CN117684285B - Reinforced flame-retardant regenerated polyester fiber and preparation method thereof - Google Patents
Reinforced flame-retardant regenerated polyester fiber and preparation method thereof Download PDFInfo
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- CN117684285B CN117684285B CN202311741974.0A CN202311741974A CN117684285B CN 117684285 B CN117684285 B CN 117684285B CN 202311741974 A CN202311741974 A CN 202311741974A CN 117684285 B CN117684285 B CN 117684285B
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- 229920000728 polyester Polymers 0.000 title claims abstract description 89
- 239000000835 fiber Substances 0.000 title claims abstract description 66
- 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 title claims abstract description 56
- 239000003063 flame retardant Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229920001577 copolymer Polymers 0.000 claims abstract description 34
- 239000002121 nanofiber Substances 0.000 claims abstract description 31
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229940051201 quinoline yellow Drugs 0.000 claims abstract description 25
- 235000012752 quinoline yellow Nutrition 0.000 claims abstract description 25
- 239000004172 quinoline yellow Substances 0.000 claims abstract description 25
- FLNRHACWTVIBQS-UHFFFAOYSA-N triphenyl(prop-2-enyl)phosphanium Chemical compound C=1C=CC=CC=1[P+](C=1C=CC=CC=1)(CC=C)C1=CC=CC=C1 FLNRHACWTVIBQS-UHFFFAOYSA-N 0.000 claims abstract description 24
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 15
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 15
- 239000007822 coupling agent Substances 0.000 claims abstract description 15
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 9
- 150000003254 radicals Chemical class 0.000 claims abstract description 9
- 238000009987 spinning Methods 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 29
- 238000009835 boiling Methods 0.000 claims description 20
- 239000003999 initiator Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- 229920000642 polymer Polymers 0.000 claims description 13
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- -1 Polyethylene terephthalate Polymers 0.000 description 2
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002134 carbon nanofiber Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- REPWBKQJAMXHFL-UHFFFAOYSA-N phenylphosphane;hydrobromide Chemical compound [Br-].[PH3+]C1=CC=CC=C1 REPWBKQJAMXHFL-UHFFFAOYSA-N 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000012763 reinforcing filler Substances 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WFFZGYRTVIPBFN-UHFFFAOYSA-N 3h-indene-1,2-dione Chemical group C1=CC=C2C(=O)C(=O)CC2=C1 WFFZGYRTVIPBFN-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 125000005493 quinolyl group Chemical group 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920006135 semi-crystalline thermoplastic polymer Polymers 0.000 description 1
- 238000007493 shaping process 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing phosphorus
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a reinforced flame-retardant regenerated polyester fiber and a preparation method thereof, and relates to the technical field of regenerated polyester fibers, wherein the reinforced flame-retardant regenerated polyester fiber comprises, by weight, 100 parts of regenerated polyester, 12-18 parts of a functional copolymer, 1-3 parts of a compatibilizer, 3-5 parts of a coupling agent, 0.6-1.2 parts of an antioxidant, 5-10 parts of a nanofiber and 1-3 parts of quinoline yellow, and the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction. The reinforced flame-retardant regenerated polyester fiber has good mechanical property, good flame retardance and sufficient ageing resistance.
Description
Technical Field
The invention relates to the technical field of regenerated polyester fibers, in particular to a reinforced flame-retardant regenerated polyester fiber and a preparation method thereof.
Background
Polyethylene terephthalate is a semi-crystalline thermoplastic polymer material with excellent performance, and is widely applied to the fields of chemical fiber, packaging, medicine, electronic machinery and the like. The treatment problem of waste polyester products comes at the same time of the rapid development of the polyester industry, and the huge stock of waste polyester products in society not only brings huge pressure to the ecological environment, but also causes serious waste of resources. It is in this situation that recycled polyester materials have grown and their advent has attracted widespread attention.
