JP7070805B1 - 凝固物の製造方法 - Google Patents
凝固物の製造方法 Download PDFInfo
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- JP7070805B1 JP7070805B1 JP2021553860A JP2021553860A JP7070805B1 JP 7070805 B1 JP7070805 B1 JP 7070805B1 JP 2021553860 A JP2021553860 A JP 2021553860A JP 2021553860 A JP2021553860 A JP 2021553860A JP 7070805 B1 JP7070805 B1 JP 7070805B1
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- urethane resin
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
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- 239000000701 coagulant Substances 0.000 claims abstract description 17
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 15
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- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 5
- 150000003077 polyols Chemical class 0.000 claims description 19
- 229920005862 polyol Polymers 0.000 claims description 17
- 239000005056 polyisocyanate Substances 0.000 claims description 12
- 229920001228 polyisocyanate Polymers 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
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- 239000000758 substrate Substances 0.000 claims description 6
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- 239000000463 material Substances 0.000 abstract description 18
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- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 4
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- 230000008023 solidification Effects 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
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- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 3
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- 230000033228 biological regulation Effects 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000004440 column chromatography Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 3
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- 238000003756 stirring Methods 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
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- 239000004254 Ammonium phosphate Substances 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
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- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 description 2
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
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- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 description 1
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- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- DPKBAXPHAYBPRL-UHFFFAOYSA-M tetrabutylazanium;iodide Chemical compound [I-].CCCC[N+](CCCC)(CCCC)CCCC DPKBAXPHAYBPRL-UHFFFAOYSA-M 0.000 description 1
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- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 description 1
- IBWGNZVCJVLSHB-UHFFFAOYSA-M tetrabutylphosphanium;chloride Chemical compound [Cl-].CCCC[P+](CCCC)(CCCC)CCCC IBWGNZVCJVLSHB-UHFFFAOYSA-M 0.000 description 1
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- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 description 1
- UQFSVBXCNGCBBW-UHFFFAOYSA-M tetraethylammonium iodide Chemical compound [I-].CC[N+](CC)(CC)CC UQFSVBXCNGCBBW-UHFFFAOYSA-M 0.000 description 1
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- QBVXKDJEZKEASM-UHFFFAOYSA-M tetraoctylammonium bromide Chemical compound [Br-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC QBVXKDJEZKEASM-UHFFFAOYSA-M 0.000 description 1
- SNNIPOQLGBPXPS-UHFFFAOYSA-M tetraoctylazanium;chloride Chemical compound [Cl-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC SNNIPOQLGBPXPS-UHFFFAOYSA-M 0.000 description 1
- KGPZZJZTFHCXNK-UHFFFAOYSA-M tetraoctylazanium;iodide Chemical compound [I-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC KGPZZJZTFHCXNK-UHFFFAOYSA-M 0.000 description 1
- VJFXTJZJJIZRKP-UHFFFAOYSA-M tetraphenylazanium;bromide Chemical compound [Br-].C1=CC=CC=C1[N+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 VJFXTJZJJIZRKP-UHFFFAOYSA-M 0.000 description 1
- BALCYVFFDOBQPW-UHFFFAOYSA-M tetraphenylazanium;chloride Chemical compound [Cl-].C1=CC=CC=C1[N+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 BALCYVFFDOBQPW-UHFFFAOYSA-M 0.000 description 1
- DKUNCCVNTUQRBB-UHFFFAOYSA-M tetraphenylazanium;iodide Chemical compound [I-].C1=CC=CC=C1[N+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 DKUNCCVNTUQRBB-UHFFFAOYSA-M 0.000 description 1
- AEFPPQGZJFTXDR-UHFFFAOYSA-M tetraphenylphosphanium;iodide Chemical compound [I-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 AEFPPQGZJFTXDR-UHFFFAOYSA-M 0.000 description 1
- WAGFXJQAIZNSEQ-UHFFFAOYSA-M tetraphenylphosphonium chloride Chemical compound [Cl-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 WAGFXJQAIZNSEQ-UHFFFAOYSA-M 0.000 description 1
- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 description 1
- FBEVECUEMUUFKM-UHFFFAOYSA-M tetrapropylazanium;chloride Chemical compound [Cl-].CCC[N+](CCC)(CCC)CCC FBEVECUEMUUFKM-UHFFFAOYSA-M 0.000 description 1
