WO2020097981A1 - 利用黄酮和金属盐制备的阻燃蚕丝及其制备方法和应用 - Google Patents
利用黄酮和金属盐制备的阻燃蚕丝及其制备方法和应用 Download PDFInfo
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- WO2020097981A1 WO2020097981A1 PCT/CN2018/117773 CN2018117773W WO2020097981A1 WO 2020097981 A1 WO2020097981 A1 WO 2020097981A1 CN 2018117773 W CN2018117773 W CN 2018117773W WO 2020097981 A1 WO2020097981 A1 WO 2020097981A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- silk
- flame
- retardant
- metal salt
- flavonoids
- Prior art date
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 62
- 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 57
- 229910052751 metal Chemical class 0.000 title claims abstract description 26
- 239000002184 metal Chemical class 0.000 title claims abstract description 26
- 150000003839 salts Chemical class 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 3
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title abstract 3
- 229930003944 flavone Natural products 0.000 title abstract 3
- 235000011949 flavones Nutrition 0.000 title abstract 3
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title abstract 3
- 150000002212 flavone derivatives Chemical class 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 28
- -1 flavone compound Chemical class 0.000 claims abstract description 24
- 239000012266 salt solution Substances 0.000 claims abstract description 4
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims description 38
- 229930003935 flavonoid Natural products 0.000 claims description 34
- 235000017173 flavonoids Nutrition 0.000 claims description 34
- IPQKDIRUZHOIOM-UHFFFAOYSA-N Oroxin A Natural products OC1C(O)C(O)C(CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IPQKDIRUZHOIOM-UHFFFAOYSA-N 0.000 claims description 19
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 claims description 19
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 claims description 19
- AQHDANHUMGXSJZ-UHFFFAOYSA-N baicalin Natural products OC1C(O)C(C(O)CO)OC1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 AQHDANHUMGXSJZ-UHFFFAOYSA-N 0.000 claims description 19
- IKIIZLYTISPENI-ZFORQUDYSA-N baicalin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC=CC=1)O2 IKIIZLYTISPENI-ZFORQUDYSA-N 0.000 claims description 19
- 229960003321 baicalin Drugs 0.000 claims description 19
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims description 19
- 235000005875 quercetin Nutrition 0.000 claims description 19
- 229960001285 quercetin Drugs 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 13
- 239000004753 textile Substances 0.000 claims description 12
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 claims description 11
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 claims description 11
- 150000002215 flavonoids Chemical class 0.000 claims description 11
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 claims description 11
- 235000005493 rutin Nutrition 0.000 claims description 11
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 claims description 11
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 claims description 11
- 229960004555 rutoside Drugs 0.000 claims description 11
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 8
- 239000011790 ferrous sulphate Substances 0.000 claims description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 8
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 8
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 4
- 150000003384 small molecules Chemical class 0.000 claims description 3
- 239000004744 fabric Substances 0.000 abstract description 35
- 238000005406 washing Methods 0.000 abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 6
- 239000011574 phosphorus Substances 0.000 abstract description 6
- 229910052736 halogen Inorganic materials 0.000 abstract description 5
- 150000002367 halogens Chemical class 0.000 abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 238000007598 dipping method Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000419 plant extract Substances 0.000 abstract 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 239000000835 fiber Substances 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229910021645 metal ion Inorganic materials 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000010668 complexation reaction Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000008363 phosphate buffer Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000034994 death Effects 0.000 description 2
- 231100000517 death Toxicity 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000007730 finishing process Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 229940061607 dibasic sodium phosphate Drugs 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 238000005108 dry cleaning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000012064 sodium phosphate buffer Substances 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
-
- 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
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- 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
- D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 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
- D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
- D06M11/71—Salts of phosphoric acids
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/152—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen having a hydroxy group bound to a carbon atom of a six-membered aromatic ring
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/165—Ethers
-
- 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
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
-
- 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
- D06M2200/20—Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease
-
- 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
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Definitions
- the invention relates to the field of fabric flame retardancy, in particular to a flame retardant silk prepared by using flavonoids and metal salts, and a preparation method and application thereof.
- silk cannot be flame-retarded and modified by blending and spinning, and can only achieve flame-retardant purposes through post-processing.
