CN111188202B - Flame-retardant high-temperature-resistant composite fabric and preparation method thereof - Google Patents
Flame-retardant high-temperature-resistant composite fabric and preparation method thereof Download PDFInfo
- Publication number
- CN111188202B CN111188202B CN202010084916.5A CN202010084916A CN111188202B CN 111188202 B CN111188202 B CN 111188202B CN 202010084916 A CN202010084916 A CN 202010084916A CN 111188202 B CN111188202 B CN 111188202B
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- China
- Prior art keywords
- flame
- temperature
- retardant high
- resistant
- retardant
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 75
- 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 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000009726 composite fabrication method Methods 0.000 title description 2
- 239000004744 fabric Substances 0.000 claims abstract description 67
- 239000004814 polyurethane Substances 0.000 claims abstract description 40
- 229920002635 polyurethane Polymers 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 28
- 239000000839 emulsion Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 12
- 229920006231 aramid fiber Polymers 0.000 claims abstract description 7
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 239000000835 fiber Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000010935 stainless steel Substances 0.000 claims abstract description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 7
- 239000002562 thickening agent Substances 0.000 claims abstract description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000009987 spinning Methods 0.000 claims abstract description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 42
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 32
- 239000002202 Polyethylene glycol Substances 0.000 claims description 31
- 229920001223 polyethylene glycol Polymers 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 11
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 claims description 11
- -1 phosphaphenanthrene compound Chemical class 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 9
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 9
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 8
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 7
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 229920002545 silicone oil Polymers 0.000 claims description 7
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 7
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000000741 silica gel Substances 0.000 claims description 5
- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 3
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 claims description 2
- LKRNXDNUDPTRRQ-UHFFFAOYSA-L CCCC[Sn++]CCCC.CCCC[Sn++]CCCC.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O Chemical compound CCCC[Sn++]CCCC.CCCC[Sn++]CCCC.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O LKRNXDNUDPTRRQ-UHFFFAOYSA-L 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 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
- 238000009941 weaving Methods 0.000 abstract description 3
- 239000011527 polyurethane coating Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 description 13
- 239000001301 oxygen Substances 0.000 description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 238000002485 combustion reaction Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000004760 aramid Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011496 polyurethane foam Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000004831 Hot glue Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical group C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3878—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus
- C08G18/3889—Low-molecular-weight compounds having heteroatoms other than oxygen having phosphorus having nitrogen in addition to phosphorus
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5096—Polyethers having heteroatoms other than oxygen containing silicon
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
- D06N3/0034—Polyamide fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/08—Inorganic fibres
- D06N2201/085—Metal fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/067—Flame resistant, fire resistant
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Dispersion Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a flame-retardant high-temperature-resistant composite fabric and a preparation method thereof, and the preparation method comprises the following steps: uniformly mixing the modified polyurethane emulsion, the thickening agent, ammonia water and the cross-linking agent to prepare a flame-retardant high-temperature-resistant coating agent, carrying out drafting and twisting processes on aramid fiber and stainless steel fiber through a roving frame and a spinning frame to obtain mixed yarn, and weaving the mixed yarn to obtain base cloth; padding the base cloth with the modified polyurethane emulsion, and performing pre-baking and baking processes to obtain the flame-retardant high-temperature-resistant base cloth; uniformly coating the flame-retardant high-temperature-resistant coating agent on the surface of the flame-retardant high-temperature-resistant base fabric, and drying the coated flame-retardant high-temperature-resistant base fabric layer to obtain a flame-retardant high-temperature-resistant composite fabric; according to the invention, the phosphorus-containing flame-retardant group and the organic silicon are introduced into the polyurethane chain to prepare the modified polyurethane emulsion, the modified polyurethane emulsion is used for padding the base fabric, and the padded base fabric is compounded with the modified polyurethane coating to obtain the composite fabric with excellent flame-retardant and high-temperature-resistant performances.
Description
Technical Field
The invention relates to the technical field of flame-retardant materials, in particular to a flame-retardant high-temperature-resistant composite fabric and a preparation method thereof.
