JP2014151233A - Agitating device having attachment removing jig - Google Patents
Agitating device having attachment removing jig Download PDFInfo
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- JP2014151233A JP2014151233A JP2013020253A JP2013020253A JP2014151233A JP 2014151233 A JP2014151233 A JP 2014151233A JP 2013020253 A JP2013020253 A JP 2013020253A JP 2013020253 A JP2013020253 A JP 2013020253A JP 2014151233 A JP2014151233 A JP 2014151233A
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- Prior art keywords
- tert
- acid
- stirrer
- butyl
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- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 12
- -1 pyrophosphoric acid compound Chemical class 0.000 claims description 57
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 17
- 235000011007 phosphoric acid Nutrition 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 238000006482 condensation reaction Methods 0.000 claims description 7
- 235000011180 diphosphates Nutrition 0.000 claims description 4
- 229940048084 pyrophosphate Drugs 0.000 claims description 4
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 2
- 238000003756 stirring Methods 0.000 description 40
- 229910052751 metal Inorganic materials 0.000 description 26
- 239000002184 metal Substances 0.000 description 26
- 239000000047 product Substances 0.000 description 14
- 229920000642 polymer Polymers 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 9
- 125000003118 aryl group Chemical group 0.000 description 9
- 235000014113 dietary fatty acids Nutrition 0.000 description 9
- 239000000194 fatty acid Substances 0.000 description 9
- 229930195729 fatty acid Natural products 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 239000007983 Tris buffer Substances 0.000 description 8
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 150000004665 fatty acids Chemical class 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 6
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 6
- 239000012964 benzotriazole Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 229910000000 metal hydroxide Inorganic materials 0.000 description 5
- 150000004692 metal hydroxides Chemical class 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 125000001931 aliphatic group Chemical group 0.000 description 4
- 239000003963 antioxidant agent Substances 0.000 description 4
- 235000006708 antioxidants Nutrition 0.000 description 4
- 239000002216 antistatic agent Substances 0.000 description 4
- 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 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 150000004985 diamines Chemical group 0.000 description 4
- 239000003925 fat Substances 0.000 description 4
- 235000019197 fats Nutrition 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
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- RTWNYYOXLSILQN-UHFFFAOYSA-N methanediamine Chemical compound NCN RTWNYYOXLSILQN-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000008065 acid anhydrides Chemical class 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- ZJIPHXXDPROMEF-UHFFFAOYSA-N dihydroxyphosphanyl dihydrogen phosphite Chemical compound OP(O)OP(O)O ZJIPHXXDPROMEF-UHFFFAOYSA-N 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical class CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 235000019198 oils Nutrition 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 150000004671 saturated fatty acids Chemical class 0.000 description 3
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 3
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 2
- BVUXDWXKPROUDO-UHFFFAOYSA-N 2,6-di-tert-butyl-4-ethylphenol Chemical compound CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 BVUXDWXKPROUDO-UHFFFAOYSA-N 0.000 description 2
- ONTODYXHFBKCDK-UHFFFAOYSA-N 2-(2,4-dimethylphenyl)-1,3,5-triazine Chemical compound CC1=CC(C)=CC=C1C1=NC=NC=N1 ONTODYXHFBKCDK-UHFFFAOYSA-N 0.000 description 2
- SZAQZZKNQILGPU-UHFFFAOYSA-N 2-[1-(2-hydroxy-3,5-dimethylphenyl)-2-methylpropyl]-4,6-dimethylphenol Chemical compound C=1C(C)=CC(C)=C(O)C=1C(C(C)C)C1=CC(C)=CC(C)=C1O SZAQZZKNQILGPU-UHFFFAOYSA-N 0.000 description 2
- MQWCQFCZUNBTCM-UHFFFAOYSA-N 2-tert-butyl-6-(3-tert-butyl-2-hydroxy-5-methylphenyl)sulfanyl-4-methylphenol Chemical compound CC(C)(C)C1=CC(C)=CC(SC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O MQWCQFCZUNBTCM-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 2
- OJGMBLNIHDZDGS-UHFFFAOYSA-N N-Ethylaniline Chemical compound CCNC1=CC=CC=C1 OJGMBLNIHDZDGS-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 235000019482 Palm oil Nutrition 0.000 description 2
- 241001483078 Phyto Species 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 125000002252 acyl group Chemical group 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 125000002723 alicyclic group Chemical group 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- GCAIEATUVJFSMC-UHFFFAOYSA-N benzene-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1C(O)=O GCAIEATUVJFSMC-UHFFFAOYSA-N 0.000 description 2
- FQUNFJULCYSSOP-UHFFFAOYSA-N bisoctrizole Chemical compound N1=C2C=CC=CC2=NN1C1=CC(C(C)(C)CC(C)(C)C)=CC(CC=2C(=C(C=C(C=2)C(C)(C)CC(C)(C)C)N2N=C3C=CC=CC3=N2)O)=C1O FQUNFJULCYSSOP-UHFFFAOYSA-N 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
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- 239000000292 calcium oxide Substances 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000003484 crystal nucleating agent Substances 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 2
- 125000005462 imide group Chemical group 0.000 description 2
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 235000012245 magnesium oxide Nutrition 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 2
- 239000002530 phenolic antioxidant Substances 0.000 description 2
- ZQBAKBUEJOMQEX-UHFFFAOYSA-N phenyl salicylate Chemical compound OC1=CC=CC=C1C(=O)OC1=CC=CC=C1 ZQBAKBUEJOMQEX-UHFFFAOYSA-N 0.000 description 2
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- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 2
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- QEDNBHNWMHJNAB-UHFFFAOYSA-N tris(8-methylnonyl) phosphite Chemical compound CC(C)CCCCCCCOP(OCCCCCCCC(C)C)OCCCCCCCC(C)C QEDNBHNWMHJNAB-UHFFFAOYSA-N 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
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- UDZNBVQPXCTQBH-UHFFFAOYSA-N (1-dihydroxyphosphanylbiphenylen-2-yl)phosphonous acid Chemical compound C1=CC=C2C3=C(P(O)O)C(P(O)O)=CC=C3C2=C1 UDZNBVQPXCTQBH-UHFFFAOYSA-N 0.000 description 1
- GRKDVZMVHOLESV-UHFFFAOYSA-N (2,3,4,5,6-pentabromophenyl)methyl prop-2-enoate Chemical compound BrC1=C(Br)C(Br)=C(COC(=O)C=C)C(Br)=C1Br GRKDVZMVHOLESV-UHFFFAOYSA-N 0.000 description 1
- ZSVFYHKZQNDJEV-UHFFFAOYSA-N (2,3,4-tribromophenyl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=C(Br)C(Br)=C1Br ZSVFYHKZQNDJEV-UHFFFAOYSA-N 0.000 description 1
- BUPRYTFTHBNSBD-UHFFFAOYSA-N (2,3,4-tribromophenyl) prop-2-enoate Chemical compound BrC1=CC=C(OC(=O)C=C)C(Br)=C1Br BUPRYTFTHBNSBD-UHFFFAOYSA-N 0.000 description 1
- POLKDMBEUGQWPE-UHFFFAOYSA-N (2,4,6-tritert-butylphenyl) dihydrogen phosphate Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=C(OP(O)(O)=O)C(C(C)(C)C)=C1 POLKDMBEUGQWPE-UHFFFAOYSA-N 0.000 description 1
- KZGROEDUAFPSGN-UHFFFAOYSA-N (2,4-ditert-butylphenyl) dihydrogen phosphate Chemical compound CC(C)(C)C1=CC=C(OP(O)(O)=O)C(C(C)(C)C)=C1 KZGROEDUAFPSGN-UHFFFAOYSA-N 0.000 description 1
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- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
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Abstract
Description
本発明は、加熱部位で内容物を加熱しながら撹拌し、内容物に含まれる水分若しくは溶媒又は内容物の反応によって生じる水、アルコール若しくは揮発分を除去する撹拌装置において、加熱部位で生成する付着物を除去する冶具を具えた撹拌装置に関する。 The present invention stirs while heating the contents at the heating site, and removes water, alcohol, or volatile matter generated by the reaction of the moisture or solvent contained in the content or the contents, and the generated product at the heating site. The present invention relates to a stirring device including a jig for removing a kimono.