- good silk flame retardant finishing must also have the characteristics of non-toxicity, less smoke, can withstand a certain degree of washing and dry cleaning, and does not hinder the original quality of silk.
- the early silk flame retardant finishing used stannic acid or boric acid-borax to be treated by dipping method, although it can obtain better flame retardant effect, but it has poor fastness to washing.
- halogen flame retardants have good flame retardant effects, their combustion products have a certain negative impact on the environment and are extremely harmful to the human body.
- Phosphorus and nitrogen flame retardants can also give silks better flame retardancy and washing resistance, but the finishing process is more complicated, and free formaldehyde will be released during finishing.
- the finished silk has the disadvantages of hard feeling and yellowing.
- the discharge of phosphorus-containing chemicals can cause eutrophication of water bodies.
- metal complexes such as titanium and zirconium can effectively improve the flame retardant performance of silk, but the applicable metal ion types are relatively small, the price is relatively expensive, and the wash resistance is also poor. Therefore, the development of flame retardants with halogen-free, high efficiency, low smoke, low toxicity, and environmental friendliness is an important research direction of flame retardants for textiles today. The above problems are urgently needed to be solved in this field.
- the technical problem to be solved by the present invention is to provide a method for preparing flame-retardant silk by using flavonoids and metal salts without enduring the use of traditional flame retardants containing nitrogen, phosphorus and halogen elements. method.
- the solution provided by the present invention is: a method for preparing flame-retardant silk using flavonoids and metal salts, including the following steps:
- step S2 Immerse the silk processed in step S1 into a metal salt solution with a concentration of 1-5 g / L, and perform heat preservation treatment at 50-70 ° C to obtain flame-retardant silk.
- the invention provides a method for improving the flame retardancy of silk by using natural small molecule flavonoid compound and metal salt combined treatment.
- Natural small-molecule flavonoids with specific structure for example, the structure satisfies at least one of the three conditions of 3-hydroxyl in ring C, 5-hydroxyl in ring A and 3'-hydroxyl and 4'-hydroxyl in ring B
- Natural small-molecule flavonoid compounds can be adsorbed on silk fibers under acidic conditions; at the same time, these small-structure natural flavonoid compounds adsorbed on silk fibers can occur with metal salts during subsequent metal salt treatment Complexation.
- metal ions can also complex with specific groups on silk fibers. The complexation between natural small-molecule flavonoid compounds, metal ions and silk fibers changes the thermal degradation process of the silk fibers when they are burned, thereby playing a flame retardant role.
- the small molecule flavonoid compound is one or more of baicalin, quercetin, or rutin.
- the heat preservation treatment time is 50-80 min.
- the metal salt is one or more of ferrous sulfate, ferric sulfate and titanium sulfate.
- the time for the heat preservation treatment in the step S2 is 30-50min.
- the present invention further provides a flame-retardant silk prepared based on the above method.
- the invention further provides an application based on the above-mentioned flame-retardant silk in textiles.
- the small molecule flavonoid compound used in the present invention is derived from plant tissues and is an environmentally friendly natural compound.
- the flame-retardant finishing method according to the present invention has a simple finishing process and obvious effects, and the metal salt used is inexpensive.
- the flame-retardant finishing method of the present invention is to give silk a good flame-retardant performance without the use of traditional flame retardants containing nitrogen, phosphorus and halogen elements, and has excellent durability. Therefore, this method It solves the environmental pollution problems caused by the use of traditional flame retardants in the production and use of flame retardant silk and the nitrogen, phosphorus and halogen elements after the flame retardant silk is discarded. It has the advantages of high efficiency and environmental protection.
- a flavonoid compound is a flavonoid compound, which is a type of yellow pigment derived from 2-phenylchromogen as a core, and the core May contain several substituents.
- Its parent core structure is a series of compounds formed by connecting two benzene rings (A ring and B ring) through the central three carbons (C ring). Its parent core structure is as follows:
- the present invention includes the following steps: selecting a natural small molecule flavonoid compound whose structure satisfies at least one of the three conditions of C ring containing 3-hydroxyl, A ring containing 5-hydroxyl and B ring containing 3'-hydroxyl and 4'-hydroxyl , Use the impregnation adsorption method to process the silk under the conditions of pH 2.5-3.5 and 70-90 °C; then, the silk is immersed in the metal salt solution with the concentration of 1-5g / L, using the impregnation adsorption method, in the 50-70 Treat the silk under the condition of °C. After the treatment is completed, wash and dry to obtain the silk with durable flame retardant function.
