CN114836849A - Antibacterial flame-retardant polyester fiber fabric and preparation method thereof - Google Patents
Antibacterial flame-retardant polyester fiber fabric and preparation method thereof Download PDFInfo
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- CN114836849A CN114836849A CN202210569136.9A CN202210569136A CN114836849A CN 114836849 A CN114836849 A CN 114836849A CN 202210569136 A CN202210569136 A CN 202210569136A CN 114836849 A CN114836849 A CN 114836849A
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- reaction
- stirring
- polyester fiber
- antibacterial flame
- finished
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- 229920000728 polyester Polymers 0.000 title claims abstract description 105
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 88
- 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 84
- 239000003063 flame retardant Substances 0.000 title claims abstract description 84
- 239000000835 fiber Substances 0.000 title claims abstract description 78
- 239000004744 fabric Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title description 3
- 238000003756 stirring Methods 0.000 claims description 123
- 238000006243 chemical reaction Methods 0.000 claims description 84
- 239000007795 chemical reaction product Substances 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 28
- 239000003607 modifier Substances 0.000 claims description 28
- 238000010992 reflux Methods 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 20
- 238000003828 vacuum filtration Methods 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- 239000012065 filter cake Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 18
- 238000001291 vacuum drying Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 238000009987 spinning Methods 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000003963 antioxidant agent Substances 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 14
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- TYMLOMAKGOJONV-UHFFFAOYSA-N 4-nitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1 TYMLOMAKGOJONV-UHFFFAOYSA-N 0.000 claims description 10
- 239000012954 diazonium Substances 0.000 claims description 10
- 150000001989 diazonium salts Chemical class 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000002390 rotary evaporation Methods 0.000 claims description 10
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 9
- 235000010288 sodium nitrite Nutrition 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- VEFLKXRACNJHOV-UHFFFAOYSA-N 1,3-dibromopropane Chemical compound BrCCCBr VEFLKXRACNJHOV-UHFFFAOYSA-N 0.000 claims description 7
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 7
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 6
- 229960001701 chloroform Drugs 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004043 dyeing Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000009941 weaving Methods 0.000 claims description 5
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-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 group 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
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 229940075529 glyceryl stearate Drugs 0.000 claims description 4
- 239000005457 ice water Substances 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
- 239000012074 organic phase Substances 0.000 claims description 4
- 238000004513 sizing Methods 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000007792 addition Methods 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000002699 waste material Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 3
- -1 dyeing Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical class OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229960000686 benzalkonium chloride Drugs 0.000 description 2
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 2
- 125000001246 bromo group Chemical group Br* 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 125000005496 phosphonium group Chemical group 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 229920001817 Agar Polymers 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VBEGHXKAFSLLGE-UHFFFAOYSA-N n-phenylnitramide Chemical compound [O-][N+](=O)NC1=CC=CC=C1 VBEGHXKAFSLLGE-UHFFFAOYSA-N 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000002743 phosphorus functional group Chemical group 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000137 polyphosphoric acid Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 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
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6581—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and nitrogen atoms with or without oxygen or sulfur atoms, as ring hetero atoms
- C07F9/65812—Cyclic phosphazenes [P=N-]n, n>=3
- C07F9/65815—Cyclic phosphazenes [P=N-]n, n>=3 n = 3
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
- D03D15/283—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/50—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04B—KNITTING
- D04B1/00—Weft knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
- D04B1/14—Other fabrics or articles characterised primarily by the use of particular thread materials
- D04B1/16—Other fabrics or articles characterised primarily by the use of particular thread materials synthetic threads
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04B—KNITTING
- D04B21/00—Warp knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
- D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/13—Physical properties anti-allergenic or anti-bacterial
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/66—Disintegrating fibre-containing textile articles to obtain fibres for re-use
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the field of polyester fiber fabrics, and aims to solve the problems of poor antibacterial property and flame retardance of the existing polyester fiber fabrics, in particular to an antibacterial flame-retardant polyester fiber fabric and a preparation method thereof.
Description
Technical Field
The invention relates to the field of polyester fiber fabrics, in particular to an antibacterial flame-retardant polyester fiber fabric and a preparation method thereof.
Background
Polyester is a polymer material with the largest production capacity and the widest application field at present, and because the raw materials for producing the polyester mainly come from petroleum and waste polyester is not naturally degradable and easily causes environmental pollution, the trend of recycling used polyester bottles, waste textiles containing polyester materials and the like is towards the trend. The preparation of the polyester fiber, commonly called as 'terylene', realizes the reasonable reutilization of the waste polyester fiber, improves the resource utilization rate and avoids the pollution to the environment. The raw materials of the regenerated polyester fiber are waste raw materials, the regenerated polyester fiber carries a large amount of bacteria, and the polyester fiber fabric prepared from the polyester fiber is generally more suitable for the reproduction of bacteria and fungi than natural fiber fabric, so that the physical health and normal work, study and life of people are influenced, the limit oxygen index of the polyester fiber is low, and the phenomena of melting and dripping during combustion are very dangerous in fire, so that the development of the antibacterial and flame-retardant multifunctional polyester fiber fabric is very important.