内容物を加熱しながら撹拌する手段としては、
(1)加熱部位を有する容器そのものを回転させることにより内容物を撹拌する方法、
(2)加熱部位を有する容器そのものを振動させることにより内容物を撹拌する方法、
(3)加熱部位を有する容器内に備えられた撹拌機を回転させることにより内容物を撹拌する方法、
(4)加熱部位を有する容器内に備えられた振動体を振動させることにより内容物を撹拌する方法、
(5)加熱部位を有する容器内に旋回流等の気流を発生させて内容物を撹拌する方法、
等が挙げられる。
本発明は、内容物を加熱しながら撹拌する手段として、上記の(3)の撹拌手段を採用した撹拌装置に関するものである。撹拌機には、羽根を有する構造のものが多いが、羽根と容器の内壁との間の空隙部分で内容物が膜状に堆積し、収率が低くなるという問題がある。また、連続運転の場合は、容器の入り口から出口まで内容物がスムーズに移動することが重要であり、容器の内部に付着物が生成するのは致命的で長時間の安定運転を達成することができない。
As a means of stirring the contents while heating,
(1) A method of stirring the contents by rotating the container itself having a heating part,
(2) A method of stirring the contents by vibrating the container itself having a heating part,
(3) A method of stirring the contents by rotating a stirrer provided in a container having a heating part,
(4) A method of stirring the contents by vibrating a vibrating body provided in a container having a heating part,
(5) A method of stirring the contents by generating an air flow such as a swirling flow in a container having a heating part,
Etc.
The present invention relates to an agitation apparatus that employs the agitation means (3) as a means for agitating the contents while heating. Many of the stirrers have a structure having blades, but there is a problem that the content is deposited in a film shape in a gap portion between the blades and the inner wall of the container, resulting in a low yield. Also, in continuous operation, it is important that the contents move smoothly from the entrance to the exit of the container, and deposits are generated inside the container to achieve a fatal and long-term stable operation. I can't.
内容物を加熱しながら撹拌する撹拌装置としては、例えば、コニカルドライヤー、ナウターミキサー、パドルドライヤー、ダブルディスクドライヤー、ロータリードライヤー等が挙げられる。
これらにおいて、溝型撹拌装置として知られているパドルドライヤーは、熱風、伝熱による加熱手段を有し、容器内部に取り付けられたパドル羽根が回転することによって内容物を撹拌しながら、製品排出口へ送り出すことができる撹拌装置である。パドルドライヤーは、微粉、顆粒、ペレット状、フレーク状等、粒径や粒子形状の制限なく利用することが可能であり、高含水率物質、泥状物質の処理、ポリマーの重合や改質処理にも利用されており、合成樹脂、汚泥、食品、化成品等、幅広い分野で使用されている。
Examples of the stirring device that stirs while heating the contents include a conical dryer, a nauter mixer, a paddle dryer, a double disc dryer, and a rotary dryer.
In these, the paddle dryer known as a groove type stirring device has a heating means by hot air and heat transfer, and the product discharge port while stirring the contents by rotating paddle blades attached inside the container. The stirring device can be sent to Paddle dryers can be used without restrictions on particle size and particle shape, such as fine powder, granules, pellets, flakes, etc., and can be used for treatment of high moisture content substances, mud substances, polymer polymerization and modification treatment. It is also used in a wide range of fields such as synthetic resin, sludge, food, and chemical products.
パドルドライヤーの使用例としては、例えば、特許文献1では、芳香族ポリカーボネートの重縮合を行っている。特許文献2では、オルトリン酸メラミンを脱水縮合させている。特許文献3では、スラリー状のリン酸二ナトリウム水溶液を乾燥させている。 As an example of using a paddle dryer, for example, in Patent Document 1, polycondensation of an aromatic polycarbonate is performed. In Patent Document 2, melamine orthophosphate is subjected to dehydration condensation. In Patent Document 3, a slurry-like disodium phosphate aqueous solution is dried.
また、特許文献4では、撹拌機の羽根の終端に、かき揚げ板を装着した撹拌装置が提案されている。 Moreover, in patent document 4, the stirring apparatus which mounted | wore the scraper board at the terminal of the blade | wing of a stirrer is proposed.
しかし、内容物(材料又は生成物等)が粘着性である場合、内容物が、撹拌装置の内壁や内容物を製品排出口へ送り出す羽根に付着したり、内容物同士でブロッキングしたりする場合があった。 However, when the contents (materials or products) are sticky, the contents may adhere to the inner wall of the agitator or the blade that feeds the contents to the product discharge port, or the contents may block each other. was there.
特に、内容物が脱水縮合反応する物質の場合、反応で生成する水が付着物を形成し、この付着物が更に内容物を取り込み巨大化することにより、撹拌装置内部で閉塞したり、撹拌機への負荷が上昇したりして連続運転が困難であった。特許文献4に記載の撹拌型乾燥装置を用いた場合も付着物の処理が不十分であり、付着物が堆積して伝熱効率が低下し、反応処理が不十分になる場合があり、改良の余地があった。 In particular, when the content is a substance that undergoes a dehydration condensation reaction, the water produced by the reaction forms an adhering substance, and this adhering substance further entraps the contents and enlarges it. Continuous operation was difficult due to an increase in the load on the vehicle. Even when the stirring type drying apparatus described in Patent Document 4 is used, the treatment of the adhering matter is insufficient, the adhering matter is accumulated, the heat transfer efficiency is lowered, and the reaction process may be insufficient. There was room.
従って、本発明の目的は、撹拌装置において、内容物の閉塞を防止し、撹拌機への負荷の上昇を抑制し、内容物の反応を向上させ、且つ長時間の連続運転を達成できる撹拌装置を提供することにある。 Accordingly, an object of the present invention is to provide a stirrer capable of preventing clogging of the contents, suppressing an increase in load on the stirrer, improving the reaction of the contents, and achieving a continuous operation for a long time. Is to provide.
本発明者は、上記目的を達成すべく鋭意検討した結果、撹拌機の羽根の両端を冶具で挟設することにより、上記目的を達成できることを見出した。 As a result of intensive studies to achieve the above object, the present inventor has found that the above object can be achieved by sandwiching both ends of a blade of a stirrer with a jig.
すなわち、本発明は、撹拌機、加熱手段及びこれらを収容する容器を備え、該容器内に投入された内容物を該加熱手段により加熱しながら該撹拌機により撹拌することにより、該内容物に含まれる水分若しくは溶媒又は該内容物の反応によって生じる水、アルコール若しくは揮発分を除去する撹拌装置において、
上記撹拌機が羽根を有する構造であって、該羽根を挟接する冶具を備えることに特徴を有する撹拌装置を提供するものである。
That is, the present invention comprises a stirrer, a heating means, and a container for storing these, and the contents put in the container are stirred by the stirrer while being heated by the heating means, whereby the contents are added. In a stirrer that removes water, alcohol, or volatile matter generated by the reaction of water or solvent contained therein or the contents thereof,
The stirrer has a structure having blades, and provides a stirring device characterized by including a jig for sandwiching the blades.
本発明の撹拌装置は、上記羽根を挟接する冶具が、2本の棒状の形状又は2枚の板状で形成されるものが好ましい。 In the stirring device of the present invention, it is preferable that the jig for sandwiching the blade is formed in two rod-like shapes or two plate-like shapes.
また、本発明は、上記撹拌装置を用いて、オルトリン酸化合物を、120〜350℃の温度条件下で脱水縮合反応させてなるピロリン酸化合物の製造方法を提供するものである。 Moreover, this invention provides the manufacturing method of the pyrophosphoric acid compound formed by carrying out dehydration condensation reaction of the orthophosphoric acid compound on the temperature conditions of 120-350 degreeC using the said stirring apparatus.
また、本発明は、撹拌機、加熱手段及びこれらを収容する容器を備え、該容器内に投入されたオルトリン酸化合物を加熱手段により、120〜350℃の温度条件下になるように加熱しながら該撹拌機により撹拌することにより、該オルトリン酸化合物に含まれる水分若しくは溶媒又は該オルトリン酸化合物の反応によって生じる水、アルコール又は揮発分を除去する製造装置において、
上記撹拌機が羽根を有する構造であって、該羽根を挟接する冶具を備えることに特徴を有するピロリン酸化合物の製造装置を提供するものである。
The present invention also comprises a stirrer, a heating means and a container for storing them, while heating the orthophosphoric acid compound charged in the container to a temperature condition of 120 to 350 ° C. by the heating means. In the production apparatus for removing water, alcohol or volatile matter produced by the reaction of the water or solvent contained in the orthophosphoric acid compound or the reaction of the orthophosphoric acid compound by stirring with the stirrer,
The stirrer has a structure having blades, and provides an apparatus for producing a pyrophosphate compound characterized by including a jig for sandwiching the blades.