The regenerated polyester material is obtained by removing bottle caps, labels and additives from polyester bottle flakes and processing the bottle flakes by using a physical or chemical method, and has the defects of high impurity content, wide molecular weight distribution, large viscosity range and difficult spinning. The polyester fiber has the advantages of high strength, good decontamination performance and the like, is widely applied to clothing fabrics and other fields, and is the polyester material with the highest use amount in the world at present. It is seen that how to make the regenerated polyester fiber with good comprehensive performance and performance stability is important.
The existing regenerated polyester fiber has the technical problems of insufficient strength and insufficient flame retardance. In order to improve the strength and the flame retardance of the regenerated polyester fiber, the strength and the flame retardance of the regenerated polyester fiber are mainly realized by adding reinforcing filler and flame retardant, however, the existing flame retardant is extremely polluted to the environment due to combustion, and the phase separation of the prepared regenerated polyester fiber is easy to occur in the long-term use process due to the compatibility problem between the reinforcing filler, the flame retardant and the regenerated polyester base material, so that the service life is influenced.
In order to solve the problems, the Chinese patent publication No. CN103409844B discloses a preparation method of reinforced flame-retardant regenerated polyester fiber, which comprises the steps of uniformly stirring and mixing dried regenerated polyester, phosphorus flame retardant and nano material at 30-180 ℃, extruding and granulating at 240-300 ℃ to obtain reinforced flame-retardant regenerated polyester composite slices, drying the reinforced flame-retardant regenerated polyester composite slices, cooling to 40-90 ℃, adding a dispersing agent to obtain spinning raw materials, spinning and drafting. The reinforced flame-retardant regenerated polyester chip provided by the invention has good spinning molding and excellent fiber quality, and the adopted nano material can generate a synergistic effect with the phosphorus flame retardant, so that the consumption of the flame retardant can be effectively reduced, the cost is reduced, the reinforcing effect can be realized, and the mechanical property of the fiber can be effectively improved. However, due to the problem of dispersibility of the nanomaterial and the problem of compatibility of the flame retardant and the nanomaterial with the polyester material, the aging resistance and mechanical properties of the fiber material still need to be further improved.
Therefore, a more effective method is needed to be required to prepare the reinforced flame-retardant regenerated polyester fiber with good mechanical properties and flame retardance and sufficient ageing resistance and the preparation method thereof.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the reinforced flame-retardant regenerated polyester fiber with good mechanical properties and flame retardance and sufficient ageing resistance and the preparation method thereof.
The invention can be realized by the following technical scheme:
The reinforced flame-retardant regenerated polyester fiber comprises, by weight, 100 parts of regenerated polyester, 12-18 parts of a functional copolymer, 1-3 parts of a compatibilizer, 3-5 parts of a coupling agent, 0.6-1.2 parts of an antioxidant, 5-10 parts of a nanofiber and 1-3 parts of quinoline yellow, wherein the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction.
Preferably, the recycled polyester is prepared by sequentially sorting, crushing, cleaning and drying recycled polyester bottle flakes.
Preferably, the preparation method of the functional copolymer comprises the following steps of adding allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate and an initiator into a high-boiling point solvent, stirring and reacting for 4-6 hours under the inert gas atmosphere at 60-70 ℃, precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and finally drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the functional copolymer.
Preferably, the mass ratio of the allyl triphenylphosphine bromide to the (9 CI) -2-vinyl pyrimidine to the methyl methacrylate to the initiator to the high boiling point solvent is 2 (0.8-1.2), 1-3, 0.04-0.07 and 15-30.
Preferably, the initiator is azobisisobutyronitrile, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone, and the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the compatibilizer is at least one of PE-g-ST and PE-g-MAH.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the antioxidant is at least one of antioxidant 1010, antioxidant 168 and antioxidant 1076.
Preferably, the nanofiber is at least one of a nanometer boron fiber and a nanometer carbon fiber, the average diameter of the nanofiber is 60-100nm, and the length of the nanofiber is 1-5mm.