How to improve the antibacterial property and the flame retardance of the existing polyester fiber fabric is the key of the invention, so that the antibacterial flame-retardant polyester fiber fabric and the preparation method thereof are urgently needed to solve the problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide an antibacterial flame-retardant polyester fiber fabric and a preparation method thereof, wherein the antibacterial flame-retardant polyester fiber fabric comprises the following steps: the preparation method comprises the steps of crushing regenerated polyester slices into powder, drying to obtain regenerated polyester powder, adding the regenerated polyester powder, an antibacterial flame-retardant modifier, an antioxidant and a dispersing agent into an extruder for melt extrusion, carrying out spinning molding through a spinning box to obtain antibacterial flame-retardant polyester fibers, carrying out spinning and weaving on the antibacterial flame-retardant polyester fibers to obtain polyester fiber gray fabric, dyeing, finishing, drying, tentering and shaping the polyester fiber gray fabric to obtain the antibacterial flame-retardant polyester fiber fabric, and solving the problems that the existing polyester fiber fabric has antibacterial property and poor flame retardance.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of an antibacterial flame-retardant polyester fiber fabric comprises the following steps:
the method comprises the following steps: weighing 40-50 parts of regenerated polyester chips, 6-18 parts of antibacterial flame-retardant modifier, 2-5 parts of antioxidant and 1.5-3.5 parts of dispersant according to parts by weight for later use;
step two: crushing the recycled polyester chips into powder, and drying to obtain recycled polyester powder;
step three: adding the regenerated polyester powder, the antibacterial flame-retardant modifier, the antioxidant and the dispersing agent into an extruder for melt extrusion, and performing spinning molding through a spinning box to obtain the antibacterial flame-retardant polyester fiber;
step four: spinning and weaving the antibacterial flame-retardant polyester fiber to obtain polyester fiber grey cloth;
step five: and dyeing, finishing, drying, tentering and sizing the polyester fiber grey cloth to obtain the antibacterial flame-retardant polyester fiber fabric.
As a further scheme of the invention: the antioxidant is prepared from antioxidant 1010 and antioxidant 1076 according to a mass ratio of 1: 1-2; the dispersing agent is sodium hexametaphosphate and glyceryl stearate in a mass ratio of 1: 1.
As a further scheme of the invention: the preparation method of the antibacterial flame-retardant modifier comprises the following steps:
a1: adding paranitroaniline and deionized water into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, stirring and dropwise adding concentrated hydrochloric acid under the conditions that the temperature is 20-30 ℃ and the stirring rate is 250-350r/min, controlling the dropwise adding rate to be 1-2 drops/s, continuously stirring until the paranitroaniline is completely dissolved under the condition that the temperature is raised to 70-75 ℃ after the dropwise adding is finished, then adding ammonium thiocyanate, heating to reflux and stirring for reaction for 8-10h, adding a reaction product into distilled water at the temperature of 60-70 ℃ after the reaction is finished, stirring for 3-5min, then carrying out vacuum filtration, placing a filter cake into a vacuum drying box, and drying for 8-10h under the condition that the temperature is 60-70 ℃ to obtain an intermediate 1;
the reaction process is as follows:
a2: adding concentrated sulfuric acid into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, heating to 35-40 ℃ while stirring under the condition that the stirring rate is 250-350r/min, controlling the heating rate to be 2-3 ℃/min, then adding the intermediate 1, continuously stirring for reacting for 40-60min, then dropwise adding hydrobromic acid while stirring, controlling the dropping rate to be 1-2 drops/s, heating to 45-50 ℃ after dropwise adding, continuously stirring for reacting for 4-5h, heating to 60-65 ℃ for continuously stirring for reacting for 4-5h, heating to 80-85 ℃ for continuously stirring for reacting for 4-5h, cooling a reaction product to room temperature after the reaction is finished, then adding the reaction product into ice water, stirring for 20-30min, then carrying out vacuum filtration, placing the filter cake in a vacuum drying oven, and drying for 6-8h at the temperature of 40-60 ℃ to obtain an intermediate 2;
the reaction process is as follows:
a3: adding the intermediate 2, N-dimethylformamide and 5% palladium carbon into a reaction kettle, introducing nitrogen to replace air in the reaction kettle for 2-3 times, then introducing hydrogen under the conditions that the temperature is 95-100 ℃ and the stirring speed is 400-one (r/min), maintaining the pressure in the reaction kettle at 1.5MPa, stirring and reacting for 8-10h, cooling a reaction product to room temperature after the reaction is finished, then rotationally evaporating the reaction product to remove the solvent, and then recrystallizing with anhydrous methanol to obtain an intermediate 3;
the reaction process is as follows:
a4: adding the intermediate 3, hexachlorocyclotriphosphazene, anhydrous potassium carbonate and acetone into a three-neck flask provided with a stirrer, a thermometer and a gas-guide tube, introducing nitrogen for protection, heating to 70-80 ℃ while stirring under the condition that the stirring rate is 250-350r/min, controlling the heating rate to be 2-3 ℃/min, then stirring at constant temperature for 50-60h, cooling the reaction product to 10-15 ℃ after the reaction is finished, then carrying out vacuum filtration, washing the filter cake for 3-5 times by using deionized water, anhydrous ethanol and n-hexane in sequence, then placing the filter cake into a vacuum drying box, and drying for 45-50h under the condition that the temperature is 70-75 ℃ to obtain an intermediate 4;
the reaction process is as follows:
a5: adding the intermediate 4, concentrated sulfuric acid and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring and dropwise adding a sodium nitrite solution under the conditions that the temperature is 0-5 ℃ and the stirring speed is 300-one and 500r/min, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring and reacting for 2-3h after the dropwise adding is finished, adding urea, continuously stirring and reacting for 1-1.5h, and then carrying out vacuum filtration to obtain a diazonium salt solution; adding hydroquinone, distilled water, sodium hydroxide and sodium dodecyl benzene sulfonate into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 20-30min under the conditions that the temperature is 0-5 ℃ and the stirring speed is 250-350r/min, then dropwise adding a diazonium salt solution while stirring, controlling the dropwise adding speed to be 2-3 drops/s, continuously stirring and reacting for 1-2h after the dropwise adding is finished, adjusting the pH of a reaction product to be 7-9 by using concentrated ammonia water after the reaction is finished, then carrying out vacuum filtration, and placing a filter cake in a vacuum drying box to be dried to constant weight to obtain an intermediate 5;
the reaction process is as follows:
a6: adding the intermediate 5, acetone and anhydrous potassium carbonate into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, stirring for 10-15min under the conditions that the temperature is 40-45 ℃ and the stirring speed is 350-550r/min, then heating to reflux and continuing to stir for reaction for 30-50min, then dropwise adding 1, 3-dibromopropane while stirring, controlling the dropwise adding speed to be 1-2 drops/s, continuing to reflux and stir for reaction for 8-10h after the dropwise adding is finished, removing the solvent from the reaction product by rotary evaporation after the reaction is finished, then adding the reaction product into ethyl acetate, washing with distilled water for 2-3 times, standing for layering, drying the organic phase with anhydrous magnesium sulfate, vacuum filtering, and rotary evaporating the filtrate to remove the solvent to obtain an intermediate 6;
the reaction process is as follows:
a7: adding the intermediate 6, triphenylphosphine and chloroform into a three-neck flask provided with a stirrer, a thermometer, a gas-guide tube and a reflux condenser tube, introducing nitrogen for protection, stirring at the stirring speed of 350-550r/min while heating to reflux, stirring at constant temperature for reaction for 10-15h, cooling the reaction product to room temperature after the reaction is finished, performing rotary evaporation on the reaction product after the reaction is finished to remove the solvent, then placing the reaction product in a vacuum drying box, and drying at the temperature of 65-75 ℃ for 30-40h to obtain the antibacterial flame-retardant modifier.
The reaction process is as follows:
as a further scheme of the invention: the dosage ratio of the paranitroaniline, the deionized water, the concentrated hydrochloric acid and the ammonium thiocyanate in the step A1 is 0.1 mol: 30-50 mL: 15-20 mL: 0.11-0.13mol, and the mass fraction of the concentrated hydrochloric acid is 36-38%.
As a further scheme of the invention: the dosage ratio of the concentrated sulfuric acid, the intermediate 1 and the hydrobromic acid in the step A2 is 35-40 g: 10 g: 1.6-2.0g, the mass fraction of the concentrated sulfuric acid is 95-98%, and the mass fraction of the hydrobromic acid is 60-65%.
As a further scheme of the invention: the dosage ratio of the intermediate 2, the N, N-dimethylformamide and the palladium-carbon in the step A3 is 0.1 mol: 100-120 mL: 0.6-1.0 g.
As a further scheme of the invention: the dosage ratio of the intermediate 3, the hexachlorocyclotriphosphazene, the anhydrous potassium carbonate and the acetone in the step A4 is 60 mmol: 10 mmol: 14.5-16.5 g: 150 and 250 mL.
As a further scheme of the invention: the use amount ratio of the intermediate 4, concentrated sulfuric acid, deionized water, sodium nitrite solution, urea, hydroquinone, distilled water, sodium hydroxide and sodium dodecyl benzene sulfonate in the step A5 is 50 mmol: 18-20 g: 40-50 mL: 10-12 mL: 0.15-0.20 g: 0.3 mol: 150-200 mL: 12.5-15.0 g: 0.15-0.25g, and the mass fraction of the sodium nitrite solution is 30%.
As a further scheme of the invention: the using ratio of the intermediate 5, acetone, anhydrous potassium carbonate and 1, 3-dibromopropane in the step A6 is 10 mmol: 150-200 mL: 0.1 mol: 0.12-0.15 mol.
As a further scheme of the invention: the dosage ratio of the intermediate 6, the triphenylphosphine and the trichloromethane in the step A7 is 10 mmol: 0.12-0.15 mol: 150 and 200 mL.
As a further scheme of the invention: the antibacterial flame-retardant polyester fiber fabric is prepared by the preparation method of the antibacterial flame-retardant polyester fiber fabric.