Background
A large amount of flammable and combustible materials exist in public places, so that fire disasters are easily caused in daily life and production, and great loss is caused to life and property safety of people. The new "fire-fighting law" of China is issued and implemented, ministries such as the public security department issue a series of fire-fighting regulations for the purpose of regulating the fire-fighting safety of public places, the national flame-retardant standard and the industry flame-retardant standard are also successively formulated and issued and implemented, and the demands of markets such as public places, transportation tools and the like on flame-retardant and flame-retardant materials are increasing day by day.
According to the fire-proof safety, automobiles, trains, airplanes, ships, seats, mattresses and the like need a large amount of flame-retardant composite fabric due to the application characteristics. Most of the currently produced composite fabrics in China are non-flame-retardant, or common composite fabrics are subjected to post-treatment by adding a flame retardant to obtain flame-retardant composite fabrics, or flame-retardant composite fabrics are obtained by adopting a method of compounding the flame-retardant fabrics with polyurethane sponge and adding the flame retardant to perform post-treatment. However, the composite fabrics have poor flame retardance, even if the oxygen index of the composite fabrics is difficult to reach 28% after the amount of the flame retardant is increased, the composite fabrics cannot meet the regulation that the oxygen index is more than or equal to 28.0% in JT/T1095-2016 (flame retardant property of interior materials of passenger cars), and cannot meet the regulation requirements that the oxygen index is more than or equal to 32.0% in GB8624-2012 (classification of combustion performance of building materials and products) and GB20286-2006 (requirement of combustion performance of flame retardant products and components in public places and identification). The environment-friendly property of the composite fabric obtained by adding the flame retardant post-treatment mode is worried, and substances such as flame retardants, glue, hot melt adhesives and the like adsorbed on the surface of the fabric can slowly overflow or slowly decompose and overflow when the composite fabric is used in a carriage seat sleeve in the heating state of an air conditioner, so that people cannot accept odor or even toxic odor, and the health of people is directly influenced.
Disclosure of Invention
The invention aims to provide a flame-retardant high-temperature-resistant composite fabric and a preparation method thereof, which can solve the following problems:
1. the existing flame-retardant fabric has poor flame-retardant effect, and the oxygen index in the flame-retardant fabric is difficult to reach 28%;
2. the existing flame-retardant fabric can generate unpleasant gas when burning, and the gas can affect the health of people.
The purpose of the invention can be realized by the following technical scheme:
the flame-retardant high-temperature-resistant composite fabric comprises a flame-retardant layer and a base fabric layer, wherein the flame-retardant layer is obtained by curing and film-forming a flame-retardant high-temperature-resistant coating agent, the base fabric layer is flame-retardant high-temperature-resistant base fabric, and the specific preparation method of the flame-retardant high-temperature-resistant composite fabric comprises the following steps:
(1) uniformly mixing the modified polyurethane emulsion, the thickening agent, the ammonia water and the crosslinking agent to prepare the flame-retardant high-temperature-resistant coating agent, wherein the mass ratio of the modified polyurethane emulsion to the thickening agent to the ammonia water to the crosslinking agent is 90-95: 4-8: 0.5-2: 0.5 to 1;
(2) the method comprises the following steps of proportioning aramid fibers and stainless steel fibers, mixing the aramid fibers and the stainless steel fibers through drawing on a drawing frame, then performing drafting and twisting processes through a roving frame and a spinning frame to obtain mixed yarns, weaving the mixed yarns to obtain base cloth, wherein the mass ratio of the aramid fibers to the stainless steel fibers is 1: 2-3;
(3) adding the modified polyurethane emulsion into a rolling groove, immersing the base cloth into the rolling groove, performing two-immersion and two-rolling, and performing pre-baking and baking processes to obtain the flame-retardant high-temperature-resistant base cloth, wherein the pre-baking temperature is 100-;
(4) and uniformly coating the flame-retardant high-temperature-resistant coating agent on the surface of the base cloth layer, airing the coated base cloth layer at room temperature, and drying in an oven at 70-90 ℃ for 5-10h to obtain the flame-retardant high-temperature-resistant composite fabric.