- GKXDJYKZFZVASJ-UHFFFAOYSA-M tetrapropylazanium;iodide Chemical compound [I-].CCC[N+](CCC)(CCC)CCC GKXDJYKZFZVASJ-UHFFFAOYSA-M 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 description 1
- NAWZSHBMUXXTGV-UHFFFAOYSA-M triethyl(hexyl)azanium;bromide Chemical compound [Br-].CCCCCC[N+](CC)(CC)CC NAWZSHBMUXXTGV-UHFFFAOYSA-M 0.000 description 1
- YAXDBEZBVYFNDT-UHFFFAOYSA-M triethyl(hexyl)azanium;chloride Chemical compound [Cl-].CCCCCC[N+](CC)(CC)CC YAXDBEZBVYFNDT-UHFFFAOYSA-M 0.000 description 1
- VGHFLAFPYDFKQN-UHFFFAOYSA-M triethyl(hexyl)azanium;iodide Chemical compound [I-].CCCCCC[N+](CC)(CC)CC VGHFLAFPYDFKQN-UHFFFAOYSA-M 0.000 description 1
- SEACXNRNJAXIBM-UHFFFAOYSA-N triethyl(methyl)azanium Chemical compound CC[N+](C)(CC)CC SEACXNRNJAXIBM-UHFFFAOYSA-N 0.000 description 1
- GRVPDGGTLNKOBZ-UHFFFAOYSA-M triethyl(methyl)azanium;bromide Chemical compound [Br-].CC[N+](C)(CC)CC GRVPDGGTLNKOBZ-UHFFFAOYSA-M 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
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- 239000002759 woven fabric Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 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
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
-
- 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
- C08G18/0838—Manufacture of polymers in the presence of non-reactive compounds
- C08G18/0842—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents
- C08G18/0861—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of a dispersing phase for the polymers or a phase dispersed in the polymers
- C08G18/0866—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of a dispersing phase for the polymers or a phase dispersed in the polymers the dispersing or dispersed phase being an aqueous medium
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Abstract
Description
オクチル酸第一錫0.1質量部の存在下、ポリエーテルポリオール(三菱化学株式会社製「PTMG2000」、数平均分子量;2,000、以下「PTMG2000」と略記する。)1,000質量部と、ポリエチレングリコール(日油株式会社製「PEG600」、数平均分子量;600、以下「PEG」と略記する。)38質量部と、ジシクロヘキシルメタンジイソシアネート(以下、「HMDI」と略記する。)262質量部とをNCO%が2.8質量%に達するまで100℃で反応させてウレタンプレポリマーA1を得た。得られたウレタンプレポリマーA1の粘度は、7,280mPa・sであった。
70℃に加熱したA1と、乳化剤としてドデシルベンゼンスルホン酸ナトリウム20質量%水溶液(第一工業製薬株式会社製「ネオゲンS-20F」)、水を二軸押出機(TEM-18SS:東芝機械製)に同時に供給、混合することで乳化液を得た。供給液それぞれの流量はA1:10kg/時、乳化剤水溶液:2.0kg/時、水:6.5kg/時、二軸押出機運転条件は50℃、260rpmであった。
その後、直ちにNCO基の95%に相当するアミノ基含量のピペラジン(以下、「PP」と略記する。)の水希釈液を添加して鎖伸長させ、最終的に不揮発分の含有率が50質量%のウレタン樹脂水分散体(1)を得た。
オクチル酸第一錫0.1質量部の存在下、PTMG2000を1,000質量部、PEG600を19質量部、HMDIを262質量部を混合し、NCO%が3.1質量%に達するまで100℃で反応させてウレタンプレポリマーA2を得た。得られたウレタンプレポリマーA2の粘度は、7,280mPa・sであった。