The invention has the beneficial effects that:
the invention relates to an antibacterial flame-retardant polyester fiber fabric and a preparation method thereof.A regenerated polyester slice is crushed into powder, the powder is dried to obtain regenerated polyester powder, the regenerated polyester powder, an antibacterial flame-retardant modifier, an antioxidant and a dispersing agent are added into an extruder to be melted and extruded, the obtained product is spun and formed by a spinning box to obtain antibacterial flame-retardant polyester fiber, the antibacterial flame-retardant polyester fiber is spun and woven to obtain polyester fiber gray fabric, and the polyester fiber gray fabric is dyed, finished, dried, stentered, antibacterial and shaped to obtain the flame-retardant polyester fiber fabric; according to the preparation method, the antibacterial flame-retardant modifier is directly mixed with the regenerated polyester powder to finally prepare fibers, and then the fibers are spun into the fabric, and the fabric is not finished by a finishing agent containing antibacterial flame-retardant property to obtain the antibacterial flame-retardant property;
an antibacterial flame-retardant modifier is also prepared in the process of preparing the antibacterial flame-retardant polyester fiber fabric, firstly, nitroaniline and hydrochloride are firstly formed under the action of hydrochloric acid and ammonium thiocyanate, then, thiourea reaction is carried out to obtain an intermediate 1, then, the intermediate 1 carries out ring-closing reaction by using hydrobromic acid to obtain an intermediate 2, the intermediate 2 reduces nitro to amino through reduction of hydrogen to obtain an intermediate 3, then, the amino on the intermediate 3 and chlorine atoms on hexachlorocyclotriphosphazene carry out nucleophilic substitution reaction, so that the intermediate 3 is connected to a framework containing organic phosphorus nitrogen to obtain an intermediate 4, the intermediate 4 reacts with sodium nitrite to form diazonium salt, then, the diazonium salt and hydroquinone carry out coupling reaction to form an azo compound, a large amount of hydroxyl is introduced to obtain an intermediate 5, then, the hydroxyl on the intermediate 5 and 1, 3-dibromopropane carry out nucleophilic substitution reaction, introducing bromine atoms to obtain an intermediate 6, and then performing nucleophilic substitution reaction on the bromine atoms on the intermediate 6 and triphenylphosphine to generate a large amount of quaternary phosphonium groups to obtain the antibacterial flame-retardant modifier; the molecule of the antibacterial flame-retardant modifier contains a large number of benzene rings and heterocyclic rings, so that the antibacterial flame-retardant modifier is endowed with good high-temperature resistance, the combustion temperature of the polyester fiber fabric is increased, the contained organic phosphorus groups are decomposed to form phosphoric acid and polyphosphoric acid compounds, the dehydration and carbonization of a polymer matrix are promoted, a carbon deposition layer is formed to inhibit the contact of combustible substances and combustible gas, the contained organic nitrogen can be decomposed to release a large number of inert gases to reduce the concentration of the combustible gas when being heated, the contact of the combustible substances and the combustible gas is further inhibited, the flame-retardant effect is achieved, a large number of quaternary phosphonium groups can be adsorbed on the bacterial cell wall with negative charges, the substance in cells is leaked, and the cells are finally killed, the antibacterial effect is achieved, therefore, when the antibacterial flame-retardant modifier is applied to polyester fiber fabrics, the antibacterial performance and the flame retardant performance of the polyester fiber fabrics can be greatly improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the embodiment is a preparation method of an antibacterial flame-retardant modifier, which comprises the following steps:
a1: adding 0.1mol of p-nitroaniline and 30mL of deionized water into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, dropwise adding 15mL of concentrated hydrochloric acid with the mass fraction of 36% while stirring at the temperature of 20 ℃ and the stirring speed of 250r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring until the p-nitroaniline is completely dissolved under the condition of heating to 70 ℃ after the dropwise adding is finished, then adding 0.11mol of ammonium thiocyanate, heating to reflux and stirring for reaction for 8 hours, adding a reaction product into distilled water with the temperature of 60 ℃ after the reaction is finished, stirring for 3 minutes, then carrying out vacuum suction filtration, placing a filter cake into a vacuum drying box, and drying for 8 hours under the temperature of 60 ℃ to obtain an intermediate 1;
a2: adding 35g of 95 mass percent concentrated sulfuric acid into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, heating to 35 ℃ while stirring at a stirring rate of 250r/min, controlling the heating rate to be 2 ℃/min, then adding 10g of the intermediate 1, continuously stirring for reaction for 40min, then dropwise adding 1.6g of 60 mass percent hydrobromic acid while stirring, controlling the dropwise adding rate to be 1 drop/s, continuously stirring for reaction for 4h under the condition of heating to 45 ℃ after dropwise adding, continuously stirring for reaction for 4h under the condition of heating to 60 ℃, continuously stirring for reaction for 4h under the condition of heating to 80 ℃, cooling a reaction product to room temperature after reaction, then adding into ice water, stirring for 20min, then carrying out vacuum filtration, placing a filter cake into a vacuum drying box, drying for 6h under the condition of 40 ℃, obtaining an intermediate 2;