The invention also provides a preparation method of the reinforced flame-retardant regenerated polyester fiber, which comprises the following steps:
Step S1, uniformly mixing other raw materials except quinoline yellow, blending and melting by a screw extruder, spinning and forming the melt by a special-shaped hole spinneret plate, and drawing and forming to obtain functional silk strips;
And S2, soaking the functional yarn prepared in the step S1 in a quinoline yellow solution with the mass percentage concentration of 10-20wt% at 50-60 ℃ for 20-40 hours, taking out and drying to obtain the reinforced flame-retardant regenerated polyester fiber.
Preferably, the spinning temperature of the spinning molding in the step S1 is 240-290 ℃ and the spinning speed is 2200-2800m/min.
Preferably, the temperature of the draft setting in the step S1 is 60-66 ℃.
Preferably, the drying in step S2 is performed at 95-105 ℃ to constant weight.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the reinforced flame-retardant regenerated polyester fiber disclosed by the invention has the advantages of simple process, convenient operation control, high preparation efficiency and finished product qualification rate, small dependence on equipment and suitability for continuous large-scale production.
(2) The reinforced flame-retardant regenerated polyester fiber disclosed by the invention has the advantages that the introduced flame-retardant component is an organic component, the compatibility with polyester is good, the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through free radical copolymerization, and phenyl phosphine bromide, pyrimidine and ester structures are simultaneously introduced into the molecular chain of the functional copolymer, and are mutually matched, so that the excellent flame retardance, ageing resistance and mechanical properties of the polyester fiber can be endowed, the added nanofiber can be further reinforced, and the flame retardance and mechanical properties can be further improved through the synergistic effect of the added nanofiber and the functional copolymer. In addition, the introduced phosphine bromide cationic structure can provide reaction sites for subsequent crosslinking and curing.
(3) According to the reinforced flame-retardant regenerated polyester fiber disclosed by the invention, ionic crosslinking is realized by soaking quinoline yellow solution in the preparation process, and quinolyl and indenedione structures are introduced to the surface of the fiber material and interact with phenyl phosphine bromide, pyrimidine and ester structures in the fiber material, so that the flame retardance, mechanical properties and ageing resistance of the fiber are further improved. Through ion exchange, bromide ions in the fiber structure can be carried out by water in the form of sodium bromide, so that the fiber structure is safe and nontoxic in use and combustion process.
Detailed Description
In order to better understand the technical solution of the present invention, the following describes the product of the present invention in further detail with reference to examples.
Example 1
The reinforced flame-retardant regenerated polyester fiber comprises, by weight, 100 parts of regenerated polyester, 12 parts of a functional copolymer, 1 part of a compatibilizer, 3 parts of a coupling agent, 0.6 part of an antioxidant, 5 parts of a nanofiber and 1 part of quinoline yellow, wherein the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction.
The recycled polyester is prepared by sequentially sorting, crushing, cleaning and drying recycled polyester bottle flakes.
The preparation method of the functional copolymer comprises the steps of adding allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate and an initiator into a high-boiling point solvent, stirring and reacting for 4 hours at 60 ℃ in an inert gas atmosphere, precipitating the mixture in water, washing the precipitated polymer with ethanol for 3 times, and finally drying the washed polymer in a vacuum drying oven at 85 ℃ until the weight is constant to obtain the functional copolymer, wherein the mass ratio of the allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate, the initiator and the high-boiling point solvent is 2:0.8:1:0.04:15, the initiator is azo diisobutyronitrile, the high-boiling point solvent is dimethyl sulfoxide, and the inert gas is nitrogen. The mass ratio of structural units respectively introduced by allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate in the copolymer is 1.98:0.79:0.98 as confirmed by quantitative elemental analysis.
The compatibilizer is PE-g-ST, the coupling agent is silane coupling agent KH550, the antioxidant is antioxidant 1010, the nanofiber is a nanometer boron fiber, and the average diameter of the nanofiber is 60nm and the length of the nanofiber is 1mm.