本発明の撹拌装置によれば、撹拌装置内における内容物の閉塞を防止し、撹拌機への負荷の上昇を抑制し、内容物の反応を向上させ、且つ長時間の連続運転を達成できる。 According to the stirring device of the present invention, it is possible to prevent clogging of the contents in the stirring device, suppress an increase in the load on the stirrer, improve the reaction of the contents, and achieve a continuous operation for a long time.
本発明の撹拌装置について、以下に詳述する。
本発明の撹拌装置は、撹拌機、加熱手段及びこれらを収容する容器を備えており、該撹拌機は、羽根を有する構造であり、通常、該羽根を軸架する回転軸を有している。
The stirring device of the present invention will be described in detail below.
The stirrer of the present invention includes a stirrer, a heating means, and a container that accommodates the stirrer, and the stirrer has a structure having blades, and usually has a rotating shaft that supports the blades. .
上記羽根を有する構造の撹拌機において、上記羽根は、特に限定なく一般的なものを用いることができ、例えば、パドル型、傾斜パドル型、デスクタービン型、湾曲羽根タービン型、ブルマージン型、アンカー型、ヘリカル型、スクリュー型、スタティックミキサー型等が挙げられ、それらを変形したものや複合したものが挙げられる。 In the stirrer having a structure having the above blades, a general blade can be used without particular limitation. For example, a paddle type, an inclined paddle type, a desk turbine type, a curved blade turbine type, a bull margin type, an anchor Examples include a mold, a helical type, a screw type, a static mixer type, and the like.
また、上記羽根は、シリカ、アルミナ、ジルコニア、炭化ケイ素等のセラミックパウダーや、窒化チタン、炭窒化チタン、チタンアルミナイトライド、アルミクロムナイトライド、クロムナイトライド、ダイヤモンドライクカーボン等の硬質物質で被覆されていてもよい。 The blades are coated with ceramic powder such as silica, alumina, zirconia, silicon carbide, and hard materials such as titanium nitride, titanium carbonitride, titanium aluminum nitride, aluminum chrome nitride, chrome nitride, diamond-like carbon, etc. May be.
上記撹拌機において、上記羽根は、上記回転軸と直接又は連結具により接続される。羽根と回転軸は、連通した中空構造であるものが好ましい。連結具がある場合は、連結具を含めて連通するものが好ましい。中空部分に熱媒体を充填したり、中空部分に通電、発熱構造を組み込んだ構造とすることが可能となり、内容物を効率よく、また均等に加熱することができる。 In the agitator, the blade is connected to the rotating shaft directly or by a coupling tool. It is preferable that the blade and the rotating shaft have a hollow structure in communication. When there is a connector, it is preferable to communicate with the connector. The hollow portion can be filled with a heat medium, or the hollow portion can be energized and a heat generating structure can be incorporated, and the contents can be efficiently and evenly heated.
上記加熱手段としては、熱風、蒸気、伝熱等の加熱方法が挙げられる。 Examples of the heating means include heating methods such as hot air, steam, and heat transfer.
上記撹拌装置に用いられる容器は、サイズ、形状、材質等特に限定することなく用いることができるが、耐熱性を有するものが好ましい。また、通常、反応槽として用いられるものであってもよい。 Although the container used for the said stirring apparatus can be used without specifically limiting size, a shape, a material, etc., what has heat resistance is preferable. Moreover, what is normally used as a reaction tank may be used.
上記容器内に投入された内容物は、上記加熱手段により加熱されながら上記撹拌機により撹拌されることにより、上記内容物に含まれる水分若しくは溶媒又は該内容物の反応によって生じる水、アルコール若しくは揮発分が除去される。
上記内容物に含まれる水分若しくは溶媒又は該内容物の反応によって生じる水、アルコール若しくは揮発分を除去する装置としては、本発明の撹拌装置から、水分やアルコール及び揮発成分を排出できる設備を有していればよく、例えば、撹拌装置の上部に、ガス排出口を設けたものが挙げられ、ガス排出口は、単独又は複数有するものであってもよい。
The contents thrown into the container are stirred by the stirrer while being heated by the heating means, whereby water or a solvent contained in the contents or water, alcohol or volatilization caused by the reaction of the contents. Minutes are removed.
As a device for removing water or solvent contained in the contents or water, alcohol or volatile matter generated by the reaction of the contents, it has equipment capable of discharging moisture, alcohol and volatile components from the stirring device of the present invention. What is necessary is just to have, for example, what provided the gas exhaust port in the upper part of the stirring apparatus is mentioned, and the gas exhaust port may have single or multiple.
上記羽根は、該羽根を挟接する冶具を備えている。
上記冶具としては、形状及び材質は特に制限無く用いることができるが、金属製であるものが好ましい。撹拌装置の損傷・摩耗を防止する観点から、羽根の材質よりも剛性が低い材質であるものが好ましい。また、撹拌装置の加熱温度以上の耐熱性を有するものが好ましい。
The blade includes a jig for sandwiching the blade.
As the jig, the shape and material can be used without particular limitation, but those made of metal are preferable. From the viewpoint of preventing the stirrer from being damaged or worn, a material having a lower rigidity than the blade material is preferable. Moreover, what has heat resistance more than the heating temperature of a stirring apparatus is preferable.
上記冶具の具体例としては、図2〜図4に示されるような2本の棒状の形状で形成されるものや、図5〜図7に示されるような2枚の板状の形状で形成されるものや、図8に示すような多数の板状の形状で形成されるものが挙げられる。
上記冶具が棒状である場合、棒の径は、3〜7mmであることが好ましく、また、上記冶具が板状である場合、板の厚みは、2〜4mmであることが好ましい。
As a specific example of the above-mentioned jig, it is formed in two rod-like shapes as shown in FIGS. 2 to 4 or formed in two plate-like shapes as shown in FIGS. And those formed in a number of plate shapes as shown in FIG.
When the jig is rod-shaped, the diameter of the rod is preferably 3 to 7 mm. When the jig is plate-shaped, the thickness of the plate is preferably 2 to 4 mm.
また、本発明の撹拌装置の前後において、内容物の乾燥装置、内容物の冷却装置を備え付けてもよい。 Moreover, you may equip the content drying apparatus and the content cooling device before and behind the stirring apparatus of this invention.
上記乾燥装置としては、内容物に含まれる水分やアルコール等の脱水又は揮発成分を除去できるものであれば特に限定されず、例えば、内容物を加熱したり、内容物を気流環境下にしたりするものや、内容物を減圧下に調整可能な機構を有するものが挙げられる。 The drying device is not particularly limited as long as it can remove dehydration or volatile components such as moisture and alcohol contained in the content, and for example, heats the content or puts the content in an air flow environment. And those having a mechanism capable of adjusting the contents under reduced pressure.
上記冷却装置としては、内容物を冷却できるものであれば特に限定されず、例えば、中空構造の羽根に水等の冷媒を流して、内容物を撹拌しながら冷却するものや、内容物に空気を送り込んで冷却する機構を有するものが挙げられる。 The cooling device is not particularly limited as long as the contents can be cooled. For example, a cooling device such as water flowing through a hollow blade is used to cool the contents while stirring. And a mechanism having a mechanism for cooling by feeding.
以下、本発明の実施の形態を好適な実施の形態として例示する撹拌装置に基づいて詳細に説明する。
図1は、撹拌機と加熱手段を備えた伝導伝熱方式の撹拌装置を水平方向で見た一部遮断全体構成図である。1は比較的横に長い容器からなる撹拌装置のケーシングであり、該ケーシング1は、後述するカバー体3を有し、全体が断面視略U字状に形成され、更に、ケーシング1の底面及び側面域を覆って、熱交換用の媒体循環路11を形成するジャケット12が設けられている。
ジャケット12の左右両端部には、熱媒入口13と熱媒出口14が設けられ、所定温度の加熱媒体(温水・蒸気)は媒体循環路11内を循環させてケーシング1を加熱する。
Hereinafter, based on the stirring apparatus which illustrates embodiment of this invention as suitable embodiment, it demonstrates in detail.
