CN105544219A - Method for modifying polyester fiber through polyethylene glycol grafted chitosan - Google Patents
Method for modifying polyester fiber through polyethylene glycol grafted chitosan Download PDFInfo
- Publication number
- CN105544219A CN105544219A CN201610048110.4A CN201610048110A CN105544219A CN 105544219 A CN105544219 A CN 105544219A CN 201610048110 A CN201610048110 A CN 201610048110A CN 105544219 A CN105544219 A CN 105544219A
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- CN
- China
- Prior art keywords
- polyethylene glycol
- polyster fibre
- grafted chitosan
- glycol grafted
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000000835 fiber Substances 0.000 title claims abstract description 166
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 89
- 239000002202 Polyethylene glycol Substances 0.000 title claims abstract description 75
- 229920001223 polyethylene glycol Polymers 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 44
- 229920000728 polyester Polymers 0.000 title claims abstract description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 66
- 238000006243 chemical reaction Methods 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 43
- 230000008569 process Effects 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 69
- 238000003756 stirring Methods 0.000 claims description 68
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 52
- 238000002156 mixing Methods 0.000 claims description 50
- 238000012986 modification Methods 0.000 claims description 33
- 230000004048 modification Effects 0.000 claims description 33
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 20
- 229940093430 polyethylene glycol 1500 Drugs 0.000 claims description 13
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 10
- 229960004132 diethyl ether Drugs 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- LGRFSURHDFAFJT-UHFFFAOYSA-N phthalic anhydride Chemical class C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 9
- 239000004480 active ingredient Substances 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 239000004744 fabric Substances 0.000 abstract description 23
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000004753 textile Substances 0.000 abstract description 5
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 230000009435 amidation Effects 0.000 abstract 2
- 238000007112 amidation reaction Methods 0.000 abstract 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 30
- 229920004933 Terylene® Polymers 0.000 description 16
- 229920004934 Dacron® Polymers 0.000 description 14
- -1 but Substances 0.000 description 8
- 230000000845 anti-microbial effect Effects 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 230000010148 water-pollination Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 125000002252 acyl group Chemical group 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000003115 biocidal effect Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 238000007788 roughening Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 2
- 235000019636 bitter flavor Nutrition 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- YRIZYWQGELRKNT-UHFFFAOYSA-N 1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O YRIZYWQGELRKNT-UHFFFAOYSA-N 0.000 description 1
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 108010022172 Chitinases Proteins 0.000 description 1
- 102000012286 Chitinases Human genes 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- FSNCEEGOMTYXKY-JTQLQIEISA-N Lycoperodine 1 Natural products N1C2=CC=CC=C2C2=C1CN[C@H](C(=O)O)C2 FSNCEEGOMTYXKY-JTQLQIEISA-N 0.000 description 1
- JHXVRRJXCDAINK-UHFFFAOYSA-N NC(=O)N.N#CC#N Chemical compound NC(=O)N.N#CC#N JHXVRRJXCDAINK-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000003542 behavioural effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 1
- 108010089934 carbohydrase Proteins 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000000490 cosmetic additive Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000004715 keto acids Chemical class 0.000 description 1
- 239000002650 laminated plastic Substances 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000575 pesticide 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
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000010415 tidying Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012549 training Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Materials Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a method for modifying polyester fiber through polyethylene glycol grafted chitosan, and belongs to the technical field of textile chemicals. The method comprises the process of pretreating the polyester fiber, the process of preparing a polyethylene glycol grafted chitosan derivative and the process of modifying the polyester fiber through the polyethylene glycol grafted chitosan. After the polyester fiber is modified through a sodium hydroxide solution, the fiber surface is roughed, adhesion of the chitosan derivative in the later period is facilitated, cyanuric acid is added for modifying amidation chitosan to obtain cyanuric acid modified amidation chitosan, the modified chitosan can better have a grafting reaction with polyethylene glycol, the flexibility and hydrophilic performance are more excellent, the modified chitosan can carry out grafting and adsorption on polyester fiber to improve the hydrophilic performance and anti-static performance of polyester molecules, the hand feel of a polyester fiber fabric is improved to a certain degree, the polyester fiber fabric has the certain antibacterial performance, and meanwhile the polyester fiber fabric is firm in grafting, good in water resistance, high in economic benefit and wide in industrial popularization prospect.