a3: adding 0.1mol of intermediate 2, 100mLN, N-dimethylformamide and 0.6g of 5% palladium carbon into a reaction kettle, introducing nitrogen to replace air in the reaction kettle for 2 times, then introducing hydrogen under the conditions that the temperature is 95 ℃ and the stirring speed is 400r/min, maintaining the pressure in the reaction kettle at 1.5MPa, stirring and reacting for 8 hours, cooling a reaction product to room temperature after the reaction is finished, then rotationally evaporating the reaction product to remove the solvent, and then recrystallizing with anhydrous methanol to obtain an intermediate 3;
a4: adding 60mmol of the intermediate 3, 10mmol of hexachlorocyclotriphosphazene, 14.5g of anhydrous potassium carbonate and 150mL of acetone into a three-neck flask provided with a stirrer, a thermometer and a gas guide tube, introducing nitrogen for protection, heating to 70 ℃ while stirring under the condition that the stirring speed is 250r/min, controlling the heating speed to be 2 ℃/min, then stirring at constant temperature for reaction for 50h, cooling the reaction product to 10 ℃ after the reaction is finished, then carrying out vacuum filtration, washing the filter cake for 3 times by using deionized water, anhydrous ethanol and n-hexane in sequence, then placing the filter cake into a vacuum drying oven, and drying for 45h under the condition that the temperature is 70 ℃ to obtain an intermediate 4;
a5: adding 50mmol of intermediate 4, 18g of concentrated sulfuric acid with the mass fraction of 95% and 40mL of deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, dropwise adding 10mL of sodium nitrite solution with the mass fraction of 30% while stirring at the temperature of 0 ℃ and the stirring speed of 300r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 2 hours after the dropwise adding is finished, then adding 0.15g of urea, continuously stirring and reacting for 1 hour, and then carrying out vacuum filtration to obtain a diazonium salt solution; adding 0.3mol of hydroquinone, 150mL of distilled water, 12.5g of sodium hydroxide and 0.15g of sodium dodecyl benzene sulfonate into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 20min at the temperature of 0 ℃ and the stirring speed of 250r/min, then dropwise adding a diazonium salt solution while stirring, controlling the dropwise adding speed to be 2 drops/s, continuously stirring and reacting for 1h after the dropwise adding is finished, adjusting the pH of a reaction product to be 7 by using 22% concentrated ammonia water after the reaction is finished, then carrying out vacuum filtration, and placing a filter cake in a vacuum drying oven to be dried to constant weight to obtain an intermediate 5;
a6: adding 10mmol of intermediate 5, 150mL of acetone and 0.1mol of anhydrous potassium carbonate into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser and a constant-pressure dropping funnel, stirring for 10min at the temperature of 40 ℃ and the stirring rate of 350r/min, heating to reflux, continuing to stir for reaction for 30min, dropwise adding 0.12mol of 1, 3-dibromopropane while stirring, controlling the dropwise adding rate to be 1 drop/s, continuing to reflux and stir for reaction for 8h after the dropwise adding is finished, removing the solvent by rotary evaporation of a reaction product after the reaction is finished, then adding the reaction product into ethyl acetate, washing for 2 times with distilled water, standing for layering, drying an organic phase with anhydrous magnesium sulfate, then carrying out vacuum filtration, and removing the solvent by rotary evaporation of a filtrate to obtain an intermediate 6;
a7: adding 10mmol of intermediate 6, 0.12mol of triphenylphosphine and 150mL of trichloromethane into a three-neck flask provided with a stirrer, a thermometer, a gas guide tube and a reflux condenser tube, introducing nitrogen for protection, heating to reflux while stirring at a stirring speed of 350r/min, stirring at a constant temperature for reaction for 10 hours, cooling a reaction product to room temperature after the reaction is finished, performing rotary evaporation on the reaction product after the reaction is finished to remove a solvent, then placing the reaction product in a vacuum drying box, and drying at the temperature of 65 ℃ for 30 hours to obtain the antibacterial flame-retardant modifier.
Example 2:
the embodiment is a preparation method of an antibacterial flame-retardant modifier, which comprises the following steps:
a1: adding 0.1mol of p-nitroaniline and 50mL of deionized water into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, dropwise adding 20mL of concentrated hydrochloric acid with the mass fraction of 38% while stirring at the temperature of 30 ℃ and the stirring speed of 350r/min, controlling the dropwise adding speed to be 2 drops/s, continuously stirring until the p-nitroaniline is completely dissolved under the condition of heating to 75 ℃ after the dropwise adding is finished, then adding 0.13mol of ammonium thiocyanate, heating to reflux and stirring for reaction for 10 hours, adding a reaction product into distilled water with the temperature of 70 ℃ after the reaction is finished, stirring for 5 minutes, then carrying out vacuum suction filtration, placing a filter cake into a vacuum drying box, and drying for 10 hours at the temperature of 70 ℃ to obtain an intermediate 1;
a2: adding 40g of 98% concentrated sulfuric acid into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, heating to 40 ℃ while stirring at a stirring rate of 350r/min, controlling the heating rate to be 3 ℃/min, then adding 10g of the intermediate 1, continuously stirring for reaction for 60min, then dropwise adding 2.0g of 65% hydrobromic acid while stirring, controlling the dropwise adding rate to be 2 drops/s, continuously stirring for reaction for 5h under the condition of heating to 50 ℃ after dropwise adding, continuously stirring for reaction for 5h under the condition of heating to 65 ℃, continuously stirring for reaction for 5h under the condition of heating to 85 ℃, cooling a reaction product to room temperature after reaction, then adding ice water into the mixture, stirring for 30min, then carrying out vacuum filtration, placing a filter cake into a vacuum drying oven, drying for 8h at the temperature of 60 ℃, obtaining an intermediate 2;