FIG. 1 is a partially cut-off overall configuration diagram of a conduction heat transfer type stirring device provided with a stirrer and a heating means when viewed in the horizontal direction. 1 is a casing of a stirrer composed of a relatively long container. The casing 1 has a cover body 3 which will be described later, and is entirely formed in a substantially U shape in a sectional view. A jacket 12 is provided to cover the side area and form a medium circulation path 11 for heat exchange.
A heat medium inlet 13 and a heat medium outlet 14 are provided at both left and right ends of the jacket 12, and a heating medium (hot water / steam) having a predetermined temperature is circulated in the medium circulation path 11 to heat the casing 1.
上記ケーシング1内には、前後に並列して、中空扇形の羽根21を有する中空回転軸2が、各々両側部を貫通した状態で回転可能に軸架されており、羽根21と回転軸2は互いの中空部が連通した構成となっている。羽根21及び回転軸2の材質は、ステンレス製(SUS304)である。 In the casing 1, a hollow rotary shaft 2 having hollow fan-shaped blades 21 arranged in parallel in the front-rear direction is rotatably mounted in a state of penetrating both sides, and the blades 21 and the rotary shaft 2 are It is the structure which the mutual hollow part connected. The material of the blades 21 and the rotating shaft 2 is made of stainless steel (SUS304).
上記回転軸2は、ケーシング外部側において、一方の回転軸2に設けたスプロケット23と駆動モータのスプロケット24をチェーン25により連動連結し、それぞれに設けられたギア22を交互に歯合させ、相互に逆回転する構成となっている。また、回転軸2の両端部には、加熱媒体(蒸気、温水等)を導入循環するためのロータリージョイント26、27が設けられており、羽根21と回転軸2が加熱体として機能するようになっている。 The rotary shaft 2 has a sprocket 23 provided on one rotary shaft 2 and a sprocket 24 of a drive motor interlockingly connected by a chain 25 on the outer side of the casing. It is the structure which reversely rotates. Further, rotary joints 26 and 27 for introducing and circulating a heating medium (steam, hot water, etc.) are provided at both ends of the rotary shaft 2 so that the blades 21 and the rotary shaft 2 function as a heating body. It has become.
回転軸2の両端部において、左側端部に原料投入口31、右側端部に製品排出口33がそれぞれ設けられており、羽根体21と回転軸2の回転によって、原料投入口31から投入された原料は、製品排出口33へ向かって移動し、回転軸2、羽根21及び媒体循環路11からの伝導伝熱により加熱され、反応や乾燥作用を受けて、製品排出口33から排出される。乾燥処理に伴い、内容物に含まれる水分、又は反応によって生じた水分、アルコール又は揮発分は、ケーシング1の上部に設けられたガス排出口32から排出される。 At both ends of the rotating shaft 2, a raw material inlet 31 is provided at the left end and a product outlet 33 is provided at the right end, and the raw material inlet 31 is charged by the rotation of the blade body 21 and the rotating shaft 2. The raw material moves toward the product discharge port 33, is heated by conduction heat transfer from the rotary shaft 2, the blade 21 and the medium circulation path 11, and is discharged from the product discharge port 33 after being subjected to reaction and drying action. . In accordance with the drying process, moisture contained in the contents or moisture, alcohol or volatile matter generated by the reaction is discharged from a gas discharge port 32 provided at the upper portion of the casing 1.
図2は、2本の棒状の形状で形成された冶具の一例を示す模式図である。径3mmのステンレス製(SUS304)の金属の棒42は、2本の金属の棒42で羽根21を挟むようにして固定される。また、金属の棒42の下端部は、回転軸2の形状に沿って、屈曲されており、羽根21の付着物だけでなく、回転軸2の付着物を脱着させることができる。 FIG. 2 is a schematic diagram showing an example of a jig formed in the shape of two rods. A stainless steel (SUS304) metal rod 42 having a diameter of 3 mm is fixed so that the blade 21 is sandwiched between the two metal rods 42. Further, the lower end portion of the metal rod 42 is bent along the shape of the rotating shaft 2, so that not only the attached matter of the blade 21 but also the attached matter of the rotating shaft 2 can be detached.
図3は、図2に示す2本の棒状の形状で形成された冶具4を装着した撹拌装置の撹拌機部分を水平方向で見た模式図である。図3に示すように、2本の金属の棒42の上端部は、羽根21の上方に設けられた支持台41に連結され、羽根21の回転に合わせて旋回できるようになっている。また、2本の金属の棒42は、上述したように、羽根21を挟むように固定され、2本の金属の棒42の下端部は、回転軸2の形状に沿って、屈曲されている。 FIG. 3 is a schematic view of the stirrer portion of the stirrer equipped with the jig 4 formed in the shape of two rods shown in FIG. 2 as viewed in the horizontal direction. As shown in FIG. 3, the upper end portions of the two metal rods 42 are connected to a support base 41 provided above the blades 21 so that they can be turned in accordance with the rotation of the blades 21. Further, as described above, the two metal bars 42 are fixed so as to sandwich the blade 21, and the lower ends of the two metal bars 42 are bent along the shape of the rotating shaft 2. .
図4は図2に示す2本の棒状の形状で形成された冶具4を装着した撹拌装置の撹拌機部分の写真である。金属の棒42は、羽根21及び回転軸2の形状に沿って設置されているが、これらと接触すると撹拌装置の運転時に異音が発生する場合があるため、0.1〜5mm程度の空間を確保することが望ましい。 FIG. 4 is a photograph of the stirrer portion of the stirrer equipped with the jig 4 formed in the shape of two rods shown in FIG. The metal bar 42 is installed along the shapes of the blades 21 and the rotary shaft 2, but if they come into contact with each other, abnormal noise may be generated during operation of the stirrer, so a space of about 0.1 to 5 mm. It is desirable to ensure.
図5(a)は、2枚の板状の形状で形成された冶具の平面図であり、図5(b)は、その側面図であり、図5(c)は、その斜視図である。ステンレス製(SUS304)の金属の板43は、2枚の金属の板43で羽根21を挟むようにして固定される。また、金属の板43の下端部は、回転軸2の形状に沿ってL字状に屈曲されており、羽根21の付着物だけでなく、回転軸2の付着物を脱着させることができるが、図7に示すように、下端部を屈曲させず、板状のままでもよい。 FIG. 5 (a) is a plan view of a jig formed in the shape of two plates, FIG. 5 (b) is a side view thereof, and FIG. 5 (c) is a perspective view thereof. . The metal plate 43 made of stainless steel (SUS304) is fixed so that the blades 21 are sandwiched between the two metal plates 43. Further, the lower end portion of the metal plate 43 is bent in an L shape along the shape of the rotary shaft 2, and not only the deposits on the blades 21 but also the deposits on the rotary shaft 2 can be detached. As shown in FIG. 7, the lower end portion may not be bent and may remain in a plate shape.
図6(a)は、図5に示す冶具を装着した撹拌装置の撹拌機部分を水平方向で見た模式図であり、図6(b)は、図6(a)の縦断面図である。図6に示すように、2枚の金属の板43の上端部は、羽根21の上方に設けられた支持台41に連結されている。また、2枚の金属の板43は、上述したように、羽根21を挟むように固定され、2枚の金属の板43の下端部は、回転軸2の形状に沿って、屈曲されている。尚、冶具4は、羽根21及び回転軸2と接触しないように、冶具4と羽根21及び回転軸2とは0.1〜5mm程度の空間を設けられている。 FIG. 6A is a schematic view of the stirrer portion of the stirrer equipped with the jig shown in FIG. 5 as viewed in the horizontal direction, and FIG. 6B is a longitudinal sectional view of FIG. . As shown in FIG. 6, the upper ends of the two metal plates 43 are connected to a support base 41 provided above the blades 21. Further, as described above, the two metal plates 43 are fixed so as to sandwich the blades 21, and the lower ends of the two metal plates 43 are bent along the shape of the rotating shaft 2. . Note that the jig 4, the blade 21, and the rotation shaft 2 are provided with a space of about 0.1 to 5 mm so that the jig 4 does not contact the blade 21 and the rotation shaft 2.