Description
Technical field:
The invention discloses a kind of method of polyethylene glycol grafted chitosan modified polyester fibre, belong to technical field of textile chemical engineering.
Background technology:
Terylene is the trade name of dacron fibre, is one of the large main force of three in synthetic fiber fiber.Because terylene linear macromolecule is symmetry benzene ring structure, good linearity and molecular chain structure stereoregular, it is had, and intensity is high, good springiness and the rigidity superior physical and mechanical properties such as large, and weak acid, alkali are stablized, there is excellent DIMENSIONAL STABILITY and good corrosion resistance, it is a kind of ideal textile fabric, but, terylene is a kind of typical hydrophobic fibre, only respectively there is a hydroxyl at its molecule two ends, and without other hydrophilic radical, molecular structure is close-packed arrays, degree of crystallinity is high, and hygroscopicity is poor.In normal conditions (20 DEG C of relative humidity 65%), the hydroscopicity of terylene only has about 0.4% (cotton 7-8%, polyamide fibre 4%, acrylic fibers 1-2%), and under the condition of 100% relative humidity, hydroscopicity is also only 0.6-0.8%.Therefore its hygroscopicity poor, easily produce electrostatic, easily stain, affect its snugness of fit.
Hydrophilic finiss, is referred to as water suction (or absorbing sweat) at first and arranges, and is to be suggested for the advanced motion clothes based on dacron or training clothes.Endowing terylene fiber or fabric hydrophilic mainly contain two kinds of methods: one is spinning modification: in the spinning process of fiber, utilize the synthetic technology of fiber to carry out modification to Structure of PET Fiber, make polyster fibre itself have hydrophilicity, thus improve the wearability of terylene; The method process routes relative complex, operability is more weak.Two is arrange modification: mostly at fiber surface modification, utilize dacron afterfinish technology and reach modification object.Namely on terylene macromolecular chain, introduce hydrophilic radical, make fabric face form hydrophilic layer, thus change fiber surface performance.
Shitosan is the product after chitin removes acetyl group, there is amino and hydroxyl in molecular structure, can be dissolved in dilute acid solution, has good water-disintegrable, gas permeability and antibiotic property, the characteristic that biologically active etc. are excellent.Comprehensively can improve the performance of fabric with chitosan finishing dacron, in chitosan finishing liquid, add catalyst and crosslinking agent, its adsorption rate can be increased, and improve its water-fastness ability.
With shitosan, hydrophilic finiss is carried out for dacron; common way first dacron is carried out alkali treatment; fiber surface roughening can be made on the one hand; be conducive to the attachment of chitosan coat; be intended on the other hand hydrolysis is to a certain degree occurred the acyl group in surperficial terylene molecular fiber and produces the carboxyl anion of some, be convenient to the combination of positive chitosan molecule and polyster fibre.Polyethylene glycol can be dissolved in water and many solvents, dissolubility is good and do not have toxic and side effect, having good biocompatibility, is a kind of high polymer long chain of flexibility, can change the flexible and toughness of softness that high molecular structure two compiles with other macromolecules after being combined.
In research in new high-tech and development plan have been listed shitosan by China, the shitosan of high molecular has very strong hydrogen bond and crystal structure closely, be insoluble to common solvent, can only dissolve in acid medium, and low-molecular-weight shitosan be water-soluble, at present, method about degradation of chitosan mainly contains three kinds, physical degradation methods: high-energy ray, ultrasonic wave, light etc., chemical degradation method: hydrogen peroxide, concentrated hydrochloric acid, and potassium permanganate; Enzymolysis edman degradation Edman: chitinase, chitosan enzyme and non-specific carbohydrase etc.