Preferably, the preparation method of the modified polyurethane emulsion comprises the following steps:
s1, drying polyethylene glycol by using silica gel, then adding the dried polyethylene glycol into N, N-dimethylformamide, stirring and heating to 60-70 ℃ to completely dissolve the polyethylene glycol, cooling to room temperature, adding hydroxyl silicone oil and stannous octoate, heating to 60-80 ℃, and reacting for 1-2 hours to obtain modified polyethylene glycol, wherein the reaction equation is as follows:
the main chain of the organic silicon is formed by Si-O bonds, the bond energy of the Si-O bonds is much larger than that of C-O bonds and C-C bonds forming organic matters, so that the organic silicon compound has better high temperature resistance than common organic compounds, the bond length of the Si-O bonds is longer, the bond angle is larger, the rotating and stretching space of a siloxane chain segment is larger, the movement is more free, and the chain segment is more flexible, so that the organic silicon material has good flexibility at low temperature.
S2, dissolving a phosphaphenanthrene compound in dichloromethane, cooling to 0-5 ℃, adding carbon tetrachloride, stirring for 10-20min, adding triethylamine and hydroxyethyl methacrylate, heating to 20-25 ℃, reacting for 10-16h, washing the reaction liquid for 3 times by using deionized water, drying an organic phase by using anhydrous sodium sulfate, filtering, and concentrating and drying the filtrate under reduced pressure to obtain an intermediate I, wherein the reaction equation is as follows:
s3, adding ethanol into a reaction bottle, adding diethanolamine and the intermediate I obtained in the step S2, heating to 60-70 ℃, reacting for 8-12h, washing the reaction liquid with deionized water for 3 times, and distilling the organic phase under reduced pressure to obtain an intermediate II, wherein the reaction equation is as follows:
the phosphorus flame retardant can simultaneously play a role in condensed phase and gas phase flame retardance, has flame retardance efficiency superior to other flame retardants, is the most widely applied flame retardant at present, is a typical phosphorus flame retardant, has a phenanthrene ring structure, good thermal stability and high reaction activity of a P-H structure, can react with active groups such as amino groups, warp groups, C ═ C double bonds and the like, can generate PO & free radicals in the combustion process of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and derivatives thereof, captures HO & H & generated by combustion, simultaneously generates phosphorus-containing oxy acid, and generates a dehydration catalyst by the polymerization reaction of the oxy acid under strong heat, catalyzing the formation of a carbon layer and delaying further combustion of the substrate.
S4, under the protection of nitrogen, adding isophorone diisocyanate, modified polyethylene glycol obtained in S1 and an intermediate II obtained in S3 into a reaction bottle, adding acetone, heating to 80-90 ℃ under stirring, dropwise adding dibutyltin dilaurate, and reacting for 4-6 hours to obtain a prepolymer I, wherein the reaction equation is as follows:
s5, adding dimethylolpropionic acid into the prepolymer I, heating to 80 ℃, reacting for 3-4h, adding acetone to adjust the system viscosity, cooling to 50-60 ℃, adding triethylamine, reacting for 0.5-1h, adding deionized water, stirring for 0.5-1h, and distilling under reduced pressure to obtain the modified polyurethane emulsion.
Preferably, the mass ratio of the polyethylene glycol, the hydroxy silicone oil and the stannous octoate in the step S1 is 1: 0.5-2: 0.01-0.05, and 8-15mL of N, N-dimethylformamide is used per gram of polyethylene glycol.
Preferably, the molar ratio of the phosphaphenanthrene compound, carbon tetrachloride, triethylamine and hydroxyethyl methacrylate in step S2 is 1: 1-1.5:1-1.5:1-1.2, using dichloromethane 8-15mL per gram of phosphaphenanthrene compound.
Preferably, the molar ratio of the diethanolamine to the intermediate one in the step S3 is 1-1.5:1, 8-15mL of ethanol is used per gram of intermediate.
Preferably, the mole ratio of the isophorone diisocyanate, the modified polyethylene glycol, the intermediate bis and the dibutyltin dilaurate in the step S4 is 1: 1-2: 2-3:0.01-0.05, and 5-10mL of acetone is used per gram of isophorone diisocyanate.