本発明の撹拌装置の有用性が顕著となるのは、上記容器に投入する内容物が脱水縮合する物質や粘着状の物質である。上記脱水縮合する物質としては、ポリエステル、ポリイミド、ポリアミド等の縮合反応して高分子になるもの、及び、オルトリン酸化合物等が挙げられる。 The usefulness of the stirrer of the present invention is remarkable for substances that are dehydrated and condensed and contents that are put into the container. Examples of the substance to be dehydrated and condensed include those that become a polymer by a condensation reaction such as polyester, polyimide, and polyamide, and orthophosphoric acid compounds.
上記ポリエステルとしては、例えば、エチレンテレフタレート、エチレン−2,6−ナフタレート、プロピレンテレフタレート、ブチレンテレフタレート、ヘキサメチレンテレフタレート、シクロヘキサンジメチレンテレフタレート、プロピレン−2,6−ナフタレート、ブチレン−2,6−ナフタレート、ヘキサメチレン−2,6−ナフタレート、シクロヘキサンジメチレン−2,6−ナフタレート単位等から選ばれた少なくとも一種の構造単位を主要構成成分とするもの、又はこれらを主成分とする共重合ポリエステル等が挙げられる。 Examples of the polyester include ethylene terephthalate, ethylene-2,6-naphthalate, propylene terephthalate, butylene terephthalate, hexamethylene terephthalate, cyclohexanedimethylene terephthalate, propylene-2,6-naphthalate, butylene-2,6-naphthalate, hexa. Examples thereof include those having at least one structural unit selected from methylene-2,6-naphthalate, cyclohexanedimethylene-2,6-naphthalate units and the like as main constituents, or copolyesters containing these as main components. .
上記ポリイミドとしては、例えば、テトラカルボン酸及び/又はその酸無水物と、脂肪族一級モノアミン及び/又は芳香族一級モノアミンと、脂肪族一級ジアミン及び/又は芳香族一級ジアミンよりなる群から選ばれる一種又は2種以上の化合物を脱水縮合したものが挙げられる。 Examples of the polyimide include one selected from the group consisting of tetracarboxylic acid and / or acid anhydride thereof, aliphatic primary monoamine and / or aromatic primary monoamine, and aliphatic primary diamine and / or aromatic primary diamine. Or what dehydrated and condensed 2 or more types of compounds is mentioned.
上記テトラカルボン酸及び/又はその酸無水物としては、例えば、エチレンテトラカルボン酸、1,2,3,4−ブタンテトラカルボン酸、シクロペンタンテトラカルボン酸、ピロメリット酸、1,2,3,4−ベンゼンテトラカルボン酸、3,3’,4,4’−ビフェニルテトラカルボン酸、2,2’,3,3’−ビフェニルテトラカルボン酸、3,3’,4,4’−ベンゾフェノンテトラカルボン酸、2,2’,3,3’−ベンゾフェノンテトラカルボン酸、ビス(2,3−ジカルボキシフェニル)メタン、ビス(3,4−ジカルボキシフェニル)メタン、1,1’ −ビス(2,3−ジカルボキシフェニル)エタン、2,2’−ビス(3,4−ジカルボキシフェニル)プロパン、2,2’−ビス(2,3−ジカルボキシフェニル)プロパン、ビス(3,4−ジカルボキシフェニル)エーテル、ビス(2,3−ジカルボキシフェニル)エーテル、ビス(3,4−ジカルボキシフェニル)スルホン、ビス(2,3−ジカルボキシフェニル)スルホン、2,3,6,7−ナフタレンテトラカルボン酸、1,4,5,8−ナフタレンテトラカルボン酸、1,2,5,6−ナフタレンテトラカルボン酸、2,3,6,7−アントラセンテトラカルボン酸、1,2,7,8−フェナントレンテトラカルボン酸、3,4,9, 10−ペリレンテトラカルボン酸、4,4’−(p−フェニレンジオキシ)ジフタル酸、4,4’−(m−フェニレンジオキシ)ジフタル酸、2,2’−ビス[(2,3−ジカルボキシフェノキシ)フェニル]プロパン等のテトラカルボン酸及び/又はその酸無水物等が挙げられる。 Examples of the tetracarboxylic acid and / or acid anhydride thereof include ethylene tetracarboxylic acid, 1,2,3,4-butanetetracarboxylic acid, cyclopentanetetracarboxylic acid, pyromellitic acid, 1,2,3, 4-benzenetetracarboxylic acid, 3,3 ′, 4,4′-biphenyltetracarboxylic acid, 2,2 ′, 3,3′-biphenyltetracarboxylic acid, 3,3 ′, 4,4′-benzophenonetetracarboxylic acid Acid, 2,2 ′, 3,3′-benzophenonetetracarboxylic acid, bis (2,3-dicarboxyphenyl) methane, bis (3,4-dicarboxyphenyl) methane, 1,1′-bis (2, 3-dicarboxyphenyl) ethane, 2,2′-bis (3,4-dicarboxyphenyl) propane, 2,2′-bis (2,3-dicarboxyphenyl) propa Bis (3,4-dicarboxyphenyl) ether, bis (2,3-dicarboxyphenyl) ether, bis (3,4-dicarboxyphenyl) sulfone, bis (2,3-dicarboxyphenyl) sulfone, 2,3,6,7-naphthalenetetracarboxylic acid, 1,4,5,8-naphthalenetetracarboxylic acid, 1,2,5,6-naphthalenetetracarboxylic acid, 2,3,6,7-anthracenetetracarboxylic acid Acid, 1,2,7,8-phenanthrenetetracarboxylic acid, 3,4,9,10-perylenetetracarboxylic acid, 4,4 ′-(p-phenylenedioxy) diphthalic acid, 4,4 ′-(m -Phenylenedioxy) diphthalic acid, tetracarboxylic acids such as 2,2′-bis [(2,3-dicarboxyphenoxy) phenyl] propane and / or acid anhydrides thereof. I can get lost.
上記脂肪族一級モノアミンとしては、例えば、炭素数2〜22の飽和又は不飽和の直鎖、分岐又は脂環系のモノアミンが挙げられ、具体的には、エチルアミン、ブチルアミン、ペンチルアミン、ヘキシルアミン、ヘプチルアミン、オクチルアミン、ノニルアミン、デシルアミン、ウンデシルアミン、ドデシルアミン、トリデシルアミン、テトラデシルアミン、ペンタデシルアミン、ヘキサデシルアミン、ヘプタデシルアミン、オクタデシルアミン、ノナデシルアミン、エイコシルアミン、ヘネイコシルアミン、ドコシルアミン、シクロヘキシルアミン、メチルシクロヘキシルアミン、ジメチルシクロヘキシルアミン、ジエチルシクロヘキシルアミン及びこれらの構造異性体等が挙げられる。 Examples of the aliphatic primary monoamine include, for example, a saturated or unsaturated linear, branched or alicyclic monoamine having 2 to 22 carbon atoms, specifically, ethylamine, butylamine, pentylamine, hexylamine, Heptylamine, octylamine, nonylamine, decylamine, undecylamine, dodecylamine, tridecylamine, tetradecylamine, pentadecylamine, hexadecylamine, heptadecylamine, octadecylamine, nonadecylamine, eicosylamine, heneicosylamine , Docosylamine, cyclohexylamine, methylcyclohexylamine, dimethylcyclohexylamine, diethylcyclohexylamine and structural isomers thereof.
上記芳香族一級モノアミンとしては、例えば、非置換又は炭素数1〜22のアルキル置換の一級アニリンが挙げられ、具体的には、アニリン、トルイジン、エチルアニリン、プロピルアニリン、ブチルアニリン、ペンチルアニリン、ヘキシルアニリン、ヘプチルアニリン、オクチルアニリン、ノニルアニリン、デシルアニリン、ウンデシルアニリン、ドデシルアニリン、トリデシルアニリン、テトラデシルアニリン、ペンタデシルアニリン、ヘキサデシルアニリン、ヘプタデシルアニリン、オクタデシルアニリン、ノナデシルアニリン、エイコシルアニリン、ヘネイコシルアニリン、ドコシルアニリン及びこれらの構造異性体等が挙げられる。 Examples of the aromatic primary monoamine include, for example, unsubstituted or alkyl-substituted primary anilines having 1 to 22 carbon atoms, and specifically include aniline, toluidine, ethylaniline, propylaniline, butylaniline, pentylaniline, hexyl. Aniline, heptylaniline, octylaniline, nonylaniline, decylaniline, undecylaniline, dodecylaniline, tridecylaniline, tetradecylaniline, pentadecylaniline, hexadecylaniline, heptadecylaniline, octadecylaniline, nonadecylaniline, eicosyl Examples include aniline, heneicosylaniline, docosylaniline, and structural isomers thereof.