a3: adding 0.1mol of intermediate 2, 120mLN, N-dimethylformamide and 1.0g of 5% palladium carbon into a reaction kettle, introducing nitrogen to replace air in the reaction kettle for 3 times, then introducing hydrogen under the conditions that the temperature is 100 ℃ and the stirring speed is 600r/min, maintaining the pressure in the reaction kettle at 1.5MPa, stirring and reacting for 10 hours, cooling a reaction product to room temperature after the reaction is finished, then rotationally evaporating the reaction product to remove the solvent, and then recrystallizing with anhydrous methanol to obtain an intermediate 3;
a4: adding 60mmol of intermediate 3, 10mmol of hexachlorocyclotriphosphazene, 16.5g of anhydrous potassium carbonate and 250mL of acetone into a three-neck flask provided with a stirrer, a thermometer and a gas guide tube, introducing nitrogen for protection, heating to 80 ℃ while stirring under the condition that the stirring speed is 350r/min, controlling the heating speed to be 3 ℃/min, then stirring at constant temperature for reaction for 60 hours, cooling the reaction product to 15 ℃ after the reaction is finished, then carrying out vacuum filtration, washing the filter cake for 5 times by using deionized water, anhydrous ethanol and n-hexane in sequence, then placing the filter cake into a vacuum drying oven, and drying for 50 hours under the condition that the temperature is 75 ℃ to obtain an intermediate 4;
a5: adding 50mmol of intermediate 4, 20g of 98% concentrated sulfuric acid and 50mL of deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, dropwise adding 12mL of 30% sodium nitrite solution while stirring at the temperature of 5 ℃ and the stirring speed of 500r/min, controlling the dropwise adding speed to be 2 drops/s, continuously stirring and reacting for 3 hours after the dropwise adding is finished, then adding 0.20g of urea, continuously stirring and reacting for 1.5 hours, and then carrying out vacuum filtration to obtain a diazonium salt solution; adding 0.3mol of hydroquinone, 200mL of distilled water, 15.0g of sodium hydroxide and 0.25g of sodium dodecyl benzene sulfonate into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 30min at the temperature of 5 ℃ and the stirring speed of 350r/min, then dropwise adding a diazonium salt solution while stirring, controlling the dropwise adding speed to be 3 drops/s, continuously stirring and reacting for 2h after the dropwise adding is finished, adjusting the pH of a reaction product to be 9 by using 22% concentrated ammonia water after the reaction is finished, then carrying out vacuum filtration, and placing a filter cake in a vacuum drying oven to be dried to constant weight to obtain an intermediate 5;
a6: adding 10mmol of intermediate 5, 200mL of acetone and 0.1mol of anhydrous potassium carbonate into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser and a constant-pressure dropping funnel, stirring at the temperature of 45 ℃ and the stirring rate of 550r/min for 15min, heating to reflux, continuing to stir for reaction for 50min, dropwise adding 0.15mol of 1, 3-dibromopropane while stirring, controlling the dropwise adding rate to be 2 drops/s, continuing to reflux and stir for reaction for 10h after the dropwise adding is finished, removing the solvent by rotary evaporation of a reaction product after the reaction is finished, then adding the reaction product into ethyl acetate, washing the ethyl acetate with distilled water for 3 times, standing for layering, drying an organic phase with anhydrous magnesium sulfate, then carrying out vacuum filtration, and removing the solvent by rotary evaporation of a filtrate to obtain an intermediate 6;
a7: adding 10mmol of intermediate 6, 0.15mol of triphenylphosphine and 200mL of trichloromethane into a three-neck flask provided with a stirrer, a thermometer, a gas guide tube and a reflux condenser tube, introducing nitrogen for protection, heating to reflux while stirring at a stirring speed of 550r/min, stirring at a constant temperature for reaction for 15 hours, cooling a reaction product to room temperature after the reaction is finished, performing rotary evaporation on the reaction product after the reaction is finished to remove a solvent, then placing the reaction product in a vacuum drying box, and drying at the temperature of 75 ℃ for 40 hours to obtain the antibacterial flame-retardant modifier.
Example 3:
the embodiment is a preparation method of an antibacterial flame-retardant polyester fiber fabric, which comprises the following steps:
the method comprises the following steps: weighing 40 parts of regenerated polyester chips, 6 parts of antibacterial flame-retardant modifier from example 1, 2 parts of antioxidant and 1.5 parts of dispersant according to parts by weight for later use; the antioxidant is prepared from antioxidant 1010 and antioxidant 1076 according to a mass ratio of 1: 1; the dispersing agent is sodium hexametaphosphate and glyceryl stearate in a mass ratio of 1: 1;
step two: crushing the recycled polyester chips into powder, and drying to obtain recycled polyester powder;
step three: adding the regenerated polyester powder, the antibacterial flame-retardant modifier, the antioxidant and the dispersing agent into an extruder for melt extrusion, and performing spinning molding through a spinning box to obtain the antibacterial flame-retardant polyester fiber;
step four: spinning and weaving the antibacterial flame-retardant polyester fiber to obtain polyester fiber grey cloth;
step five: and dyeing, finishing, drying, tentering and sizing the polyester fiber grey cloth to obtain the antibacterial flame-retardant polyester fiber fabric.