Preferably, in the step S5, the mass ratio of the dimethylolpropionic acid to the prepolymer one to the triethylamine is 1: 2-5: 0.1-0.5, 5-8mL of acetone and 3-5mL of deionized water are used for each gram of dimethylolpropionic acid.
Preferably, the cross-linking agent is XR-501 (Shanghai West chemical technology Co., Ltd.), and the thickening agent is DM-5256 (Chengdu Demei Elite chemical Co., Ltd.).
The invention has the beneficial effects that:
by modifying polyurethane, the modified polyurethane is used for a base cloth coating, so that the fabric which is high in flame retardance and more environment-friendly is obtained; the water-based polyurethane is used as a main raw material, water is used as a dispersing agent to replace an organic solvent in solvent-based polyurethane, so that the water-based polyurethane is environment-friendly, non-toxic and low in energy consumption, the physical and chemical structure of a molecular chain is kept unchanged, the performance of the water-based polyurethane can be basically comparable to that of solvent-based polyurethane, and acetone with low boiling point and low toxicity is used as a solvent in the reaction process, so that the water-based polyurethane can be recycled, the energy is saved, in addition, the water-based polyurethane can be diluted by adding water to adjust the solid content, and is safe, convenient and easy to use and clean;
the phosphorus-containing compound branched chain is introduced into the polyurethane, so that the flame retardant property of the polyurethane material is effectively improved, the phosphorus-containing compound is easy to react with oxygen under the heating condition to generate phosphoric acid at first, then generate metaphosphoric acid and finally generate stable polymetaphosphoric acid, the finally generated glassy polymetaphosphoric acid covers the surface of the base material, and the polymetaphosphoric acid mainly plays a flame retardant role in two aspects: on one hand, the polymer surface is quickly carbonized into a film, oxygen and heat are isolated, and internal materials are prevented from continuously burning; on the other hand, the polymer is a strong acid, has strong dehydration function, takes oxygen from the polymer, promotes the dehydration of the polymer to form a carbon layer capable of isolating oxygen and heat, thereby preventing or reducing the generation of combustible gas and playing a role in flame retardance;
by introducing organosilicon into the main chain of polyurethane, siloxane bonds (Si-O) and- [ Si-O ] in the molecular structure of organosilicon]xThe structure of the polyurethane has high thermal stability, the high temperature resistance and the flame retardant property of the polyurethane can be improved at the same time, and the carbonization layer formed by the organosilicon at high temperature is more compact and continuous, so that the further combustion of the base material can be delayed; organosilicon can not produce the molten drop in combustion process, and burning speed is slow, can not discharge poisonous smog, compares the fire-retardant surface fabric environmental protection more that contains halogen, in addition, through introducing the silica-oxygen bond in the polyurethane main chain, can improve performances such as oxidation resistance, low temperature compliance and the low surface energy of polyurethane, makes polyurethane coating surface not fragile, and easily clearance.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing modified polyurethane emulsion:
s1, drying polyethylene glycol by using silica gel, then adding 100g of dried polyethylene glycol into 10mLN, N-dimethylformamide, stirring and heating to 60 ℃ to completely dissolve the polyethylene glycol, adding 80g of hydroxyl silicone oil and 1g of stannous octoate, heating to 80 ℃, and reacting for 2 hours to obtain modified polyethylene glycol;
s2, dissolving 50g of phosphaphenanthrene compound in 500mL of dichloromethane, cooling to below 5 ℃, adding 45g of carbon tetrachloride, stirring for 20min, adding 30g of triethylamine and 40g of hydroxyethyl methacrylate, heating to 25 ℃, reacting for 12h, washing the reaction liquid with deionized water for 3 times, drying the organic phase with anhydrous sodium sulfate, filtering, and concentrating the filtrate under reduced pressure to dryness to obtain an intermediate I;
s3, adding 500mL of ethanol into a reaction bottle, adding 28g of diethanolamine and the intermediate I obtained in the step S2, heating to 70 ℃, reacting for 10 hours, washing the reaction liquid with deionized water for 3 times, and distilling the organic phase under reduced pressure to obtain an intermediate II;
s4, under the protection of nitrogen, adding 50g of isophorone diisocyanate, 60g of modified polyethylene glycol obtained in S1 and 40g of intermediate obtained in S3 into a reaction bottle, adding 300mL of acetone, heating to 80 ℃ under stirring, dropwise adding 0.5g of dibutyltin dilaurate, and reacting for 6 hours to obtain a prepolymer I;
s5, adding 10g of dimethylolpropionic acid into 50g of prepolymer I, heating to 80 ℃, reacting for 3-4h, adding 300mL of acetone, cooling to 50-60 ℃, adding triethylamine, reacting for 0.5-1h, distilling under reduced pressure to remove acetone, adding 150mL of deionized water, and stirring for 0.5h to obtain the modified polyurethane emulsion A.