上記脂肪族一級ジアミンとしては、例えば、炭素数1〜12のメチレン基で結合された一級ジアミンや脂環基を有するジアミンが挙げられ、具体的には、エチレンジアミン、トリメチレンジアミン、テトラメチレンジアミン、ペンタメチレンジアミン、ヘキサメチレンジアミン、ヘプタメチレンジアミン、オクタメチレンジアミン、ノナメチレンジアミン、デカメチレンジアミン、ウンデカメチレンジアミン、ドデカメチレンジアミン、1,3−ビスアミノシクロヘキサン、ジアミノジシクロヘキシルメタン、m−キシレンジアミン及びこれらの構造異性体等が挙げられる。 Examples of the aliphatic primary diamine include primary diamines bonded with methylene groups having 1 to 12 carbon atoms and diamines having an alicyclic group. Specifically, ethylene diamine, trimethylene diamine, tetramethylene diamine, Pentamethylenediamine, hexamethylenediamine, heptamethylenediamine, octamethylenediamine, nonamethylenediamine, decamethylenediamine, undecamethylenediamine, dodecamethylenediamine, 1,3-bisaminocyclohexane, diaminodicyclohexylmethane, m-xylenediamine and These structural isomers can be mentioned.
上記芳香族一級ジアミンとしては、例えば、ベンジジン、ジメチルベンジジン、ジアミノジフェニルメタン、ジアミノジトリルメタン、ジアミノジフェニルエタン、ジアミノジフェニルプロパン、ジアミノジフェニルブタン、ジアミノジフェニルエーテル、ジアミノジフェニルスルホン、ジアミノジフェニルベンゾフェノン、o,m,p−フェニレンジアミン、トリレンジアミン、キシレンジアミン等及びこれらの例示した芳香族一級ジアミンの炭化水素基を構造単位に有する芳香族一級ジアミン等が挙げられる。 Examples of the aromatic primary diamine include benzidine, dimethylbenzidine, diaminodiphenylmethane, diaminoditolylmethane, diaminodiphenylethane, diaminodiphenylpropane, diaminodiphenylbutane, diaminodiphenyl ether, diaminodiphenylsulfone, diaminodiphenylbenzophenone, o, m, Examples thereof include p-phenylenediamine, tolylenediamine, xylenediamine, and the like, and aromatic primary diamines having a hydrocarbon group of these exemplified aromatic primary diamines as structural units.
上記オルトリン酸化合物としては、例えば、リン酸アンモニウム、リン酸メラミン、リン酸アセトグアナミン、リン酸ベンゾグアナミン、リン酸アクリルグアナミン、リン酸2,4−ジアミノ−6−ノニル−1,3,5−トリアジン、リン酸2,4−ジアミノ−6−ヒドロキシ−1,3,5−トリアジン、リン酸2−アミノ−4,6−ジヒドロキシ−1,3,5−トリアジン、リン酸2,4−ジアミノ−6−メトキシ−1,3,5−トリアジン、リン酸2,4−ジアミノ−6−エトキシ−1,3,5−トリアジン、リン酸2,4−ジアミノ−6−プロポキシ−1,3,5−トリアジン、リン酸2,4−ジアミノ−6−イソプロポキシ−1,3,5−トリアジン、リン酸2,4−ジアミノ−6−メルカプト−1,3,5−トリアジン、リン酸2−アミノ−4,6−ジメルカプト−1,3,5−トリアジン、リン酸N,N,N’,N’−テトラメチルジアミノメタン、リン酸エチレンジアミン、リン酸N,N’−ジメチルエチレンジアミン、リン酸N,N’−ジエチルエチレンジアミン、リン酸N,N−ジメチルエチレンジアミン、リン酸N,N−ジエチルエチレンジアミン、リン酸N,N,N’,N’−テトラメチルエチレンジアミン、リン酸1,2−プロパンジアミン、リン酸1,3−プロパンジアミン、リン酸テトラメチレンジアミン、リン酸ペンタメチレンジアミン、リン酸ヘキサメチレンジアミン、リン酸1、7−ジアミノへプタン、リン酸1,8−ジアミノオクタン、リン酸1,9ージアミノノナン、リン酸1,10−ジアミノデカン、リン酸ピペラジン、リン酸trans−2,5−ジメチルピペラジン、リン酸1,4−ビス(2−アミノエチル)ピペラジン、リン酸1,4−ビス(3−アミノプロピル)ピペラジン等が挙げられる。 Examples of the orthophosphoric acid compound include ammonium phosphate, melamine phosphate, acetoguanamine phosphate, benzoguanamine phosphate, acrylic guanamine phosphate, 2,4-diamino-6-nonyl-1,3,5-triazine phosphate 2,4-diamino-6-hydroxy-1,3,5-triazine phosphate, 2-amino-4,6-dihydroxy-1,3,5-triazine phosphate, 2,4-diamino-6 phosphate -Methoxy-1,3,5-triazine, 2,4-diamino-6-ethoxy-1,3,5-triazine phosphate, 2,4-diamino-6-propoxy-1,3,5-triazine phosphate 2,4-diamino-6-isopropoxy-1,3,5-triazine phosphate, 2,4-diamino-6-mercapto-1,3,5-triazine phosphate, phosphoric acid 2 Amino-4,6-dimercapto-1,3,5-triazine, phosphoric acid N, N, N ′, N′-tetramethyldiaminomethane, phosphoric acid ethylenediamine, phosphoric acid N, N′-dimethylethylenediamine, phosphoric acid N , N′-diethylethylenediamine, phosphoric acid N, N-dimethylethylenediamine, phosphoric acid N, N-diethylethylenediamine, phosphoric acid N, N, N ′, N′-tetramethylethylenediamine, phosphoric acid 1,2-propanediamine, 1,3-propanediamine phosphate, tetramethylenediamine phosphate, pentamethylenediamine phosphate, hexamethylenediamine phosphate, 1,7-diaminoheptane phosphate, 1,8-diaminooctane phosphate, 1, phosphate phosphate 9-Diaminononane, 1,10-diaminodecane phosphate, piperazine phosphate, tran phosphate 2,5-dimethylpiperazine, phosphoric acid 1,4-bis (2-aminoethyl) piperazine, phosphoric acid 1,4-bis (3-aminopropyl) piperazine, and the like.
上記オルトリン酸化合物を、120〜350℃の温度条件下で脱水縮合反応することによってピロリン酸化合物を製造することができる。また、オルトリン酸化合物の水溶液又はスラリーを乾燥して無水塩としてから、焼成することでもピロリン酸化合物を製造することができる。上記オルトリン酸化合物は、正塩を使用してもよいし、酸性塩を使用してもよく、それらの混合物を使用してもよい。また対応する塩基を過剰に含んでいてもよい。 A pyrophosphate compound can be produced by subjecting the orthophosphoric acid compound to a dehydration condensation reaction at a temperature of 120 to 350 ° C. The pyrophosphate compound can also be produced by drying an aqueous solution or slurry of an orthophosphoric acid compound to form an anhydrous salt and then firing. As the orthophosphoric acid compound, a normal salt may be used, an acidic salt may be used, or a mixture thereof may be used. Moreover, the corresponding base may be included excessively.
また、特開平5−170893号公報等で開示されているように、芳香族ポリカーボネートのガラス転移点以上の温度で固相重合させる製造方法の場合にも本発明の撹拌装置を利用することができる。 Further, as disclosed in JP-A-5-170893 and the like, the stirrer of the present invention can also be used in the case of a production method in which solid state polymerization is performed at a temperature higher than the glass transition point of an aromatic polycarbonate. .
また、特開2000−191769号公報又は特開2001−302738号公報で提案されているように、ポリマーを官能化させる方法においても、本発明の撹拌装置を利用することができる。ポリマーを官能化させる方法としては、ポリマーの融点以上の温度でポリマーと官能化化合物を溶融混練する方法が挙げられるが、ポリマーを溶媒に溶解させたものに貧溶媒を加えて粒状の沈殿物を析出させ、官能化化合物と混合して反応して加熱することにより、ポリマーの融点以下の温度でポリマーを官能化させる方法を用いる場合にも本発明の撹拌装置を利用することができる。 Further, as proposed in Japanese Patent Application Laid-Open No. 2000-191769 or Japanese Patent Application Laid-Open No. 2001-302738, the stirring device of the present invention can also be used in a method of functionalizing a polymer. As a method for functionalizing the polymer, there is a method in which the polymer and the functionalized compound are melt-kneaded at a temperature equal to or higher than the melting point of the polymer. However, a granular solvent is obtained by adding a poor solvent to the polymer dissolved in a solvent. The stirrer of the present invention can also be used when using a method in which a polymer is functionalized at a temperature below the melting point of the polymer by precipitation, mixing with a functionalized compound, reaction, and heating.