The people such as Dai Jie disclose the article of a section " polyethylene glycol grafted chitosan is on impact of dacron performance " by name in the 43rd volume the 9th phase of " synthetic fiber " impurity in 2014, take shitosan as raw material, 2 bit aminos are closed by phthalic anhydride, utilize cyanuric trichloride to be introduced on polyglycol chain by 6 of shitosan hydroxyls, obtain water-soluble good chitosan derivatives.With this finishing agent, dacron is processed, finishing agent mass concentration be 8g/L, the time of baking is 5 minutes, baking temperature is 120 DEG C time, dacron has good mechanical property, hydrophilicity and antistatic property, of the present invention closest to prior art, but this technology is the finishing agent adopting polyethylene glycol grafted chitosan to obtain carries out last phase tidying up to dacron, preparation process time is of a specified duration, technological process is complicated, and the hydrophily of dacron after arranging and the resistance to water of resistance to voltage not good, be unfavorable for suitability for industrialized production.
Summary of the invention:
The object of the invention is to for the deficiencies in the prior art, a kind of method of polyethylene glycol grafted chitosan modified polyester fibre is provided, pass through chemical modification, continue to be connected with polyster fibre molecule after polyethylene glycol grafted chitosan, improve hydrophilicity and the antistatic property of terylene molecule, also have some improvement to the feel of polyster fibre and anti-microbial property, its grafting is simultaneously firm, water-tolerant; This polyster fibre is directly carried out textile applications, requires no the arrangement in later stage, there is higher economic benefit and application and popularization value.
The invention provides following technical scheme:
A method for polyethylene glycol grafted chitosan modified polyester fibre, comprises the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1-1.5 hour under 50-55 DEG C of temperature conditions of 20-22% by polyster fibre mass fraction, mechanical agitation speed is 100-150 rev/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:30-40; After preliminary treatment, polyster fibre is drained and use cold water flush again and 20-30 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 50-55 DEG C of heating condition, add 20 milliliters of phthalic anhydrides again, at 135 DEG C, react 6-7 hour, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:3-5 mixing, 30 DEG C of heating stirring reaction 10-15 hour, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 7-10 times of insoluble matter solid, staticly settles after stirring 2-3 hour at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5-7 according to amount of substance, add mixed weight 20-25 toluene solution doubly, stirring reaction 8-10 hour at 60-80 DEG C of temperature, mixing speed is 20-30 rev/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:20-25; be warming up to 120-150 DEG C; mechanic whirl-nett reaction 3-5 hour; mixing speed is 200-300 rev/min; stirring reaction terminates the calcium chloride solution of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 80-100 DEG C of stirring reaction 1-2 hour; mixing speed is 400-600 rev/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 80-90 DEG C of oven dry 2-3 time through cold water flush.
Preferably, described active constituent content >=97% preparing cyanuric acid in polyethylene glycol grafted chitosan derivative, its addition is in cyanuric acid active ingredient.
Preferably, in described polyethylene glycol grafted chitosan modified polyester fibre, the mass concentration of calcium chloride solution is 10-15%.
Preferably, be sodium hydroxide solution stir process 1.5 hours under 55 DEG C of temperature conditions of 20% by polyster fibre mass fraction in the described first step, mechanical agitation speed is 120 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:35-40; After preliminary treatment, polyster fibre is drained and use cold water flush again and 20-30 DEG C of oven dry, obtain preliminary treatment polyster fibre.
Preferably, in described second step by amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:4 mixing, 30 DEG C are heated stirring reaction 12 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 8 times of insoluble matter solid, stirs after 3 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan.
Preferably, cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5 according to amount of substance in described second step, add the toluene solution of mixed weight 20 times, stirring reaction 10 hours at 60-80 DEG C of temperature, mixing speed is 20-30 rev/min.
Preferably, preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution in described 3rd step; bath raio is 1:20; be warming up to 140 DEG C; mechanic whirl-nett reaction 5 hours; mixing speed is 200 revs/min; stirring reaction terminates the calcium chloride solution of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 100 DEG C of stirring reactions 1 hour; mixing speed is 400 revs/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 90 DEG C of oven dry 2-3 time through cold water flush.