Example 4:
the embodiment is a preparation method of an antibacterial flame-retardant polyester fiber fabric, which comprises the following steps:
the method comprises the following steps: weighing 50 parts of regenerated polyester chips, 18 parts of antibacterial flame-retardant modifier from example 2, 5 parts of antioxidant and 3.5 parts of dispersant according to parts by weight for later use; the antioxidant is prepared from antioxidant 1010 and antioxidant 1076 according to a mass ratio of 1: 2; the dispersing agent is sodium hexametaphosphate and glyceryl stearate in a mass ratio of 1: 1;
step two: crushing the recycled polyester chips into powder, and drying to obtain recycled polyester powder;
step three: adding the regenerated polyester powder, the antibacterial flame-retardant modifier, the antioxidant and the dispersing agent into an extruder for melt extrusion, and performing spinning molding through a spinning box to obtain the antibacterial flame-retardant polyester fiber;
step four: spinning and weaving the antibacterial flame-retardant polyester fiber to obtain polyester fiber grey cloth;
step five: and dyeing, finishing, drying, tentering and sizing the polyester fiber grey cloth to obtain the antibacterial flame-retardant polyester fiber fabric.
Comparative example 1:
comparative example 1 differs from example 4 in that no antibacterial flame retardant modifier is added.
Comparative example 2:
comparative example 2 differs from example 4 in that a mixture of benzalkonium chloride antibacterial agent and aluminum hydroxide flame retardant in equal mass ratio is used instead of the antibacterial flame retardant modifier.
Comparative example 3:
comparative example 3 is the antibacterial flame-retardant polyester fabric prepared according to example 3 of the application number CN202010782353.7 and the preparation method thereof.
The flame retardant performance of the antibacterial flame-retardant polyester fiber fabrics in examples 3-4 and comparative examples 1-3 is tested according to GB/T5454-1997 textile flame performance test oxygen index method, the antibacterial performance of the antibacterial flame-retardant polyester fiber fabrics in examples 3-4 and comparative examples 1-3 is tested according to the agar plate diffusion method in GB/T20944.1-2007 first part of evaluation of textile antibacterial performance, and the antibacterial rates of escherichia coli and staphylococcus aureus are calculated, and the results are shown in the following table:
referring to the data in the table, according to the comparison between the example and the comparative example 1, it can be known that the flame retardant and antibacterial performance of the polyester fiber fabric can be obviously improved by adding the antibacterial flame retardant modifier, according to the comparison between the example and the comparative example 2, it can be known that the flame retardant and antibacterial performance of the polyester fiber fabric can also be improved by the mixture of benzalkonium chloride and aluminum hydroxide, but the effect is far inferior to that of the antibacterial flame retardant modifier in the application, and according to the comparison between the example and the comparative example 3, it can be known that the flame retardant and antibacterial performance of the polyester fiber fabric in the application is higher than that of the antibacterial flame retardant polyester fabric in the prior art, and the performance is better.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The preparation method of the antibacterial flame-retardant polyester fiber fabric is characterized by comprising the following steps of:
the method comprises the following steps: weighing 40-50 parts of regenerated polyester chips, 6-18 parts of antibacterial flame-retardant modifier, 2-5 parts of antioxidant and 1.5-3.5 parts of dispersant according to parts by weight for later use;
step two: crushing the recycled polyester chips into powder, and drying to obtain recycled polyester powder;
step three: adding the regenerated polyester powder, the antibacterial flame-retardant modifier, the antioxidant and the dispersing agent into an extruder for melt extrusion, and performing spinning molding through a spinning box to obtain the antibacterial flame-retardant polyester fiber;
step four: spinning and weaving the antibacterial flame-retardant polyester fiber to obtain polyester fiber grey cloth;
step five: and dyeing, finishing, drying, tentering and sizing the polyester fiber grey cloth to obtain the antibacterial flame-retardant polyester fiber fabric.
2. The preparation method of the antibacterial flame-retardant polyester fiber fabric according to claim 1, wherein the antioxidant is an antioxidant 1010 and an antioxidant 1076 in a mass ratio of 1: 1-2; the dispersing agent is sodium hexametaphosphate and glyceryl stearate in a mass ratio of 1: 1.
3. The preparation method of the antibacterial flame-retardant polyester fiber fabric according to claim 1, wherein the preparation method of the antibacterial flame-retardant modifier comprises the following steps:
a1: adding p-nitroaniline and deionized water into a four-neck flask, dropwise adding concentrated hydrochloric acid while stirring, heating after dropwise adding, continuously stirring until the p-nitroaniline is completely dissolved, then adding ammonium thiocyanate, heating to reflux, stirring for reaction, adding a reaction product into distilled water after reaction is finished, then performing vacuum filtration, and drying a filter cake to obtain an intermediate 1;
a2: adding concentrated sulfuric acid into a three-neck flask, stirring, adding the intermediate 1, continuously stirring for reaction, dropwise adding hydrobromic acid while stirring, heating after dropwise adding, continuously stirring for reaction, cooling a reaction product to room temperature after the reaction is finished, adding the reaction product into ice water, performing vacuum filtration, and drying a filter cake to obtain an intermediate 2;
a3: adding the intermediate 2, N-dimethylformamide and 5% palladium carbon into a reaction kettle, introducing nitrogen to replace air in the reaction kettle, then introducing hydrogen and stirring for reaction, cooling a reaction product to room temperature after the reaction is finished, and then performing rotary evaporation and recrystallization to obtain an intermediate 3;
a4: adding the intermediate 3, hexachlorocyclotriphosphazene, anhydrous potassium carbonate and acetone into a three-neck flask, stirring for reaction, cooling a reaction product after the reaction is finished, then carrying out vacuum filtration, washing a filter cake, and drying to obtain an intermediate 4;
a5: adding the intermediate 4, concentrated sulfuric acid and deionized water into a three-neck flask, dropwise adding a sodium nitrite solution while stirring, continuously stirring for reaction after dropwise adding is finished, then adding urea for continuous stirring for reaction, and then carrying out vacuum filtration to obtain a diazonium salt solution; adding hydroquinone, distilled water, sodium hydroxide and sodium dodecyl benzene sulfonate into a three-neck flask, stirring, dropwise adding a diazonium salt solution while stirring, continuously stirring for reaction after dropwise adding is finished, adjusting the pH of a reaction product with concentrated ammonia water after the reaction is finished, then performing vacuum filtration, and drying a filter cake to obtain an intermediate 5;
a6: adding the intermediate 5, acetone and anhydrous potassium carbonate into a four-neck flask, stirring, heating to reflux, continuously stirring for reaction, dropwise adding 1, 3-dibromopropane while stirring, continuously refluxing and stirring for reaction after the dropwise addition is finished, performing rotary evaporation on a reaction product after the reaction is finished, adding the reaction product into ethyl acetate, washing with distilled water, standing for layering, and drying an organic phase to obtain an intermediate 6;
a7: adding the intermediate 6, triphenylphosphine and trichloromethane into a three-neck flask, heating to reflux while stirring, stirring at constant temperature for reaction, cooling a reaction product to room temperature after the reaction is finished, rotationally evaporating the reaction product after the reaction is finished, and drying to obtain the antibacterial flame-retardant modifier.