上記官能化化合物としては、分子内に少なくとも一個の炭素−炭素二重結合又は三重結合、及び、カルボキシル基、酸化アシル基、イミノ基、イミド基、水酸基及びグリシジル基からなる群から選ばれる少なくとも一個の官能基を有する少なくとも1種の有機化合物が挙げられる。これらの官能化化合物のうち、分子内に二重結合、少なくとも一個のカルボキシル基、酸化アシル基又はイミド基を分子内に有する化合物が好ましい。具体的には、無水マレイン酸、マレイン酸、フマル酸、フェニルマレイミド、イタコン酸、グリシジルメタクリレート、クリシジルアクリレート等が挙げられる。 The functional compound is at least one selected from the group consisting of at least one carbon-carbon double bond or triple bond in the molecule, and a carboxyl group, an acyl oxide group, an imino group, an imide group, a hydroxyl group, and a glycidyl group. And at least one organic compound having a functional group of: Of these functionalized compounds, compounds having a double bond, at least one carboxyl group, an acyl oxide group or an imide group in the molecule are preferred. Specific examples include maleic anhydride, maleic acid, fumaric acid, phenylmaleimide, itaconic acid, glycidyl methacrylate, and clicidyl acrylate.
また、通常一般に使用される添加剤とポリマーを予め混合し押出機等の成形加工機で造粒後、得られた造粒品を乾燥する場合にも、本発明の撹拌装置を利用することができる。 In addition, the stirring device of the present invention can also be used in the case of drying the resulting granulated product after premixing the commonly used additive and polymer in advance and granulating with a molding machine such as an extruder. it can.
上記通常一般に使用される添加剤としては、例えば、フェノール系酸化防止剤、リン系酸化防止剤、チオエーテル系酸化防止剤、紫外線吸収剤、重金属不活性化剤、難燃剤、金属石鹸、ハイドロタルサイト、充填剤、滑剤、帯電防止剤、顔料、染料、可塑剤、結晶核剤等が挙げられる。 Examples of the generally commonly used additives include phenolic antioxidants, phosphorus antioxidants, thioether antioxidants, UV absorbers, heavy metal deactivators, flame retardants, metal soaps, hydrotalcite , Fillers, lubricants, antistatic agents, pigments, dyes, plasticizers, crystal nucleating agents and the like.
上記フェノール系酸化防止剤としては、例えば、2,6−ジ−第三ブチル−4−エチルフェノール、2−第三ブチル−4,6−ジメチルフェノール、スチレン化フェノール、2,2’−メチレンビス(4−エチル−6−第三ブチルフェノール)、2,2’−チオビス−(6−第三ブチル−4−メチルフェノール)、2,2’−チオジエチレンビス[3−(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオネート]、2−メチル−4,6−ビス(オクチルスルファニルメチル)フェノール、2,2’−イソブチリデンビス(4,6−ジメチルフェノール)、イソオクチル−3−(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオネート、N,N’−ヘキサン−1,6−ジイルビス[3−(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオンアミド、2,2’−オキサミド−ビス[エチル−3−(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオネート]、2−エチルヘキシル−3−(3’,5’−ジ−第三ブチル−4’−ヒドロキシフェニル)プロピオネート、2,2’−エチレンビス(4,6−ジ−第三ブチルフェノール)、3,5−ビス(1,1−ジメチルエチル)−4−ヒドロキシ−ベンゼンプロパン酸及びC13−15アルキルのエステル、2,5−ジ−第三アミルヒドロキノン、ヒンダードフェノールの重合物(アデカパルマロマール社製商品名AO.OH998)、2,2’−メチレンビス[6−(1−メチルシクロヘキシル)−p−クレゾール]、2−第三ブチル−6−(3−第三ブチル−2−ヒドロキシ−5−メチルベンジル)−4−メチルフェニルアクリレート、2−[1−(2−ヒドロキシ−3,5−ジ−第三ペンチルフェニル)エチル]−4,6−ジ−第三ペンチルフェニルアクリレート、6−[3−(3−第三ブチル−4−ヒドロキシ−5−メチル)プロポキシ]−2,4,8,10−テトラ−第三ブチルベンズ[d,f][1,3,2]−ジオキサホスフォビン、ヘキサメチレンビス[3−(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオネート、ビス[モノエチル(3,5−ジ−第三ブチル−4−ヒドロキシベンジル)ホスホネートカルシウム塩、5,7−ビス(1,1−ジメチルエチル)−3−ヒドロキシ−2(3H)−ベンゾフラノン、とo−キシレンとの反応生成物、2,6−ジ−第三ブチル−4−(4,6−ビス(オクチルチオ)−1,3,5−トリアジン−2−イルアミノ)フェノール、DL−a−トコフェノール(ビタミンE)、2,6−ビス(α−メチルベンジル)−4−メチルフェノール、ビス[3,3−ビス−(4’−ヒドロキシ−3’−第三ブチル−フェニル)ブタン酸]グリコールエステル、2,6−ジ−第三ブチル−p−クレゾール、2,6−ジフェニル−4−オクタデシロキシフェノール、ステアリル(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオネート、ジステアリル(3,5−ジ−第三ブチル−4−ヒドロキシベンジル)ホスホネート、トリデシル−3,5−ジ−第三ブチル−4−ヒドロキシベンジルチオアセテート、チオジエチレンビス[(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオネート]、4,4’−チオビス(6−第三ブチル−m−クレゾール)、2−オクチルチオ−4,6−ジ(3,5−ジ−第三ブチル−4−ヒドロキシフェノキシ)−s−トリアジン、2,2’−メチレンビス(4−メチル−6−第三ブチルフェノール)、ビス[3,3−ビス(4−ヒドロキシ−3−第三ブチルフェニル)ブチリックアシッド]グリコールエステル、4,4’−ブチリデンビス(2,6−ジ−第三ブチルフェノール)、4,4’−ブチリデンビス(6−第三ブチル−3−メチルフェノール)、2,2’−エチリデンビス(4,6−ジ−第三ブチルフェノール)、1,1,3−トリス(2−メチル−4−ヒドロキシ−5−第三ブチルフェニル)ブタン、ビス[2−第三ブチル−4−メチル−6−(2−ヒドロキシ−3−第三ブチル−5−メチルベンジル)フェニル]テレフタレート、1,3,5−トリス(2,6−ジメチル−3−ヒドロキシ−4−第三ブチルベンジル)イソシアヌレート、1,3,5−トリス(3,5−ジ−第三ブチル−4−ヒドロキシベンジル)イソシアヌレート、1,3,5−トリス(3,5−ジ−第三ブチル−4−ヒドロキシベンジル)−2,4,6−トリメチルベンゼン、1,3,5−トリス[(3,5−ジ−第三ブチル−4−ヒドロキシフェニル)プロピオニルオキシエチル]イソシアヌレート、テトラキス[メチレン−3−(3’,5’−ジ−第三ブチル−4’−ヒドロキシフェニル)プロピオネート]メタン、2−第三ブチル−4−メチル−6−(2−アクリロイルオキシ−3−第三ブチル−5−メチルベンジル)フェノール、3,9−ビス[2−(3−第三ブチル−4−ヒドロキシ−5−メチルヒドロシンナモイルオキシ)−1,1−ジメチルエチル]−2,4,8,10−テトラオキサスピロ[5.5]ウンデカン、トリエチレングリコールビス[β−(3−第三ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオネート]、ステアリル−3−(3,5−ジ第三ブチル−4−ヒドロキシフェニル)プロピオン酸アミド、パルミチル−3−(3,5−ジ第三ブチル−4−ヒドロキシフェニル)プロピオン酸アミド、ミリスチル−3−(3,5−ジ第三ブチル−4−ヒドロキシフェニル)プロピオン酸アミド、ラウリル−3−(3,5−ジ第三ブチル−4−ヒドロキシフェニル)プロピオン酸アミド等の3−(3,5−ジアルキル−4−ヒドロキシフェニル)プロピオン酸誘導体等が挙げられる。 