The preparation method of the reinforced flame-retardant regenerated polyester fiber comprises the following steps:
Step S1, uniformly mixing other raw materials except quinoline yellow, blending and melting by a screw extruder, spinning and forming the melt by a special-shaped hole spinneret plate, and drawing and forming to obtain functional silk strips;
And S2, soaking the functional yarn prepared in the step S1 in a quinoline yellow solution with the mass percentage concentration of 10wt% at 50 ℃ for 20 hours, taking out and drying to obtain the reinforced flame-retardant regenerated polyester fiber.
The spinning temperature of the spinning molding in the step S1 is 240 ℃, the spinning speed is 2200m/min, the temperature of the drafting sizing in the step S1 is 60 ℃, and the drying in the step S2 is to constant weight at 95 ℃.
Example 2
The reinforced flame-retardant regenerated polyester fiber comprises, by weight, 100 parts of regenerated polyester, 14 parts of a functional copolymer, 1.5 parts of a compatibilizer, 3.5 parts of a coupling agent, 0.8 part of an antioxidant, 6 parts of a nanofiber and 1.5 parts of quinoline yellow, wherein the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction.
The recycled polyester is prepared by sequentially sorting, crushing, cleaning and drying recycled polyester bottle flakes.
The preparation method of the functional copolymer comprises the steps of adding allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate and an initiator into a high-boiling point solvent, stirring and reacting for 4.5 hours at 63 ℃ in an inert gas atmosphere, precipitating the polymer in water, washing the precipitated polymer with ethanol for 4 times, and finally drying the polymer in a vacuum drying oven at 88 ℃ to constant weight to obtain the functional copolymer, wherein the mass ratio of the allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate to the initiator to the high-boiling point solvent is 2:0.9:1.5:0.05:17, the initiator is azodiisobutyronitrile, the high-boiling point solvent is N, N-dimethylformamide, and the inert gas is helium.
The compatibilizer is PE-g-MAH, the coupling agent is silane coupling agent KH560, the antioxidant is antioxidant 168, the nanofiber is carbon nanofiber, and the average diameter of the nanofiber is 70nm and the length of the nanofiber is 2mm.
The preparation method of the reinforced flame-retardant regenerated polyester fiber comprises the following steps:
Step S1, uniformly mixing other raw materials except quinoline yellow, blending and melting by a screw extruder, spinning and forming the melt by a special-shaped hole spinneret plate, and drawing and forming to obtain functional silk strips;
and S2, soaking the functional yarn prepared in the step S1 in a quinoline yellow solution with the mass percentage concentration of 13wt% at 53 ℃ for 25 hours, taking out and drying to obtain the reinforced flame-retardant regenerated polyester fiber.
The spinning temperature of the spinning molding in the step S1 is 260 ℃, the spinning speed is 2400m/min, the temperature of the drafting sizing in the step S1 is 62 ℃, and the drying in the step S2 is to constant weight at 98 ℃.
Example 3
The reinforced flame-retardant regenerated polyester fiber comprises, by weight, 100 parts of regenerated polyester, 15 parts of a functional copolymer, 2 parts of a compatibilizer, 4 parts of a coupling agent, 0.9 part of an antioxidant, 7.5 parts of a nanofiber and 2 parts of quinoline yellow, wherein the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction.
The recycled polyester is prepared by sequentially sorting, crushing, cleaning and drying recycled polyester bottle flakes.
The preparation method of the functional copolymer comprises the steps of adding allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate and an initiator into a high-boiling point solvent, stirring and reacting for 5 hours under the atmosphere of inert gas at 65 ℃, precipitating the mixture in water, washing the precipitated polymer with ethanol for 5 times, and finally drying the washed polymer in a vacuum drying oven at 90 ℃ until the weight is constant to obtain the functional copolymer, wherein the mass ratio of the allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate, the initiator and the high-boiling point solvent is 2:1:2:0.055:23, the initiator is azo diisobutyronitrile, the high-boiling point solvent is N-methyl pyrrolidone, and the inert gas is neon.