Example 2
Preparing modified polyurethane emulsion:
s1, drying polyethylene glycol by using silica gel, then adding 100g of dried polyethylene glycol into 10mLN, N-dimethylformamide, stirring and heating to 60 ℃ to completely dissolve the polyethylene glycol, adding 60g of hydroxy silicone oil and 1g of stannous octoate, heating to 80 ℃, and reacting for 2 hours to obtain modified polyethylene glycol;
s2, dissolving 50g of phosphaphenanthrene compound in 500mL of dichloromethane, cooling to below 5 ℃, adding 50g of carbon tetrachloride, stirring for 20min, adding 40g of triethylamine and 45g of hydroxyethyl methacrylate, heating to 25 ℃, reacting for 12h, washing the reaction solution with deionized water for 3 times, drying an organic phase with anhydrous sodium sulfate, filtering, and concentrating the filtrate under reduced pressure to dryness to obtain an intermediate I;
s3, adding 500mL of ethanol into a reaction bottle, adding 30g of diethanolamine and the intermediate I obtained in the step S2, heating to 70 ℃ for reaction for 10 hours, washing the reaction liquid with deionized water for 3 times, and distilling an organic phase under reduced pressure to obtain an intermediate II;
s4, under the protection of nitrogen, adding 50g of isophorone diisocyanate, 65g of modified polyethylene glycol obtained in S1 and 45g of intermediate obtained in S3 into a reaction bottle, adding 300mL of acetone, heating to 80 ℃ under stirring, dropwise adding 0.5g of dibutyltin dilaurate, and reacting for 6 hours to obtain a prepolymer I;
s5, adding 10g of dimethylolpropionic acid into 50g of the prepolymer I, heating to 80 ℃, reacting for 3-4h, adding 300mL of acetone, cooling to 50-60 ℃, adding triethylamine, reacting for 0.5-1h, distilling under reduced pressure to remove acetone, adding 150mL of deionized water, and stirring for 0.5h to obtain the modified polyurethane emulsion B.
Example 3
Preparing modified polyurethane emulsion:
s1, drying polyethylene glycol by using silica gel, adding 80g of dried polyethylene glycol into 10mLN, N-dimethylformamide, stirring and heating to 60 ℃ to completely dissolve the polyethylene glycol, adding 80g of hydroxy silicone oil and 1g of stannous octoate, heating to 80 ℃, and reacting for 2 hours to obtain modified polyethylene glycol;
s2, dissolving 50g of phosphaphenanthrene compound in 500mL of dichloromethane, cooling to below 5 ℃, adding 40g of carbon tetrachloride, stirring for 20min, adding 35g of triethylamine and 40g of hydroxyethyl methacrylate, heating to 25 ℃, reacting for 12h, washing the reaction solution with deionized water for 3 times, drying an organic phase with anhydrous sodium sulfate, filtering, and concentrating the filtrate under reduced pressure to dryness to obtain an intermediate I;
s3, adding 500mL of ethanol into a reaction bottle, adding 28g of diethanolamine and the intermediate I obtained in the step S2, heating to 70 ℃, reacting for 10 hours, washing the reaction liquid with deionized water for 3 times, and distilling the organic phase under reduced pressure to obtain an intermediate II;
s4, under the protection of nitrogen, adding 60g of isophorone diisocyanate, 70g of modified polyethylene glycol obtained by S1 and 40g of intermediate obtained by S3 into a reaction bottle, adding 300mL of acetone, heating to 80 ℃ under stirring, dropwise adding 0.5g of dibutyltin dilaurate, and reacting for 6 hours to obtain a prepolymer I;
s5, adding 15g dimethylolpropionic acid into 50g of the prepolymer I, heating to 80 ℃, reacting for 3-4h, adding 300mL of acetone, cooling to 50-60 ℃, adding triethylamine, reacting for 0.5-1h, distilling under reduced pressure to remove acetone, adding 150mL of deionized water, and stirring for 0.5h to obtain the modified polyurethane emulsion C.