- Baicalin has 5-hydroxyl on ring A
- quercetin has 5-hydroxyl on ring A
- 3-hydroxyl on ring C 3-hydroxyl on ring C
- 3'-hydroxyl and 4'-hydroxyl on ring B rutin on A
- the ring has 5-hydroxyl
- the B ring has 3'-hydroxyl and 4'-hydroxyl.
- the flame retardant properties of silk fabrics are in accordance with GB / T 5454-1997 "Textile Combustion Performance Experimental Oxygen Index Method” and GB / T 5455-2014 "Textile Combustion Performance Vertical Damage Length, Smoldering and Afterburning Time” "Measure” to measure.
- the washing method of the flame-retardant silk fabric is carried out according to the standard of GB / T 3921-2008 "Textile color fastness test soap color fastness", using a special detergent for silk fabric 2g / L, bath ratio 1:50, at 40 °C Wash once every 30 minutes. Repeat washing to the required number of times.
- Table 1 shows the flame retardant properties of silk fabrics treated with 1% and 5% baicalin, quercetin and rutin, and then treated with 2g / L ferrous sulfate and titanium sulfate.
- the silk fabric treated with the natural flavonoid compound is immersed in a 1-5 g / L ferric sulfate solution and treated at 70 ° C. for 30 min. After the treatment, it is washed with cold water and dried to obtain a flame-retardant functional silk fabric.
- Table 2 shows the flame retardant properties of silk fabrics treated with 5% baicalin, quercetin and rutin, and then treated with 1-5 g / L ferric sulfate.
- the silk fabric treated with baicalin / quercetin mixed liquid and then treated with ferrous sulfate / titanium sulfate mixed liquid has a limiting oxygen index of 27.5%, and the damage length during vertical burning is 9.5cm, which meets China ’s GB / T17591-2006 "Flame retardant fabric" B1 flame retardant performance requirements (damage length less than 15cm).
- Example 3 The silk fabric prepared in Example 3 was subjected to a washing durability test, and the results are shown in Table 3.
- Table 3 shows that after repeated washing for many times, the limit oxygen index of the flame-retardant silk changes little, and the damage length during vertical combustion is still less than 15cm, which meets the B1 flame retardancy in China's GB / T 17591-2006 "flame retardant fabric" Performance requirements (damage length less than 15cm).
- This example illustrates that the flame retardant effect of silk prepared by the method of the present invention has excellent washing durability or water washing durability.
- Comparative Example 1 Untreated silk fabric.
- Comparative Example 2 A mixed aqueous solution of 2.5% (relative weight to silk) baicalin and 2.5% (relative weight to silk) quercetin was prepared, and the pH was adjusted to 3 with citric acid / disodium hydrogen phosphate buffer at room temperature Stir thoroughly; according to the bath ratio of 1:50 (silk weight to solution volume ratio), weigh the silk double-crepe fabric, immerse the silk fabric in the mixed liquid of baicalin and quercetin, and increase the temperature to 2 °C / min to Incubate at 80 ° C for 60 minutes. After the treatment, rinse with cold water and dry to obtain a silk fabric treated with baicalin / quercetin mixture.
- Comparative Example 3 The silk fabric was immersed in a 4g / L ferrous sulfate solution, treated at 50 ° C for 30 minutes, washed and dried.
- Comparative Example 4 The silk fabric was immersed in a 4g / L titanium sulfate solution, treated at 50 ° C for 30 minutes, washed and dried.
- Table 4 lists the burning properties of these silk fabric controls.
- the limit oxygen index of silk treated with ferrous sulfate and titanium sulfate is 25.9% and 25.8% respectively, and the damage length during vertical combustion is 24.2cm and 20.1cm, which cannot meet the requirements of China ’s GB / T 17591-2006 Fire-retardant fabric "B1 level flame retardant performance requirements.
- flavonoids can be adsorbed on silk fibers under acidic conditions; at the same time, these small natural flavonoid compounds with specific structures adsorbed on silk fibers can be used in the subsequent metal salt treatment process.
- Metal salts are complexed.