Dacron is carried out alkali treatment; fiber surface roughening can be made on the one hand; be conducive to the attachment of chitosan coat; be intended on the other hand hydrolysis is to a certain degree occurred the acyl group in surperficial terylene molecular fiber and produces the carboxyl anion of some, be convenient to the combination of positive chitosan molecule and polyster fibre.
Cyanuric acid, has another name called cyanuric acid, white crystals, separate out from water, be with two crystallizations water, mildly bitter flavor, substantially nontoxic, can hot water be dissolved in, be slightly soluble in cold water, the aqueous solution is in acid, the aqueous solution of potassium hydroxide and NaOH can be dissolved in, be insoluble to the organic solvents such as cold alcohol, ether, benzene, there are two kinds of isomers, i.e. keto-acid and enol-type structure, normally exists with the mixture of two kinds of isomers.Cyanuric acid is mainly used in synthesizing chlorinated derivative, salt, lipid, TCCA, DCCNa or potassium; For the synthesis of cyanogen urea acid-formaldehyde resin, epoxy resin, antioxidant, coating, paint, adhesive, pesticide herbicide, metal cyanide corrosion inhibiter, polymer modification agent etc.; For production, the synthesizing new bleaching agent of medicine halotrizinol; Can be used for swimming pool chlorine stabilizing agent, sterilization, decontamination; Also can be directly used in nylon, Sai Ke, raw materials for production etc. such as combustion agent and cosmetic additive agent, laminated plastic and high temp glass steel etc.The present invention adopts cyanuric acid to carry out modification to amidatioon shitosan, improve the extent of polymerization of shitosan and polyethylene glycol, and adsorptivity and the compatibility of shitosan can be improved, after polyethylene glycol grafted chitosan derivative is mixed with pretreated polyster fibre modification, hydrophilic radical is incorporated in polyster fibre macromolecular chain, and connect closely, water-tolerant, for improving hydrophily and the flexibility of polyster fibre, chitosan molecule also has good anti-microbial property simultaneously, can the good anti-microbial property of endowing terylene fabric, increase economic efficiency.
Polyethylene glycol 1500 outward appearance be oyster white ancient costume without, hydroxyl value is 68-83mgKO hour/g, and molecular weight is 1350-1650, moisture≤1.0%, and the p one hour value of 1% aqueous solution is 5.0-7.0.Polyethylene glycol product is nontoxic, nonirritant, mildly bitter flavor, have good water-soluble, and have good intermiscibility with many organic matter components, there are excellent lubricity, moisture retention, dispersiveness, bonding agent, antistatic additive and softener etc., all have in the industries such as cosmetics, pharmacy, chemical fibre, rubber, plastics, papermaking, paint, plating, agricultural chemicals, intermetallic composite coating and food processing and apply very widely.The present invention adopts polyethylene glycol 1500 and modified shitosan to carry out grafting process, obtains polyethylene glycol grafted chitosan, then carries out modification with polyethylene glycol grafted chitosan to polyster fibre, improves the hydrophilicity of polyster fibre.
Beneficial effect of the present invention:
1. the present invention optimizes the Project on Pre of dacron; fiber surface roughening can be made on the one hand; be conducive to the attachment of chitosan coat; be there is hydrolysis to a certain degree in the acyl group in surperficial terylene molecular fiber on the other hand and produce the carboxyl anion of some, being convenient to the combination of positive chitosan molecule and polyster fibre.
2. the present invention adopts cyanuric acid to carry out modification to amidatioon shitosan, improve the extent of polymerization of shitosan and polyethylene glycol, and adsorptivity and the compatibility of shitosan can be improved, after polyethylene glycol grafted chitosan derivative is mixed with pretreated polyster fibre modification, hydrophilic radical is incorporated in polyster fibre macromolecular chain, and connect closely, water-tolerant, for improving hydrophily and the flexibility of polyster fibre, simultaneously chitosan molecule also has good anti-microbial property, can the certain anti-microbial property of endowing terylene fabric.
