanediol is 1: 1.8: 0.07: 0.20: 0.05, modified copolyester was formed by the method described above.
In this embodiment, the sea component in the sea island fiber is the modified copolyester, the island component is PA6, and the mass ratio of the sea component to the island component in this embodiment is 1: 9.
by adopting a melt composite spinning technology, the island component PA6 is fed into a first screw extruder for melt extrusion, and meanwhile, the sea component modified copolyester is fed into a second screw extruder for extrusion; the temperature of the fifth zone in the first screw extruder is 265-270 ℃, 270-275 ℃, 275-280 ℃ and 270-2275 ℃; the temperature of the fifth area in the second screw extruder is 250-265 ℃, 265-275 ℃, 260-270 ℃ and 260-280 ℃;
filtering the two melts after melt extrusion through a prefilter respectively, conveying the two melts into a composite spinning manifold, metering the two melts through a metering pump, and conveying the two melts into a composite spinning assembly, wherein the temperature of the composite spinning manifold is 265-280 ℃, the two melts are sprayed out through a composite spinning spinneret to obtain nascent fibers, and the nascent fibers are stretched, heat-set and wound to obtain 150dtex DTY island filaments with 16 islands and PA6 as islands.
The DTY sea-island filament in the embodiment is treated in 50 ℃ water solution of 10 wt% of ethylene glycol and 8 wt% of sodium nitrate for 40min, the sea component modified copolyester of the sea-island fully drawn yarn is completely dissolved, and superfine fiber only containing PA6 is formed, wherein the mass ratio of the modified copolyester to water is 1: 10.
The method for testing the strength after fiber opening is GBT-14344-.
The parameter method of the blackness in the application refers to the whiteness chromaticity test method GB/T17644-2008 of textile fibers.
The comparative example 1 in the application is that LDPE is taken as a sea material, semi-dull PA6+ black PA6 master batches with the same mixing ratio are taken as island materials in the prior art, the sea-island fiber with the monofilament titer of 3.0dtex and 37 islands is prepared by melt spinning of a sea-island fiber composite component, and the superfine PA6 fiber is obtained after fiber opening and sea material removal by a benzene reduction method.
Compared with the example 2 and the comparative example 1, the PA6 sea-island fiber with the same specification has the same theoretical sea-island proportion, the breaking strength after fiber splitting is different, the blackness L value of the superfine fiber after fiber splitting is obviously different, and the blackness of the fiber before and after toluene reduction fiber splitting is different by 5. And (3) proving that: the toluene reduction and fiber opening conditions in comparative example 1 may damage the island component and cause discoloration of the island component; the modified copolyester is used as a sea material, the fiber opening weight loss is in accordance with the theoretical sea island proportion, the fiber opening is complete, and the physical and chemical properties of the island component material PA6 are not influenced due to the mild fiber opening condition.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. The sea-island fiber with PA6 as an island component is characterized in that the sea-island fiber with PA6 as the island component is modified copolyester as the sea component, and the structural formula of the modified copolyester is shown as the following formula:
wherein the repeating unit
Is randomly selected from
M is potassium or sodium; n is more than or equal to 95.
2. The sea-island fiber of claim 1, wherein the mass ratio of the sea component to the island component is 1: (1-9).
3. The sea-island fiber of claim 1, wherein in the modified copolyester,
4. The sea-island fiber of claim 1, wherein the modified copolyester is structurally characterized
5. The sea-island fiber of claim 1, wherein the modified copolyester has an intrinsic viscosity of (0.4 to 0.7) dL/g; and/or the melting point of the modified copolyester is 200-240 ℃.
6. A process for preparing an island fiber according to any of claims 1 to 5 comprising the steps of:
by adopting a melt composite spinning technology, the island component PA6 is fed into a first screw extruder for melt extrusion, and meanwhile, the sea component modified copolyester is fed into a second screw extruder for melt extrusion;
the two melts after melt extrusion enter a composite spinning box body, are respectively metered by a metering pump, are sprayed out by a composite spinning spinneret to obtain nascent fibers, and then are subjected to post-treatment to obtain the sea-island fibers taking PA6 as island components.
7. The method of claim 6, wherein the post-treatment is selected from one or more of stretching, heat-setting, winding, texturing, bundling, crimping, and cutting.
8. The method of claim 6, wherein the temperature of the five zones in the first screw extruder is 265 ℃ to 270 ℃, 270 ℃ to 275 ℃, 275 ℃ to 280 ℃, 270 ℃ to 275 ℃;
and/or the temperature of the fifth area in the second screw extruder is 250-265 ℃, 265-275 ℃, 260-270 ℃ and 260-280 ℃;
and/or the temperature of the composite spinning manifold is 265-280 ℃.
9. PA6 superfine fiber, which is obtained by splitting the sea-island fiber of any one of claims 1 to 5 in water containing swelling agent and cosolvent to remove sea components.
10. The PA6 ultrafine fiber according to claim 9, wherein the mass ratio of sea-island fiber with PA6 as island component to water is 1: (10-100);
and/or the temperature of the water is 60-70 ℃;
and/or the time of the fiber opening treatment is 30 min-120 min;
and/or the mass of the swelling agent in water is 5-25 wt%;
and/or the mass of the cosolvent in the water is 2-20 wt%;
and/or the swelling agent is one or more selected from sulfolane, urea, isopropanol, glycol, polyoxyethylene and polyvinylpyrrolidone;
and/or the cosolvent is selected from NH-containing4 +、K+And Na+Is one or more of the soluble salts of (A), the anion of the soluble salt is selected from SO4 2-、CO3 2-、NO3 -、Ac-And Cl-One or more of (a).
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| CN115747988A (en) * | 2022-11-17 | 2023-03-07 | 明新梅诺卡(江苏)新材料有限公司 | Preparation method of superfine fiber taking modified PVA as sea |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100822283B1 (en) * | 2002-10-30 | 2008-04-16 | 주식회사 코오롱 | A method of extracting sea component from woven or knitted fabric with sea-island type composite fiber |
| KR101489437B1 (en) * | 2013-12-13 | 2015-02-03 | 도레이케미칼 주식회사 | Extractable co-polyester in hot-water with low temperature and method for manufacturing thereof |
| KR101566843B1 (en) * | 2011-08-11 | 2015-11-06 | 도레이 카부시키가이샤 | Islands-in-sea fiber |
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2020
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100822283B1 (en) * | 2002-10-30 | 2008-04-16 | 주식회사 코오롱 | A method of extracting sea component from woven or knitted fabric with sea-island type composite fiber |
| KR101566843B1 (en) * | 2011-08-11 | 2015-11-06 | 도레이 카부시키가이샤 | Islands-in-sea fiber |
| KR101489437B1 (en) * | 2013-12-13 | 2015-02-03 | 도레이케미칼 주식회사 | Extractable co-polyester in hot-water with low temperature and method for manufacturing thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115747988A (en) * | 2022-11-17 | 2023-03-07 | 明新梅诺卡(江苏)新材料有限公司 | Preparation method of superfine fiber taking modified PVA as sea |
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