70℃に加熱したA2と、乳化剤としてドデシルベンゼンスルホン酸ナトリウム20質量%水溶液(第一工業製薬株式会社製「ネオゲンS-20F」)、水を二軸押出機(TEM-18SS:東芝機械製)に同時に供給、混合することで乳化液を得た。供給液それぞれの流量はA2:10kg/時、乳化剤水溶液:2.0kg/時、水:0.1kg/時、二軸押出機運転条件は50℃、260rpmであった。
その後、直ちにNCO基の95%に相当するアミノ基含量のイソホロンジアミン(以下、「IPDA」と略記する。)の水希釈液を添加して鎖伸長させ、最終的に不揮発分の含有率が60質量%のウレタン樹脂水分散体(2)を得た。
オクチル酸第一錫0.1質量部の存在下、PTMG2000を1,000質量部、PEGを18質量部、HMDIを262質量部を混合し、NCO%が3.1質量%に達するまで100℃で反応させてウレタンプレポリマーA3を得た。得られたウレタンプレポリマーA3の粘度は、7,280mPa・sであった。
70℃に加熱したA3と、乳化剤としてポリプロピレンポリエチレン共重合体(株式会社ADEKA製「プロロニックL-64」)、水を二軸押出機(TEM-18SS:東芝機械製)に同時に供給、混合することで乳化液を得た。供給液それぞれの流量はA3:10kg/時、乳化剤:0.5kg/時、水:5.8kg/時、二軸押出機運転条件は50℃、260rpmであった。
その後、直ちにNCO基の95%に相当するアミノ基含量のIPDAの水希釈液を添加して鎖伸長させ、最終的に不揮発分の含有率が50質量%のウレタン樹脂水分散体(3)を得た。
オクチル酸第一錫0.1質量部の存在下、PTMG2000を1,000質量部、PEGを18質量部、HMDIを262質量部を混合し、NCO%が3.1質量%に達するまで100℃で反応させてウレタンプレポリマーA4を得た。得られたウレタンプレポリマーA4の粘度は、7,280mPa・sであった。
70℃に加熱したA4と、乳化剤としてドデシルベンゼンスルホン酸ナトリウム20質量%水溶液(第一工業製薬株式会社製「ネオゲンS-20F」)、ポリプロピレンポリエチレン共重合体(株式会社ADEKA製「プロロニックL-64」)、水を二軸押出機(TEM-18SS:東芝機械製)に同時に供給、混合することで乳化液を得た。供給液それぞれの流量はA5:10kg/時、乳化剤水溶液S-20F:1.3kg/時、乳化剤L-64:0.3kg/時、水:2.4kg/時、二軸押出機運転条件は50℃、260rpmであった。
その後、直ちにNCO基の95%に相当するアミノ基含量のエチレンジアミン(以下「EA」と略記する。)の水希釈液を添加して鎖伸長させ、最終的に不揮発分の含有率が60質量%のウレタン樹脂水分散体(4)を得た。
オクチル酸第一錫0.1質量部の存在下、ポリカーボネートジオールポリオール(宇部興産株式会社製「ETERNACOLL UH-200」、数平均分子量;2,000)1,000質量部と、PEG38質量部と、HMDI262質量部とをNCO%が2.8質量%に達するまで100℃で反応させてウレタンプレポリマーA5を得た。得られたウレタンプレポリマーA5の粘度は、29,000mPa・sであった。
70℃に加熱したA5と、乳化剤としてドデシルベンゼンスルホン酸ナトリウム20質量%水溶液(第一工業製薬株式会社製「ネオゲンS-20F」)、水を二軸押出機(TEM-18SS:東芝機械製)に同時に供給、混合することで乳化液を得た。供給液それぞれの流量はA1:10kg/時、乳化剤水溶液:2.0kg/時、水:6.5kg/時、二軸押出機運転条件は50℃、260rpmであった。
その後、直ちにNCO基の95%に相当するアミノ基含量のPPの水希釈液を添加して鎖伸長させ、最終的に不揮発分の含有率が50質量%のウレタン樹脂水分散体(5)を得た。
オクチル酸第一錫0.1質量部の存在下、PTMG2000を1,000質量部、ジメチロールプロピオン酸(以下「DMPA」と略記する。)を18質量部、HMDIを262質量部を混合し、NCO%が2.4質量%に達するまで100℃で反応させてウレタンプレポリマーB1を得た。得られたウレタンプレポリマーB1の粘度は、949,000mPa・sであった。
70℃に加熱したB1と、中和剤としてトリエチルアミン、乳化剤としてポリプロピレンポリエチレン共重合体(株式会社ADEKA製「プロロニックL-64」)、水を二軸押出機(TEM-18SS:東芝機械製)に同時に供給、混合することで乳化液を得た。供給液それぞれの流量はA5:10kg/時、中和剤:0.1kg/時、乳化剤L-64:0.3kg/時、水:8.5kg/時、二軸押出機運転条件は50℃、260rpmであった。
その後、直ちにNCO基の95%に相当するアミノ基含量のピペラジン(以下「PP」と略記する。)の水希釈液を添加して鎖伸長させ、最終的に不揮発分の含有率が50質量%のウレタン樹脂水分散体(R1)を得た。
得られたウレタン樹脂水分散体(1)~(3)それぞれ1,000質量部に、イオン交換水を加え、固形分が30質量%となるように調整し、さらに増粘剤(Borchers社製「Borchi Gel L75N」10質量部を加え、メカニカルミキサーを2,000rpmにて攪拌した配合液を作製した。
次いで、ポリエステル繊維不織布(目付250g/m2)を前記配合液に含浸させた後、ゴムローラーマングルを用いて含浸量が200%となるように不要な配合液を搾り取った。次いで、配合液を含ませた不織布を25℃の5質量%塩化ナトリウム水溶液の凝固浴(以下「NaCl」と略記する。)に3分間浸漬させて、ウレタン樹脂を凝固させた。更に凝固後の加工布に水をかけ流しながら、ゴムローラーマングルで10回絞り水洗した。最後に、120℃の熱風乾燥機にて30分乾燥させて凝固物を有する繊維基材を得た。
得られたウレタン樹脂水分散体(4)~(5)それぞれ1,000質量部に、イオン交換水を加え、固形分が30質量%となるように調整し、さらに増粘剤(Borchers社製「Borchi Gel L75N」10質量部を加え、メカニカルミキサーを2,000rpmにて攪拌した配合液を作製した。