3. the present invention adopts polyethylene glycol 1500 and modified shitosan to carry out grafting process, obtains polyethylene glycol grafted chitosan, then carries out modification with polyethylene glycol grafted chitosan to polyster fibre, improves the hydrophilicity of polyster fibre.
4. method of modifying of the present invention can improve hydrophilicity and the antistatic property of terylene molecule, the feel of fabrics of polyester is also had some improvement, the anti-microbial property that endowing terylene fabric is certain, its grafting is simultaneously firm, water-tolerant, has higher economic benefit and commercial introduction prospect.
Detailed description of the invention:
Be described in detail embodiments of the invention below, the present embodiment is implemented under premised on invention technical scheme, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.The experimental program of unreceipted actual conditions in embodiment, the condition that conveniently condition or manufacturer advise usually is implemented.
Embodiment one
A method for polyethylene glycol grafted chitosan modified polyester fibre, comprises the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1 hour under 50 DEG C of temperature conditions of 20% by polyster fibre mass fraction, mechanical agitation speed is 100 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:30; After preliminary treatment, polyster fibre is drained and use cold water flush again and 20 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 50 DEG C of heating conditions, add 20 milliliters of phthalic anhydrides again, react 6 hours at 135 DEG C, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:3 mixing, 30 DEG C are heated stirring reaction 10 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 7 times of insoluble matter solid, stirs after 2 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5 according to amount of substance, add the toluene solution of mixed weight 20 times, stirring reaction 8 hours at 60 DEG C of temperature, mixing speed is 20 revs/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:20; be warming up to 120 DEG C; mechanic whirl-nett reaction 3 hours; mixing speed is 200 revs/min; stirring reaction terminates the calcium chloride solution (mass concentration is 10%) of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 80 DEG C of stirring reactions 1 hour; mixing speed is 400 revs/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 80 DEG C of oven dry 2 times through cold water flush.
Embodiment two
A method for polyethylene glycol grafted chitosan modified polyester fibre, comprises the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1.5 hours under 55 DEG C of temperature conditions of 22% by polyster fibre mass fraction, mechanical agitation speed is 150 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:40; After preliminary treatment, polyster fibre is drained and use cold water flush again and 30 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 55 DEG C of heating conditions, add 20 milliliters of phthalic anhydrides again, react 7 hours at 135 DEG C, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:5 mixing, 30 DEG C are heated stirring reaction 15 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 10 times of insoluble matter solid, stirs after 3 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:7 according to amount of substance, add the toluene solution of mixed weight 25 times, stirring reaction 10 hours at 80 DEG C of temperature, mixing speed is 30 revs/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:25; be warming up to 150 DEG C; mechanic whirl-nett reaction 5 hours; mixing speed is 300 revs/min; stirring reaction terminates the calcium chloride solution (mass concentration is 15%) of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 100 DEG C of stirring reactions 2 hours; mixing speed is 600 revs/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 90 DEG C of oven dry 3 times through cold water flush.
Embodiment three
A method for polyethylene glycol grafted chitosan modified polyester fibre, comprises the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1 hour under 55 DEG C of temperature conditions of 20% by polyster fibre mass fraction, mechanical agitation speed is 150 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:30; After preliminary treatment, polyster fibre is drained and use cold water flush again and 30 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 55 DEG C of heating conditions, add 20 milliliters of phthalic anhydrides again, react 6 hours at 135 DEG C, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:5 mixing, 30 DEG C are heated stirring reaction 10 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 10 times of insoluble matter solid, stirs after 2 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:7 according to amount of substance, add the toluene solution of mixed weight 20 times, stirring reaction 8 hours at 80 DEG C of temperature, mixing speed is 20 revs/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:20; be warming up to 150 DEG C; mechanic whirl-nett reaction 3 hours; mixing speed is 300 revs/min; stirring reaction terminates the calcium chloride solution (mass concentration is 10%) of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 100 DEG C of stirring reactions 1 hour; mixing speed is 600 revs/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 90 DEG C of oven dry 2 times through cold water flush.