The compatibilizer is PE-g-ST, the coupling agent is silane coupling agent KH570, the antioxidant is antioxidant 1076, the nanofiber is a nanometer boron fiber, and the average diameter of the nanofiber is 80nm and the length of the nanofiber is 3.5mm.
The preparation method of the reinforced flame-retardant regenerated polyester fiber comprises the following steps:
Step S1, uniformly mixing other raw materials except quinoline yellow, blending and melting by a screw extruder, spinning and forming the melt by a special-shaped hole spinneret plate, and drawing and forming to obtain functional silk strips;
And S2, soaking the functional yarn prepared in the step S1 in a quinoline yellow solution with the mass percentage concentration of 15wt% at 55 ℃ for 30 hours, taking out and drying to obtain the reinforced flame-retardant regenerated polyester fiber.
The spinning temperature of the spinning molding in the step S1 is 270 ℃, the spinning speed is 2600m/min, the temperature of the drawing molding in the step S1 is 64 ℃, and the drying in the step S2 is to constant weight at 100 ℃.
Example 4
The reinforced flame-retardant regenerated polyester fiber comprises, by weight, 100 parts of regenerated polyester, 17 parts of a functional copolymer, 2.5 parts of a compatibilizer, 4.5 parts of a coupling agent, 1.1 parts of an antioxidant, 9 parts of a nanofiber and 2.5 parts of quinoline yellow, wherein the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction.
The recycled polyester is prepared by sequentially sorting, crushing, cleaning and drying recycled polyester bottle flakes.
The preparation method of the functional copolymer comprises the steps of adding allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate and an initiator into a high-boiling point solvent, stirring and reacting for 5.5 hours at 68 ℃ in an inert gas atmosphere, precipitating the mixture in water, washing the precipitated polymer with ethanol for 6 times, and finally drying the washed polymer in a vacuum drying oven at 93 ℃ to constant weight to obtain the functional copolymer, wherein the mass ratio of the allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate to the initiator to the high-boiling point solvent is 2:1.1:2.5:0.065:28, the initiator is azo diisobutyronitrile, the high-boiling point solvent is a mixture formed by mixing dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone according to the mass ratio of 1:3:2, and the inert gas is argon.
The compatibilizer is a mixture formed by mixing PE-g-ST and PE-g-MAH according to a mass ratio of 3:5, the coupling agent is a mixture formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 1:3:5, the antioxidant is a mixture formed by mixing an antioxidant 1010, an antioxidant 168 and an antioxidant 1076 according to a mass ratio of 1:2:3, the nanofiber is a mixture formed by mixing a nano boron fiber and a nano carbon fiber according to a mass ratio of 1:3, and the average diameter of the nanofiber is 90nm and the length of the nanofiber is 4mm.
The preparation method of the reinforced flame-retardant regenerated polyester fiber comprises the following steps:
Step S1, uniformly mixing other raw materials except quinoline yellow, blending and melting by a screw extruder, spinning and forming the melt by a special-shaped hole spinneret plate, and drawing and forming to obtain functional silk strips;
And S2, soaking the functional yarn prepared in the step S1 in a quinoline yellow solution with the mass percentage concentration of 18wt% at 58 ℃ for 35 hours, taking out and drying to obtain the reinforced flame-retardant regenerated polyester fiber.
The spinning temperature of the spinning molding in the step S1 is 280 ℃, the spinning speed is 2700m/min, the temperature of the drafting sizing in the step S1 is 65 ℃, and the drying in the step S2 is to constant weight at 103 ℃.