- metal ions can also complex with specific groups on silk fibers. The complexation between natural small-molecule flavonoid compounds, metal ions and silk fibers changes the thermal degradation process of the silk fibers when they are burned, thereby playing a flame retardant role.
- the silk treated with natural small molecule flavonoid compounds and metal salts has good flame retardant properties and excellent wash resistance.
- the flame-retardant silk prepared in this application can be used in textiles.
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Abstract
本发明公开了一种利用黄酮和金属盐制备的阻燃蚕丝及其制备方法和应用。包括以下步骤：选用结构上至少满足C环上含有3-羟基、A环含有5-羟基和B环上含有3'-羟基和4'-羟基三个条件之一的天然小分子黄酮化合物，利用浸渍吸附法，在pH为2.5～3.5和70-90℃的条件下处理蚕丝；然后，蚕丝浸入到浓度为1-5g/L的金属盐溶液当中，利用浸渍吸附法，在50-70℃的条件下处理蚕丝，处理完毕，水洗、烘干，即得耐久性阻燃功能蚕丝。本发明利用天然植物提取物和金属盐制备具有良好的阻燃性能的蚕丝织物，能够避免在生产和使用过程因使用含有氮、磷、卤族元素的传统阻燃剂而带来的环境污染问题，具有高效、环保、简便易行的优点。
Description
本发明涉及织物阻燃领域，具体涉及一种利用黄酮和金属盐制备的阻燃蚕丝及其制备方法和应用。
近年来，随着纺织技术的不断发展和人们自身安全意识的不断提升，人们对纺织品的防火安全性能也日益重视。据统计，由纺织品引起的住宅火灾次数占总火灾次数的五分之一，而死亡人数占总死亡人数的一半。因此，如何提高纺织品阻燃性能也是功能性纺织品领域的重要研究课题。蚕丝作为最常见的天然蛋白质纤维之一，因其光泽柔和自然、穿着透气舒适而深受消费者喜爱，常用于制作高档服装、窗帘和床上用品等。而蚕丝装饰物和部分日用服装对阻燃性能有着较高的要求。
蚕丝作为天然纤维无法通过共混纺丝的方法对其进行阻燃改性，只能通过后整理加工的方法来达到阻燃目的。此外，良好的蚕丝阻燃整理还必须兼有无毒性、发烟少、可耐一定程度的水洗和干洗以及不妨碍蚕丝原有品质的特点。早期的蚕丝阻燃整理利用的是锡酸或者硼酸-硼砂通过浸渍法进行处理，虽可获得较好的阻燃效果，但耐水洗牢度差。卤系阻燃剂虽然阻燃效果好，但是其燃烧产物对环境有一定的负面影响，而且对人体的危害性极大。磷氮类阻燃剂也可赋予蚕丝较好的阻燃性能和耐水洗性能，但整理工艺比较复杂，整理时会释放游离的甲醛，整理后的蚕丝存在手感发硬和泛黄的缺点，同时含磷化学品的排放会引起水体的富营养化。在Zirpro工艺中，钛、锆等金属络合物能有效地提升蚕丝的阻燃性能，但所适用的金属离子种类较少，且价格相对昂贵，耐洗 性也不佳。因此，开发具有无卤、高效、低烟、低毒、环境友好型的阻燃剂是当今纺织品用阻燃剂的重要研究方向。上述问题是本领域亟需解决的问题。
发明内容
本发明要解决的技术问题是提供一种在不使用传统的含氮、磷及卤族元素阻燃剂的条件下仍赋予了蚕丝良好的阻燃性能的利用黄酮和金属盐制备阻燃蚕丝的方法。
为了解决上述技术问题，本发明提供的方案是：利用黄酮和金属盐制备阻燃蚕丝的方法，包括以下步骤：