Embodiment four
A method for polyethylene glycol grafted chitosan modified polyester fibre, comprises the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1.5 hours under 50 DEG C of temperature conditions of 22% by polyster fibre mass fraction, mechanical agitation speed is 100 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:40; After preliminary treatment, polyster fibre is drained and use cold water flush again and 20 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 50 DEG C of heating conditions, add 20 milliliters of phthalic anhydrides again, react 7 hours at 135 DEG C, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:3 mixing, 30 DEG C are heated stirring reaction 15 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 7 times of insoluble matter solid, stirs after 3 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5 according to amount of substance, add the toluene solution of mixed weight 25 times, stirring reaction 8 hours at 60 DEG C of temperature, mixing speed is 30 revs/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:25; be warming up to 120 DEG C; mechanic whirl-nett reaction 5 hours; mixing speed is 200 revs/min; stirring reaction terminates the calcium chloride solution (mass concentration is 15%) of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 80 DEG C of stirring reactions 2 hours; mixing speed is 400 revs/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 80 DEG C of oven dry 3 times through cold water flush.
Embodiment five
A method for polyethylene glycol grafted chitosan modified polyester fibre, comprises the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1.5 hours under 55 DEG C of temperature conditions of 20% by polyster fibre mass fraction, mechanical agitation speed is 120 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:35; After preliminary treatment, polyster fibre is drained and use cold water flush again and 20 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 50 DEG C of heating conditions, add 20 milliliters of phthalic anhydrides again, react 6 hours at 135 DEG C, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:4 mixing, 30 DEG C are heated stirring reaction 12 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 8 times of insoluble matter solid, stirs after 3 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5 according to amount of substance, add the toluene solution of mixed weight 20 times, stirring reaction 10 hours at 60 DEG C of temperature, mixing speed is 20 revs/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:20; be warming up to 140 DEG C; mechanic whirl-nett reaction 5 hours; mixing speed is 200 revs/min; stirring reaction terminates the calcium chloride solution (mass concentration is 10%) of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 100 DEG C of stirring reactions 1 hour; mixing speed is 400 revs/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 90 DEG C of oven dry 2 times through cold water flush.
Embodiment six
A method for polyethylene glycol grafted chitosan modified polyester fibre, comprises the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1.5 hours under 55 DEG C of temperature conditions of 20% by polyster fibre mass fraction, mechanical agitation speed is 120 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:40; After preliminary treatment, polyster fibre is drained and use cold water flush again and 30 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 55 DEG C of heating conditions, add 20 milliliters of phthalic anhydrides again, react 7 hours at 135 DEG C, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:4 mixing, 30 DEG C are heated stirring reaction 12 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 8 times of insoluble matter solid, stirs after 3 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5 according to amount of substance, add the toluene solution of mixed weight 20 times, stirring reaction 10 hours at 80 DEG C of temperature, mixing speed is 30 revs/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:20; be warming up to 140 DEG C; mechanic whirl-nett reaction 5 hours; mixing speed is 200 revs/min; stirring reaction terminates the calcium chloride solution (mass concentration is 15%) of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 100 DEG C of stirring reactions 1 hour; mixing speed is 400 revs/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 90 DEG C of oven dry 3 times through cold water flush.
Described active constituent content >=97% preparing cyanuric acid in polyethylene glycol grafted chitosan derivative, its addition is in cyanuric acid active ingredient.
Comparative example:
Without the polyster fibre of modification.
It is terylene PARSTER fiber that the embodiment of the present invention and comparative example use, grammes per square metre 244g/m
2.
Method of testing:
The thin elevation measurement of fiber hair:
Be fixed on support by the fabric sample upper end of 2.5cm × 20cm, lower end is immersed in potassium permanganate solution, the lifting height of solution on fabric after mensuration 30min.
Antistatic property measures: test by rower FZ/T01042-1996 " textile material antistatic property electrostatic pressure, sheet resistance and the assay method of half-life ".
Washability measures: wash the fabric arranged according to GB/T8629-2001 standard of washing, measure the wetting time of fabric after washing, and compare with the fabric wetting time of washing prefinishing, judge its washability.