4. The preparation method of the antibacterial flame-retardant polyester fiber fabric according to claim 3, wherein the dosage ratio of the paranitroaniline, the deionized water, the concentrated hydrochloric acid and the ammonium thiocyanate in the step A1 is 0.1 mol: 30-50 mL: 15-20 mL: 0.11-0.13mol, wherein the mass fraction of the concentrated hydrochloric acid is 36-38%; the dosage ratio of the concentrated sulfuric acid, the intermediate 1 and the hydrobromic acid in the step A2 is 35-40 g: 10 g: 1.6-2.0g, the mass fraction of the concentrated sulfuric acid is 95-98%, and the mass fraction of the hydrobromic acid is 60-65%.
5. The preparation method of the antibacterial flame-retardant polyester fiber fabric according to claim 3, wherein the using amount ratio of the intermediate 2, N-dimethylformamide and palladium carbon in the step A3 is 0.1 mol: 100-120 mL: 0.6-1.0 g; the dosage ratio of the intermediate 3, the hexachlorocyclotriphosphazene, the anhydrous potassium carbonate and the acetone in the step A4 is 60 mmol: 10 mmol: 14.5-16.5 g: 150 and 250 mL.
6. The preparation method of the antibacterial flame-retardant polyester fiber fabric according to claim 3, wherein the dosage ratio of the intermediate 4, concentrated sulfuric acid, deionized water, sodium nitrite solution, urea, hydroquinone, distilled water, sodium hydroxide and sodium dodecyl benzene sulfonate in the step A5 is 50 mmol: 18-20 g: 40-50 mL: 10-12 mL: 0.15-0.20 g: 0.3 mol: 150-200 mL: 12.5-15.0 g: 0.15-0.25g, wherein the mass fraction of the sodium nitrite solution is 30%; the using ratio of the intermediate 5, acetone, anhydrous potassium carbonate and 1, 3-dibromopropane in the step A6 is 10 mmol: 150-200 mL: 0.1 mol: 0.12-0.15 mol.
7. The preparation method of the antibacterial flame-retardant polyester fiber fabric according to claim 3, wherein the dosage ratio of the intermediate 6, triphenylphosphine and chloroform in the step A7 is 10 mmol: 0.12-0.15 mol: 150 and 200 mL.
8. The antibacterial flame-retardant polyester fiber fabric is characterized in that the antibacterial flame-retardant polyester fiber fabric is prepared by the preparation method of the antibacterial flame-retardant polyester fiber fabric according to any one of claims 1 to 7.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819305A (en) * | 2022-10-09 | 2023-03-21 | 浙江迪邦化工有限公司 | Continuous preparation process of p-nitrophenylthiourea |
| CN115928291A (en) * | 2023-02-21 | 2023-04-07 | 无锡市泛博纺织有限公司 | Antibacterial flame-retardant suede, preparation method and application thereof in automotive interior |
| CN117431680A (en) * | 2023-11-27 | 2024-01-23 | 潮州市苏菲亚时装有限公司 | Preparation method of light and thin breathable fabric |
| CN115819305B (en) * | 2022-10-09 | 2024-06-07 | 浙江迪邦化工有限公司 | Continuous preparation process of p-nitrophenyl thiourea |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819305A (en) * | 2022-10-09 | 2023-03-21 | 浙江迪邦化工有限公司 | Continuous preparation process of p-nitrophenylthiourea |
| CN115819305B (en) * | 2022-10-09 | 2024-06-07 | 浙江迪邦化工有限公司 | Continuous preparation process of p-nitrophenyl thiourea |
| CN115928291A (en) * | 2023-02-21 | 2023-04-07 | 无锡市泛博纺织有限公司 | Antibacterial flame-retardant suede, preparation method and application thereof in automotive interior |
| CN117431680A (en) * | 2023-11-27 | 2024-01-23 | 潮州市苏菲亚时装有限公司 | Preparation method of light and thin breathable fabric |
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