Example 4
Preparing a flame-retardant high-temperature-resistant composite fabric:
(1) uniformly mixing 45g of modified polyurethane emulsion A/B/C, 4g of thickening agent, 1g of ammonia water and 0.5g of crosslinking agent to prepare a flame-retardant high-temperature-resistant coating agent;
(2) mixing aramid fiber and stainless steel fiber in a ratio of 1: 2, drawing and mixing on a drawing frame, then performing drafting and twisting processes on the drawn yarn by a roving frame and a spinning frame to obtain mixed yarn, and weaving the mixed yarn to obtain base cloth;
(3) adding the modified polyurethane emulsion A/B/C into a rolling groove, immersing the base cloth into the rolling groove, carrying out two-immersion and two-rolling, and carrying out pre-baking at 120 ℃ for 40s and baking at 160 ℃ for 30s to obtain the flame-retardant high-temperature-resistant base cloth;
(4) and uniformly coating the flame-retardant high-temperature-resistant coating agent on the surface of the base fabric layer, airing the coated base fabric layer for 24 hours at room temperature, and drying in an oven at 80 ℃ for 8 hours to obtain the flame-retardant high-temperature-resistant composite fabric A/B/C.
Comparative example 1
The thickness is 5mm, the density is 25kg/m3And (3) compounding the flame-retardant soft polyurethane foam sponge (Shanghai Xin new material science and technology Co., Ltd.) with the base cloth obtained in the step (2) to obtain a comparative fabric D, wherein the flame-retardant soft polyurethane foam sponge has a limit oxygen index of 22.8%.
Example 5
The test of the fabric obtained by the invention and the comparative fabric is as follows:
the limiting oxygen index is tested by the method of GB/T5454-1997;
the horizontal burning velocity test passes the test of the method of GB 8410-2006;
the vertical burning velocity test passes the method test of GB 32086-2015;
the smoke density grade test passes the test method of GB/T8627-2007;
the test results are shown in the following table:
the above table shows that the flame retardant performance of the flame retardant and high temperature resistant composite fabric prepared by the invention is greatly improved compared with the existing flame retardant fabric, wherein the horizontal burning speed of A, B, C is 0, the vertical burning speed is less than 10mm/min, the flame retardant performance is excellent, the limiting oxygen index is also more than 30%, the regulation that the oxygen index is more than or equal to 28.0% in JT/T1095-2016 flame retardant property of interior materials of passenger cars is met, and the smoke density grade is far lower than that of the existing flame retardant fabric.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
1. A preparation method of a flame-retardant high-temperature-resistant composite fabric is characterized by comprising the following steps of:
(1) uniformly mixing the modified polyurethane emulsion, the thickening agent, the ammonia water and the crosslinking agent to prepare the flame-retardant high-temperature-resistant coating agent, wherein the mass ratio of the modified polyurethane emulsion to the thickening agent to the ammonia water to the crosslinking agent is 90-95: 4-8: 0.5-2: 0.5 to 1;
(2) carry out the ratio with aramid fiber and stainless steel fiber, mix through the drawing on the drawing frame, then carry out draft and twisting process through fly frame and spinning frame, obtain the blended yarn, weave the blended yarn, obtain the base cloth, aramid fiber and stainless steel fiber's mass ratio is 1: 2-3;
(3) adding the modified polyurethane emulsion into a rolling groove, immersing the base cloth into the rolling groove, performing two-immersion and two-rolling, and performing pre-baking and baking processes to obtain the flame-retardant high-temperature-resistant base cloth, wherein the pre-baking temperature is 100-;