Bacteriostasis property measures:
Adopt shake flask method, measure the bacteriostasis rate of polyster fibre.
Hand feel performance is tested: close order and touch the fabric after arranging, with 5-10 people for a small group, grade, according to different feels, PRINTED FABRIC is carried out hand feel evaluation, concrete assessment method is: carry out feel grading from flexibility, smooth feeling two aspect, be divided into 5 grades, 1 grade the poorest, fabric feeling is comparatively hard, and sliding glutinous sense is poor.5 grades best, and fabrics feel soft, cunning are glutinous.
Concrete grading as shown in Table 1.
Table one: feel is graded
| 5 grades | 4 grades | 3 grades | 2 grades | 2 grades |
| Very good | Well | In | Slightly poor | Difference |
Table two: fabric hydrophilic, flexibility feature after the embodiment of the present invention arranges
The hydrophilicity of the modified polyster fibre of the present invention improves, in the large molecule of shitosan, a large amount of hydrophilic aminos and hydroxyl and peg molecule form hydrophily polymer film at fiber surface, increase its hydrophily, it combines closely simultaneously, resistance to water is high, there is higher economic benefit, and the hand feeling quality of dacron can be improved to a certain extent.
Table three: fabric antistatic behaviour and biocidal property after the embodiment of the present invention arranges
The electric conductivity of the modified polyster fibre of the present invention increases, half life, antistatic effect obtains good improvement, and due to the introducing of chitosan molecule, give the anti-microbial property that fabric is certain, owing to linking closely between polyster fibre with polyethylene glycol grafted chitosan derivative, thus its antistatic property and biocidal property durability also higher, there is comparatively good economic benefit.
Above content is only better embodiment of the present invention, and for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.
Claims (7)
1. a method for polyethylene glycol grafted chitosan modified polyester fibre, is characterized in that: comprise the following steps:
The first step: preliminary treatment polyster fibre:
Be sodium hydroxide solution stir process 1-1.5 hour under 50-55 DEG C of temperature conditions of 20-22% by polyster fibre mass fraction, mechanical agitation speed is 100-150 rev/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:30-40; After preliminary treatment, polyster fibre is drained and use cold water flush again and 20-30 DEG C of oven dry, obtain preliminary treatment polyster fibre;
Second step: prepare polyethylene glycol grafted chitosan derivative:
Get the N that 20g shitosan is dissolved in 300 milliliters, in dinethylformamide solution, stir 10 hours under 50-55 DEG C of heating condition, add 20 milliliters of phthalic anhydrides again, at 135 DEG C, react 6-7 hour, use mixture of ice and water cryoprecipitation, filter, through absolute ethyl alcohol, water washing, 50 DEG C of oven dry, obtain amidatioon shitosan;
By amidatioon shitosan, cyanuric acid, Na
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:3-5 mixing, 30 DEG C of heating stirring reaction 10-15 hour, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 7-10 times of insoluble matter solid, staticly settles after stirring 2-3 hour at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan;
Cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5-7 according to amount of substance, add mixed weight 20-25 toluene solution doubly, stirring reaction 8-10 hour at 60-80 DEG C of temperature, mixing speed is 20-30 rev/min, obtains polyethylene glycol grafted chitosan derivative solution;
3rd step: polyethylene glycol grafted chitosan modified polyester fibre:
Preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution; bath raio is 1:20-25; be warming up to 120-150 DEG C; mechanic whirl-nett reaction 3-5 hour; mixing speed is 200-300 rev/min; stirring reaction terminates the calcium chloride solution of rear interpolation preliminary treatment polyster fibre weight 0.5%; be cooled to 80-100 DEG C of stirring reaction 1-2 hour; mixing speed is 400-600 rev/min, after being drained by fiber after reaction terminates, obtain modified polyster fibre 80-90 DEG C of oven dry 2-3 time through cold water flush.
2. the method for a kind of polyethylene glycol grafted chitosan modified polyester fibre according to claim 1, it is characterized in that: described active constituent content >=97% preparing cyanuric acid in polyethylene glycol grafted chitosan derivative, its addition is in cyanuric acid active ingredient.