S1、将蚕丝浸入至pH值为2.5-3.5的小分子黄酮化合物溶液中，于70-90℃进行保温处理，所述小分子黄酮化合物对蚕丝的相对重量为1-5％，所述小分子黄酮化合物至少满足以下结构的一种，其母核的3位被羟基取代、5位被羟基取代或3’位和4’位同时被羟基取代；
S2、将经过步骤S1处理后的蚕丝浸入到浓度为1-5g/L的金属盐溶液当中，于50-70℃进行保温处理，得到阻燃蚕丝。
本发明提供了一种利用天然小分子黄酮化合物和金属盐联合处理提高蚕丝阻燃性的方法。一些特定结构的天然小分子黄酮化合物，例如，结构上至少满足C环上含有3-羟基、A环含有5-羟基和B环上含有3’-羟基和4’-羟基三个条件之一的天然小分子黄酮化合物，可在酸性条件下吸附于蚕丝纤维上；同时，吸附于蚕丝纤维上的这些特定结构的天然小分子黄酮化合物，在后续的金属盐处理的过程中，可与金属盐发生络合作用，另外，金属离子也能与蚕丝纤维上特定基团发生络合作用。天然小分子黄酮化合物、金属离子和蚕丝纤维之间的络合作用，改变了蚕丝纤维燃烧时的热降解进程，从而起到阻燃作用。
进一步的是：所述小分子黄酮化合物为黄芩苷、槲皮素或芦丁中的一种或多种。
进一步的是：所述步骤S1当中，保温处理的时间为50-80min。
进一步的是：所述金属盐为硫酸亚铁、硫酸铁和硫酸钛中的一种或多种。
进一步的是：所述步骤S2中保温处理的时间为30-50min。
本发明进一步的提供了一种基于上述方法所制备的阻燃蚕丝。
本发明进一步的提供了一种基于上述阻燃蚕丝在纺织中的应用。
本发明的有益效果：
1、本发明使用的小分子黄酮化合物来源于植物组织，为环境友好型的天然化合物。
2、本发明涉及的阻燃整理的方法整理过程简单、效果明显，所用的金属盐价格低廉。
3、本发明涉及的阻燃整理的方法是在不使用传统的含氮、磷及卤族元素阻燃剂的条件下仍赋予了蚕丝良好的阻燃性能，且耐久性优异，因此，该方法解决了因使用传统阻燃剂而带来的在阻燃蚕丝生产和使用过程中以及阻燃蚕丝被废弃后氮、磷及卤族元素带来的环境污染问题，具有高效环保的优点。
下面结合具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好地理解本发明并能予以实施，但所举实施例不作为对本发明的限定。
所应理解的是，在本领域中，小分子指分子量小于500的物质，黄酮化合物即黄酮类化合物，其是以2-苯基色原酮为母核而衍生的一类黄色色素，母核上可含有若干取代基，其母核结构为两个苯环(A环与B环)通过中央三碳(C环)相互联接而成的一系列化合物，其母核结构式如下：
本发明包括以下步骤：选用结构上至少满足C环上含有3-羟基、A环含有5-羟基和B环上含有3’-羟基和4’-羟基三个条件之一的天然小分子黄酮化合物，利用浸渍吸附法，在pH为2.5～3.5和70-90℃的条件下处理蚕丝；然后，蚕丝浸入到浓度为1-5g/L的金属盐溶液当中，利用浸渍吸附法，在50-70℃的条件下处理蚕丝，处理完毕，水洗、烘干，即得耐久性阻燃功能蚕丝。
为了便于理解，本申请还提供了以下几种具体的实施例，本发明提供的以下实施例中，采用三种典型的天然小分子黄酮化合物对蚕丝进行处理，它们分别是黄芩苷、槲皮素和芦丁，其化学结构如下：
黄芩苷：
槲皮素:
芦丁:
黄芩苷在A环上有5-羟基，槲皮素在A环有5-羟基、在C环上有3-羟基、 在B环上有3’-羟基和4’-羟基，芦丁在A环有5-羟基、在B环上有3’-羟基和4’-羟基。
在以下实施例中，蚕丝织物的阻燃性能按照GB/T 5454-1997《纺织品燃烧性能实验氧指数法》和GB/T 5455-2014《纺织品燃烧性能垂直方向损毁长度阴燃和续燃时间的测定》进行测定。阻燃蚕丝织物的水洗方法参照GB/T 3921-2008《纺织品色牢度试验耐皂洗色牢度》标准进行，使用丝毛织物专用洗涤剂2g/L，浴比1:50，40℃下洗涤30min为一次。重复水洗至所需水洗次数。