Example 5
The reinforced flame-retardant regenerated polyester fiber comprises, by weight, 100 parts of regenerated polyester, 18 parts of a functional copolymer, 3 parts of a compatibilizer, 5 parts of a coupling agent, 1.2 parts of an antioxidant, 10 parts of a nanofiber and 3 parts of quinoline yellow, wherein the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction.
The recycled polyester is prepared by sequentially sorting, crushing, cleaning and drying recycled polyester bottle flakes.
The preparation method of the functional copolymer comprises the steps of adding allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate and an initiator into a high-boiling point solvent, stirring and reacting for 6 hours at 70 ℃ in an inert gas atmosphere, precipitating in water, washing the precipitated polymer with ethanol for 6 times, and finally drying the polymer in a vacuum drying oven at 95 ℃ until the weight is constant to obtain the functional copolymer, wherein the mass ratio of the allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine, methyl methacrylate to the initiator to the high-boiling point solvent is 2:1.2:3:0.07:30, the initiator is azo diisobutyronitrile, the high-boiling point solvent is dimethyl sulfoxide, and the inert gas is nitrogen.
The compatibilizer is PE-g-ST, the coupling agent is silane coupling agent KH550, the antioxidant is antioxidant 168, the nanofiber is carbon nanofiber, and the average diameter of the nanofiber is 100nm and the length of the nanofiber is 5mm.
The preparation method of the reinforced flame-retardant regenerated polyester fiber comprises the following steps:
Step S1, uniformly mixing other raw materials except quinoline yellow, blending and melting by a screw extruder, spinning and forming the melt by a special-shaped hole spinneret plate, and drawing and forming to obtain functional silk strips;
and S2, soaking the functional yarn prepared in the step S1 in a quinoline yellow solution with the mass percentage concentration of 20wt% at 60 ℃ for 40 hours, taking out and drying to obtain the reinforced flame-retardant regenerated polyester fiber.
The spinning temperature of the spinning molding in the step S1 is 290 ℃, the spinning speed is 2800m/min, the temperature of the drawing and shaping in the step S1 is 66 ℃, and the drying in the step S2 is to constant weight at 105 ℃.
Comparative example 1
A reinforced flame retardant recycled polyester fiber and a method for preparing the same are basically the same as example 1, except that quinoline yellow is not added.
Comparative example 2
A reinforced flame-retardant recycled polyester fiber and a method for preparing the same are basically the same as in example 1, except that (9 CI) -2-vinyl pyrimidine is not added.
Meanwhile, in order to evaluate the specific technical effects of the reinforced flame-retardant regenerated polyester fiber, the reinforced flame-retardant regenerated polyester fiber is subjected to related performance test, the test results are shown in table 1, the test method comprises the steps of detecting the flame retardance of each product according to GB/T5454-1997 textile combustion performance test oxygen index method, detecting the mechanical properties according to GB/T14344-2022 chemical fiber filament tensile property test method, wherein the specific test conditions are that a pre-tension value is set to 5cN, the clamping length is set to 250mm, the tensile rate is set to 250mm/min, each fiber sample is tested for 10-20 times until stable data are obtained, the CV value is required to be kept within 15%, the aging resistance is that each product is cooled to room temperature after being placed at 85 ℃ for 100 hours, the breaking strength is tested again according to the test method of the mechanical properties, and the retention rate of the breaking strength after aging is calculated, and the larger value is, the aging resistance is better.
TABLE 1
| Project | Breaking strength (cN/dtex) | Limiting oxygen index (%) | Aging resistance (%) |
| Example 1 | 3.9 | 32.6 | 99.0 |
| Example 2 | 4.1 | 33.1 | 99.4 |
| Example 3 | 4.4 | 33.8 | 99.6 |
| Example 4 | 4.5 | 34.2 | 99.7 |
| Example 5 | 4.7 | 34.8 | 99.9 |
| Comparative example 1 | 3.1 | 30.1 | 97.3 |
| Comparative example 2 | 3.4 | 29.7 | 96.8 |
As can be seen from Table 1, the reinforced flame retardant recycled polyester fiber disclosed in the examples of the present invention has better breaking strength, aging resistance and flame retardant properties than the comparative example product, and the addition of quinoline yellow and (9 CI) -2-vinyl pyrimidine is beneficial for improving the above properties.