次いで、ポリエステル繊維不織布(目付250g/m2)を前記配合液に含浸させた後、ゴムローラーマングルを用いて含浸量が200%となるように不要な配合液を搾り取った。次いで、配合液を含ませた不織布を25℃の5質量%の硫酸アンモニウム水溶液の凝固浴(以下「硫酸アンモニウム」と略記する。)に3分間浸漬させて、ウレタン樹脂を凝固させた。更に凝固後の加工布に水をかけ流しながら、ゴムローラーマングルで10回絞り水洗した。最後に、120℃の熱風乾燥機にて30分乾燥させて凝固物を有する繊維基材を得た。
得られたウレタン樹脂水分散体(1)1,000質量部に、イオン交換水を加え、固形分が30質量%となるように調整し、さらに増粘剤(Borchers社製「Borchi Gel L75N」10質量部を加え、メカニカルミキサーを2,000rpmにて攪拌した配合液を作製した。
次いで、ポリエステル繊維不織布(目付250g/m2)を前記配合液に含浸させた後、120℃の熱風乾燥機にて30分加熱乾燥することにより感熱凝固させた繊維基材を得た。
得られたウレタン樹脂水分散体(R1)1,000質量部に、実施例1~4と同様にイオン交換水を加え、固形分が30質量%となるように調整し、さらに架橋剤(日清紡ケミカル社製「カルボジライトV-02-L2」)50質量部、増粘剤(Borchers社製「Borchi Gel L75N」)10質量部を加え、メカニカルミキサーを2,000rpmにて攪拌した配合液を作製した。
次いで、実施例1~4と同様の加工を実施し、凝固物を有する繊維基材を得た。
合成例及び比較合成例で用いたポリオール等の数平均分子量は、ゲル・パーミエーション・カラムクロマトグラフィー(GPC)法により、下記の条件で測定し得られた値を示す。
カラム:東ソー株式会社製の下記のカラムを直列に接続して使用した。
「TSKgel G5000」(7.8mmI.D.×30cm)×1本
「TSKgel G4000」(7.8mmI.D.×30cm)×1本
「TSKgel G3000」(7.8mmI.D.×30cm)×1本
「TSKgel G2000」(7.8mmI.D.×30cm)×1本
検出器:RI(示差屈折計)
カラム温度:40℃
溶離液:テトラヒドロフラン(THF)
流速:1.0mL/分
注入量:100μL(試料濃度0.4質量%のテトラヒドロフラン溶液)
標準試料:下記の標準ポリスチレンを用いて検量線を作成した。
東ソー株式会社製「TSKgel 標準ポリスチレン A-500」
東ソー株式会社製「TSKgel 標準ポリスチレン A-1000」
東ソー株式会社製「TSKgel 標準ポリスチレン A-2500」
東ソー株式会社製「TSKgel 標準ポリスチレン A-5000」
東ソー株式会社製「TSKgel 標準ポリスチレン F-1」
東ソー株式会社製「TSKgel 標準ポリスチレン F-2」
東ソー株式会社製「TSKgel 標準ポリスチレン F-4」
東ソー株式会社製「TSKgel 標準ポリスチレン F-10」
東ソー株式会社製「TSKgel 標準ポリスチレン F-20」
東ソー株式会社製「TSKgel 標準ポリスチレン F-40」
東ソー株式会社製「TSKgel 標準ポリスチレン F-80」
東ソー株式会社製「TSKgel 標準ポリスチレン F-128」
東ソー株式会社製「TSKgel 標準ポリスチレン F-288」
東ソー株式会社製「TSKgel 標準ポリスチレン F-550」
実施例及び比較例で得られたウレタン樹脂水分散体をレーザー回折/散乱式粒度分布測定装置(株式会社堀場製作所製「LA-910」)を使用して、分散液として水を使用し、相対屈折率=1.10、粒子径基準が面積の時の平均粒子径を測定した。
得られた加工布を触感により以下のように評価した。
「A」;腰感、充実感ともに特に優れている。
「B」;腰感があり、充実感も感じられる。
「C」;腰感、充実感にやや劣る。
「D」;腰感、充実感が全く感じられない。
攪拌翼を有するSUS製セパラブルフラスコに1質量%水酸化ナトリウム水溶液を入れ、95℃に加熱した。フラスコ内に加工布を入れ、30分、50rpmで攪拌した。その後、含浸加工布を取り出し、加工布に水をかけ流しながら、ゴムローラーマングルで10回絞り水洗した。最後に、120℃の熱風乾燥機にて30分乾燥させた繊維基材を触感により評価した。
「A」;腰感、充実感ともに特に優れている。
「B」;腰感があり、充実感も感じられる。
「C」;腰感、充実感にやや劣る。
「D」;腰感、充実感が全く感じられない。
PTFE製耐圧容器中に5質量%かつpH4.5の0.5M酢酸ナトリウム緩衝液と前記[耐アルカリ性の評価方法]の試験後の加工布を入れ、120℃で24時間加熱した。その後、取り出した加工布に水をかけ流しながら、ゴムローラーマングルで10回絞り水洗した。最後に、120℃の熱風乾燥機にて30分乾燥させた繊維基材を触感により評価した。
「A」;腰感、充実感ともに特に優れている。
「B」;腰感があり、充実感も感じられる。
「C」;腰感、充実感にやや劣る。
「D」;腰感、充実感が全く感じられない。
Claims (1)
- 繊維基材に、ノニオン性基を有する化合物(a1)、ポリオール(a3)、及び、ポリイソシアネート(a4)を必須原料としたウレタン樹脂(X)の水分散体を含浸させ、次いで、凝固剤(Y)に浸漬させる凝固物の製造方法であり、前記化合物(a1)が、数平均分子量が300~600の範囲のポリエチレングリコール(前記ウレタン樹脂(X)の側鎖として導入されるものを除く。)であり、その使用率が、ウレタン樹脂(X)を構成する原料の合計質量中0.25質量%以上5質量%以下であり、前記凝固剤(Y)が、金属化合物(Y1)、酸化合物(Y2)、及び、前記酸化合物(Y2)以外の非金属化合物(Y3)からなる群より選ばれる1種以上であることを特徴とする凝固物の製造方法。
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