实施例1
S1、分别配制1％和5％(对蚕丝的相对重量)的黄芩苷、槲皮素和芦丁水溶液，用柠檬酸/磷酸氢二钠缓冲剂调节其pH至2.5，常温下充分搅拌；按照浴比1:50(蚕丝重量与溶液体积比)，称取蚕丝双绉织物，将蚕丝织物浸入到黄芩苷、槲皮素和芦丁溶液中，以2℃/min的速度升温至70℃，保温处理80min，处理结束后，冷水冲洗。
S2、将上述天然黄酮化合物处理后的蚕丝织物分别浸入2g/L的硫酸亚铁和硫酸钛溶液中，于50℃处理50min，处理后，冷水冲洗、烘干，得到阻燃蚕丝织物。
表1是经1％和5％黄芩苷、槲皮素和芦丁处理、再经2g/L硫酸亚铁和硫酸钛处理的蚕丝织物的阻燃性能。
表1
由表1可以看出所有蚕丝织物的极限氧指数均高于26.6％，垂直燃烧时的损毁长度均小于15cm，均满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求(损毁长度小于15cm)。
实施例2
S1、配制5％(对蚕丝的相对重量)的黄芩苷、槲皮素和芦丁水溶液，用柠檬酸/磷酸氢二钠缓冲剂调节其pH至3.5，常温下充分搅拌；按照浴比1:50(蚕丝重量与溶液体积比)，称取蚕丝双绉织物，将蚕丝织物浸入到黄芩苷、槲皮素和芦丁溶液中，以2℃/min的速度升温至90℃，保温处理50min，处理结束后，冷水冲洗。
S2、将上述天然黄酮化合物处理后的蚕丝织物浸入1-5g/L的硫酸铁溶液中，于70℃处理30min，处理后，冷水冲洗、烘干，得到阻燃功能蚕丝织物。
表2是经5％黄芩苷、槲皮素和芦丁处理、再经1-5g/L硫酸铁处理的蚕丝织物的阻燃性能。
表2
由表2可以看出，所有蚕丝织物的极限氧指数均高于26.5％，垂直燃烧时的损毁长度均小于12cm，均满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求(损毁长度小于15cm)。
实施例3
S1、配制2.5％(对蚕丝的相对重量)黄芩苷和2.5％(对蚕丝的相对重量)槲皮素的混合水溶液，用柠檬酸/磷酸氢二钠缓冲剂调节其pH至3，常温下充 分搅拌；按照浴比1:50(蚕丝重量与溶液体积比)，称取蚕丝双绉织物，将蚕丝织物浸入到黄芩苷和槲皮素混合液中，以2℃/min的速度升温至80℃，保温处理60min，处理结束后，冷水冲洗。
S2、将上述天然黄酮化合物处理后的蚕丝织物浸入2.5g/L硫酸亚铁和2.5g/L硫酸钛混合液中，于60℃处理40min，处理后，冷水冲洗、烘干，得到耐久性的阻燃功能的蚕丝织物。
经黄芩苷/槲皮素混合液处理、再经硫酸亚铁/硫酸钛混合液处理的蚕丝织物的极限氧指数为27.5％，垂直燃烧时的损毁长度为9.5cm，满足我国GB/T17591-2006《阻燃织物》中B1级阻燃性能要求(损毁长度小于15cm)。
对实施例3所制备的蚕丝织物进行耐洗性试验，结果见表3。
表3
| 洗涤次数 | 极限氧指数(％) | 损毁长度(cm) |
| 0 | 27.5 | 9.5 |
| 5 | 27.0 | 10.9 |
| 10 | 26.9 | 11.1 |
| 15 | 26.8 | 11.2 |
| 20 | 26.8 | 11.3 |
表3表明，经多次重复洗涤后，阻燃蚕丝的极限氧指数变化较小，垂直燃烧时的损毁长度仍小于15cm，满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求(损毁长度小于15cm)。本实施例说明用本发明方法制备的蚕丝的阻燃效果具有优异的耐洗性或水洗耐久性。
此外，本申请还提供以下几种对照例
对照例1：未处理的蚕丝织物。
对照例2：配制2.5％(对蚕丝的相对重量)黄芩苷和2.5％(对蚕丝的相对重量)槲皮素的混合水溶液，用柠檬酸/磷酸氢二钠缓冲剂调节其pH至3，常温下充分搅拌；按照浴比1:50(蚕丝重量与溶液体积比)，称取蚕丝双绉织物，将蚕丝织物浸入到黄芩苷和槲皮素混合液中，以2℃/min的速度升温至80℃， 保温处理60min，处理结束后，冷水冲洗、烘干，得到黄芩苷/槲皮素混合液处理的蚕丝织物。