The present invention is not limited to the above-mentioned embodiments, and those skilled in the art can easily implement the present invention as described above, but many equivalent changes, modifications and variations of the present invention can be made by using the above-mentioned disclosed technical matters without departing from the scope of the present invention, and meanwhile, any equivalent changes, modifications and variations of the above-mentioned embodiments according to the essential technology of the present invention are still within the scope of the technical matters of the present invention.
Claims (7)
1. The reinforced flame-retardant regenerated polyester fiber is characterized by comprising, by weight, 100 parts of regenerated polyester, 12-18 parts of a functional copolymer, 1-3 parts of a compatibilizer, 3-5 parts of a coupling agent, 0.6-1.2 parts of an antioxidant, 5-10 parts of nanofibers and 1-3 parts of quinoline yellow, wherein the functional copolymer is prepared from allyl triphenylphosphine bromide, (9 CI) -2-vinyl pyrimidine and methyl methacrylate through a free radical copolymerization reaction, and the preparation method of the functional copolymer comprises the steps of adding the allyl triphenylphosphine bromide, (9) -2-vinyl pyrimidine and methyl methacrylate and an initiator into a high-boiling-point solvent, stirring and reacting for 4-6 hours in an inert gas atmosphere at 60-70 ℃, precipitating in water, washing the precipitated polymer with ethanol for 3-6 times, and finally drying in a vacuum drying box at 85-95 ℃ until the weight to obtain the functional copolymer, wherein the allyl triphenylphosphine bromide, (9) -2-vinyl pyrimidine and methyl acrylate have a constant boiling point ratio of (1.07:2.0:2:0);
the preparation method of the reinforced flame-retardant regenerated polyester fiber comprises the following steps:
Step S1, uniformly mixing other raw materials except quinoline yellow, blending and melting by a screw extruder, spinning and forming the melt by a special-shaped hole spinneret plate, and drawing and forming to obtain functional silk strips;
And S2, soaking the functional yarn prepared in the step S1 in a quinoline yellow solution with the mass percentage concentration of 10-20wt% at 50-60 ℃ for 20-40 hours, taking out and drying to obtain the reinforced flame-retardant regenerated polyester fiber.
2. The reinforced flame-retardant regenerated polyester fiber according to claim 1, wherein the regenerated polyester is produced by sequentially sorting, pulverizing, washing and drying the recovered polyester bottle flakes.
3. The reinforced flame-retardant regenerated polyester fiber according to claim 1, wherein the initiator is azobisisobutyronitrile, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, and N-methylpyrrolidone, and the inert gas is any one of nitrogen, helium, neon, and argon.
4. The reinforced flame-retardant regenerated polyester fiber according to claim 1, wherein the compatibilizer is at least one of PE-g-ST and PE-g-MAH, and the coupling agent is at least one of silane coupling agent KH550, silane coupling agent KH560 and silane coupling agent KH 570.
5. The reinforced flame-retardant regenerated polyester fiber according to claim 1, wherein the antioxidant is at least one of antioxidant 1010, antioxidant 168 and antioxidant 1076, the nanofiber is at least one of a nano boron fiber and a nano carbon fiber, and the average diameter of the nanofiber is 60-100nm, and the length of the nanofiber is 1-5mm.
6. The reinforced flame-retardant regenerated polyester fiber according to claim 1, wherein the spinning temperature of the spinning molding in the step S1 is 240-290 ℃, the spinning speed is 2200-2800m/min, and the temperature of the drafting setting in the step S1 is 60-66 ℃.
7. The reinforced flame retardant recycled polyester fiber of claim 1, wherein the drying in step S2 is at 95-105 ℃ to constant weight.
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