(4) uniformly coating the flame-retardant high-temperature-resistant coating agent on the surface of the flame-retardant high-temperature-resistant base fabric, placing the coated base fabric at room temperature for airing, and drying in an oven at 70-90 ℃ for 5-10h to obtain a flame-retardant high-temperature-resistant composite fabric;
the preparation method of the modified polyurethane emulsion comprises the following steps:
s1, drying polyethylene glycol by using silica gel, then adding the dried polyethylene glycol into N, N-dimethylformamide, stirring and heating to 60-70 ℃ to completely dissolve the polyethylene glycol, adding hydroxyl silicone oil and stannous octoate, heating to 60-80 ℃, and reacting for 1-2h to obtain modified polyethylene glycol;
s2, dissolving a phosphaphenanthrene compound in dichloromethane, cooling to 0-5 ℃, adding carbon tetrachloride, stirring for 10-20min, adding triethylamine and hydroxyethyl methacrylate, heating to 20-25 ℃, reacting for 10-16h, washing the reaction solution for 3 times by using deionized water, drying an organic phase by using anhydrous sodium sulfate, filtering, and concentrating and drying the filtrate under reduced pressure to obtain an intermediate I, wherein the phosphaphenanthrene compound is 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide;
s3, adding ethanol into a reaction bottle, adding diethanolamine and the intermediate I obtained in the step S2, heating to 60-70 ℃, reacting for 8-12h, washing the reaction liquid with deionized water for 3 times, and distilling an organic phase under reduced pressure to obtain an intermediate II;
s4, under the protection of nitrogen, adding isophorone diisocyanate, modified polyethylene glycol obtained in S1 and an intermediate II obtained in S3 into a reaction bottle, adding acetone, heating to 80-90 ℃ under stirring, dropwise adding dibutyltin dilaurate, and reacting for 4-6h to obtain a prepolymer I;
s5, adding dimethylolpropionic acid into the prepolymer I, heating to 80 ℃, reacting for 3-4h, adding acetone, cooling to 50-60 ℃, adding triethylamine, reacting for 0.5-1h, adding deionized water, stirring for 0.5-1h, and distilling under reduced pressure to obtain the modified polyurethane emulsion.
2. The preparation method of the flame-retardant high-temperature-resistant composite fabric according to claim 1, wherein the mass ratio of the polyethylene glycol to the hydroxy silicone oil to the stannous octoate in step S1 is 1: 0.5-2: 0.01-0.05, and 8-15mL of N, N-dimethylformamide is used per gram of polyethylene glycol.
3. The preparation method of the flame-retardant high-temperature-resistant composite fabric according to claim 1, wherein the molar ratio of the phosphaphenanthrene compound to the carbon tetrachloride to the triethylamine to the hydroxyethyl methacrylate in step S2 is 1: 1-1.5:1-1.5:1-1.2, using dichloromethane 8-15mL per gram of phosphaphenanthrene compound.
4. The preparation method of the flame-retardant high-temperature-resistant composite fabric according to claim 1, wherein the molar ratio of the diethanolamine to the intermediate I in the step S3 is 1-1.5:1, 8-15mL of ethanol is used per gram of intermediate.
5. The preparation method of the flame-retardant high-temperature-resistant composite fabric according to claim 1, wherein in the step S4, the molar ratio of isophorone diisocyanate to the modified polyethylene glycol to the intermediate bis-dibutyltin dilaurate is 1: 1-2: 0.5-1:0.01-0.05, and 5-10mL of acetone is used per gram of isophorone diisocyanate.
6. The preparation method of the flame-retardant high-temperature-resistant composite fabric according to claim 1, wherein the mass ratio of the dimethylolpropionic acid to the prepolymer I to the triethylamine in the step S5 is 1: 2-5: 0.1-0.5, 5-8mL of acetone and 3-5mL of deionized water are used for each gram of prepolymer.
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| CN113999342B (en) * | 2021-10-25 | 2022-08-12 | 厦门大学 | A kind of migratory polymer-based functional modifier and its preparation method and application |
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