3. the method for a kind of polyethylene glycol grafted chitosan modified polyester fibre according to claim 1, is characterized in that: in described polyethylene glycol grafted chitosan modified polyester fibre, the mass concentration of calcium chloride solution is 10-15%.
4. the method for a kind of polyethylene glycol grafted chitosan modified polyester fibre according to claim 1, it is characterized in that: be sodium hydroxide solution stir process 1.5 hours under 55 DEG C of temperature conditions of 20% by polyster fibre mass fraction in the described first step, mechanical agitation speed is 120 revs/min, and the solid-to-liquid ratio of polyster fibre and sodium hydroxide solution is 1:35-40; After preliminary treatment, polyster fibre is drained and use cold water flush again and 20-30 DEG C of oven dry, obtain preliminary treatment polyster fibre.
5. the method for a kind of polyethylene glycol grafted chitosan modified polyester fibre according to claim 1 and 2, is characterized in that: by amidatioon shitosan, cyanuric acid, Na in described second step
2cO
3according to the DMF solution adding mixing quality 10 times after weight ratio 30:1:4 mixing, 30 DEG C are heated stirring reaction 12 hours, cross and filter solvent; To add acetone and ether mixed solution that volume ratio is 1: 1 in insoluble matter, mixed solution addition is 8 times of insoluble matter solid, stirs after 3 hours and staticly settle at 50 DEG C of temperature, filter, with washed with diethylether, naturally dry, obtain cyanuric acid modification amidatioon shitosan.
6. the method for a kind of polyethylene glycol grafted chitosan modified polyester fibre according to claim 1, it is characterized in that: cyanuric acid modification amidatioon shitosan is mixed with polyethylene glycol 1500 than for 1:5 according to amount of substance in described second step, add the toluene solution of mixed weight 20 times, stirring reaction 10 hours at 60-80 DEG C of temperature, mixing speed is 20-30 rev/min.
7. the method for a kind of polyethylene glycol grafted chitosan modified polyester fibre according to claim 1 or 3, it is characterized in that: preliminary treatment polyster fibre is added in polyethylene glycol grafted chitosan derivative solution in described 3rd step, bath raio is 1:20, be warming up to 140 DEG C, mechanic whirl-nett reaction 5 hours, mixing speed is 200 revs/min, stirring reaction terminates the calcium chloride solution of rear interpolation preliminary treatment polyster fibre weight 0.5%, be cooled to 100 DEG C of stirring reactions 1 hour, mixing speed is 400 revs/min, modified polyster fibre is obtained 90 DEG C of oven dry 2-3 time through cold water flush after being drained by fiber after reaction terminates.
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| CN108748514A (en) * | 2018-06-12 | 2018-11-06 | 阜南县腾博工艺品有限公司 | A kind of derivative modified plank processing method of polyethylene glycol grafted chitosan |
| CN108818847A (en) * | 2018-06-12 | 2018-11-16 | 阜南县腾博工艺品有限公司 | A kind of improvement bamboo clappers fungus-proof antisepsis treatment process |
| CN110528280A (en) * | 2019-05-20 | 2019-12-03 | 苏州海曼纺织科技有限公司 | A kind of modified technique of high performance PET fiber |
| CN110591040A (en) * | 2019-09-29 | 2019-12-20 | 浙江理工大学 | Preparation method of environment-friendly type softening agent for antibacterial facial tissue |
| CN110904723A (en) * | 2019-10-28 | 2020-03-24 | 浙江理工大学 | Preparation method of super-moisturizing and high-antibacterial softening agent for facial tissues |
| CN112281292A (en) * | 2020-09-30 | 2021-01-29 | 嘉兴华绰纺织股份有限公司 | Production process of biological modified polyester warp-knitted fabric |
| CN113830879A (en) * | 2021-09-02 | 2021-12-24 | 中工武大设计集团有限公司 | Chitosan surface coating modified rope-shaped artificial aquatic weed and preparation method thereof |
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