对照例3：将蚕丝织物浸入到4g/L的硫酸亚铁溶液中，于50℃处理30min，洗净、烘干。
对照例4：将蚕丝织物浸入到4g/L的硫酸钛溶液中，于50℃处理30min，洗净、烘干。
表4列出了这些蚕丝织物对照样的燃烧性能。
表4
由表4可以看出，未处理蚕丝的极限氧指数为23.6％，在垂直燃烧时完全燃烧，损毁长度为30.0cm；单独黄芩苷/槲皮素混合液处理的蚕丝的极限氧指数为24.4％，在垂直燃烧测试时亦完全燃烧，损毁长度为30.0cm；未处理蚕丝和单独黄芩苷/槲皮素混合液处理的蚕丝均没有阻燃性。另外，单独用硫酸亚铁和硫酸钛处理的蚕丝的极限氧指数分别为25.9％和25.8％，垂直燃烧时的损毁长度分别为24.2cm和20.1cm，不能满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求。
以上实施例说明，采用本发明中利用天然小分子黄酮化合物和金属盐联合处理制备阻燃蚕丝的方法，能赋予蚕丝良好的阻燃性能，而且阻燃功能的水洗耐久性优异。该方法具有环保、高效、简单易行的优点。
本申请的原理是：黄酮类化合物可在酸性条件下吸附于蚕丝纤维上；同时，吸附于蚕丝纤维上的这些特定结构的天然小分子黄酮化合物，在后续的金属盐 处理的过程中，可与金属盐发生络合作用，另外，金属离子也能与蚕丝纤维上特定基团发生络合作用。天然小分子黄酮化合物、金属离子和蚕丝纤维之间的络合作用，改变了蚕丝纤维燃烧时的热降解进程，从而起到阻燃作用。
本申请利用天然小分子黄酮化合物和金属盐联合处理的蚕丝具有良好的阻燃性能以及优异的耐洗性。
此外，本申请制备的阻燃蚕丝可以应用于纺织当中。
以上所述实施例仅是为充分说明本发明而所举的较佳的实施例，本发明的保护范围不限于此。本技术领域的技术人员在本发明基础上所作的等同替代或变换，均在本发明的保护范围之内。本发明的保护范围以权利要求书为准。
Claims (7)
- 利用黄酮和金属盐制备阻燃蚕丝的方法，其特征在于，包括以下步骤：S1、将蚕丝浸入至pH值为2.5-3.5的小分子黄酮化合物溶液中，于70-90℃进行保温处理，所述小分子黄酮化合物对蚕丝的相对重量为1-5％，所述小分子黄酮化合物至少满足以下结构的一种，其母核的3位被羟基取代、5位被羟基取代或3’位和4’位同时被羟基取代；S2、将经过步骤S1处理后的蚕丝浸入到浓度为1-5g/L的金属盐溶液当中，于50-70℃进行保温处理，得到阻燃蚕丝。
- 如权利要求1所述的利用黄酮和金属盐制备阻燃蚕丝的方法，其特征在于，所述小分子黄酮化合物为黄芩苷、槲皮素或芦丁中的一种或多种。
- 如权利要求1所述的利用黄酮和金属盐制备阻燃蚕丝的方法，其特征在于，所述步骤S1当中，保温处理的时间为50-80min。
- 如权利要求1所述的利用黄酮和金属盐制备阻燃蚕丝的方法，其特征在于，所述金属盐为硫酸亚铁、硫酸铁和硫酸钛中的一种或多种。
- 如权利要求1所述的利用黄酮和金属盐制备阻燃蚕丝的方法，其特征在于，所述步骤S2中保温处理的时间为30-50min。
- 根据权利要求1至5中任一方法所制备的阻燃蚕丝。
- 根据权利要求1至5中任一方法所制备的阻燃蚕丝在纺织中的应用。
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| CN110106708B (zh) * | 2019-05-24 | 2021-11-02 | 苏州大学 | 一种非虹彩结构色织物及其制备方法 |
| CN110172823B (zh) * | 2019-06-27 | 2020-10-30 | 四川大学 | 一种无甲醛耐水洗阻燃织物的制备方法 |
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