Examples of the phenolic antioxidant include 2,6-di-tert-butyl-4-ethylphenol, 2-tert-butyl-4,6-dimethylphenol, styrenated phenol, 2,2′-methylenebis ( 4-ethyl-6-tert-butylphenol), 2,2′-thiobis- (6-tert-butyl-4-methylphenol), 2,2′-thiodiethylenebis [3- (3,5-di-tert. Tributyl-4-hydroxyphenyl) propionate], 2-methyl-4,6-bis (octylsulfanylmethyl) phenol, 2,2′-isobutylidenebis (4,6-dimethylphenol), isooctyl-3- ( 3,5-di-tert-butyl-4-hydroxyphenyl) propionate, N, N′-hexane-1,6-diylbis [3- (3,5-di-tert-butyl-4 Hydroxyphenyl) propionamide, 2,2′-oxamido-bis [ethyl-3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate], 2-ethylhexyl-3- (3 ′, 5 ′ -Di-tert-butyl-4'-hydroxyphenyl) propionate, 2,2'-ethylenebis (4,6-di-tert-butylphenol), 3,5-bis (1,1-dimethylethyl) -4- Hydroxy-benzenepropanoic acid and ester of C13-15 alkyl, 2,5-di-tertiary amylhydroquinone, hindered phenol polymer (trade name AO.OH998, manufactured by Adeka Palmaloma), 2,2′-methylenebis [ 6- (1-methylcyclohexyl) -p-cresol], 2-tert-butyl-6- (3-tert-butyl-2-hydroxy-5-methyl) Rubenzyl) -4-methylphenyl acrylate, 2- [1- (2-hydroxy-3,5-di-tert-pentylphenyl) ethyl] -4,6-di-tert-pentylphenyl acrylate, 6- [3- (3-tert-butyl-4-hydroxy-5-methyl) propoxy] -2,4,8,10-tetra-tert-butylbenz [d, f] [1,3,2] -dioxaphosphobin, Hexamethylene bis [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionate, bis [monoethyl (3,5-di-tert-butyl-4-hydroxybenzyl) phosphonate calcium salt, 5,7 -Bis (1,1-dimethylethyl) -3-hydroxy-2 (3H) -benzofuranone and the reaction product of o-xylene, 2,6-di-tert-butyl-4- (4,6-bis (O Cutylthio) -1,3,5-triazin-2-ylamino) phenol, DL-a-tocophenol (vitamin E), 2,6-bis (α-methylbenzyl) -4-methylphenol, bis [3,3 -Bis- (4'-hydroxy-3'-tert-butyl-phenyl) butanoic acid] glycol ester, 2,6-di-tert-butyl-p-cresol, 2,6-diphenyl-4-octadecyloxyphenol , Stearyl (3,5-di-tert-butyl-4-hydroxyphenyl) propionate, distearyl (3,5-di-tert-butyl-4-hydroxybenzyl) phosphonate, tridecyl-3,5-di-tert. Butyl-4-hydroxybenzylthioacetate, thiodiethylenebis [(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] 4,4′-thiobis (6-tert-butyl-m-cresol), 2-octylthio-4,6-di (3,5-di-tert-butyl-4-hydroxyphenoxy) -s-triazine, 2, 2'-methylenebis (4-methyl-6-tert-butylphenol), bis [3,3-bis (4-hydroxy-3-tert-butylphenyl) butyric acid] glycol ester, 4,4'-butylidenebis (2 , 6-di-tert-butylphenol), 4,4′-butylidenebis (6-tert-butyl-3-methylphenol), 2,2′-ethylidenebis (4,6-di-tert-butylphenol), 1, 1,3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, bis [2-tert-butyl-4-methyl-6- (2-hydroxy-3-tert-butyl-5- Mechi Rubenzyl) phenyl] terephthalate, 1,3,5-tris (2,6-dimethyl-3-hydroxy-4-tert-butylbenzyl) isocyanurate, 1,3,5-tris (3,5-di-tert. Butyl-4-hydroxybenzyl) isocyanurate, 1,3,5-tris (3,5-di-tert-butyl-4-hydroxybenzyl) -2,4,6-trimethylbenzene, 1,3,5-tris [(3,5-di-tert-butyl-4-hydroxyphenyl) propionyloxyethyl] isocyanurate, tetrakis [methylene-3- (3 ′, 5′-di-tert-butyl-4′-hydroxyphenyl) propionate ] Methane, 2-tert-butyl-4-methyl-6- (2-acryloyloxy-3-tert-butyl-5-methylbenzyl) phenol, 3,9-bis [2- 3-tert-butyl-4-hydroxy-5-methylhydrocinnamoyloxy) -1,1-dimethylethyl] -2,4,8,10-tetraoxaspiro [5.5] undecane, triethylene glycol bis [ β- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate], stearyl-3- (3,5-ditert-butyl-4-hydroxyphenyl) propionic acid amide, palmityl-3- (3 , 5-Di-tert-butyl-4-hydroxyphenyl) propionic acid amide, myristyl-3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid amide, lauryl-3- (3,5-di-) 3- (3,5-dialkyl-4-hydroxyphenyl) propionic acid derivatives such as tert-butyl-4-hydroxyphenyl) propionic acid amide Can be mentioned.
上記リン系酸化防止剤としては、例えば、トリフェニルホスファイト、ジイソオクチルホスファイト、ヘプタキストリホスファイト、トリイソデシルホスファイト、ジフェニルイソオクチルホスファイト、ジイソオクチルフェニルホスファイト、ジフェニルトリデシルホスファイト、トリイソオクチルホスファイト、トリラウリルホスファイト、ジフェニルホスファイト、トリス(ジプロピレングリコール)ホスファイト、ジイソデシルペンタエリスリトールジホスファイト、ジオレイルヒドロゲンホスファイト、トリラウリルトリチオホスファイト、ビス(トリデシル)ホスファイト、トリス(イソデシル)ホスファイト、トリス(トリデシル)ホスファイト、ジフェニルデシルホスファイト、ジノニルフェニルビス(ノニルフェニル)ホスファイト、ポリ(ジプロピレングリコール)フェニルホスファイト、テトラフェニルジプロピルグリコールジホスファイト、トリスノニルフェニルホスファイト、トリス(2,4−ジ−第三ブチルフェニル)ホスファイト、トリス(2,4−ジ−第三ブチル−5−メチルフェニル)ホスファイト、トリス〔2−第三ブチル−4−(3−第三ブチル−4−ヒドロキシ−5−メチルフェニルチオ)−5−メチルフェニル〕ホスファイト、トリデシルホスファイト、オクチルジフェニルホスファイト、ジ(デシル)モノフェニルホスファイト、ジステアリルペンタエリスリトールジホスファイト、ジステアリルペンタエリスリトールとステアリン酸カルシウム塩との混合物、アルキル(C10)ビスフェノールAホスファイト、ジ(トリデシル)ペンタエリスリトールジホスファイト、ジ(ノニルフェニル)ペンタエリスリトールジホスファイト、ビス(2,4−ジ−第三ブチルフェニル)ペンタエリスリトールジホスファイト、ビス(2,6−ジ−第三ブチル−4−メチルフェニル)ペンタエリスリトールジホスファイト、ビス(2,4,6−トリ−第三ブチルフェニル)ペンタエリスリトールジホスファイト、ビス(2,4−ジクミルフェニル)ペンタエリスリトールジホスファイト、テトラフェニル−テトラ(トリデシル)ペンタエリスリトールテトラホスファイト、ビス(2,4−ジ−第三ブチル−6−メチルフェニル)エチルホスファイト、テトラ(トリデシル)イソプロピリデンジフェノールジホスファイト、テトラ(トリデシル)−4,4’−n−ブチリデンビス(2−第三ブチル−5−メチルフェノール)ジホスファイト、ヘキサ(トリデシル)−1,1,3−トリス(2−メチル−4−ヒドロキシ−5−第三ブチルフェニル)ブタントリホスファイト、テトラキス(2,4−ジ−第三ブチルフェニル)ビフェニレンジホスホナイト、9,10−ジハイドロ−9−オキサ−10−ホスファフェナンスレン−10−オキサイド、(1−メチル−1―プロパニル−3−イリデン)トリス(2−1,1−ジメチルエチル)−5−メチル−4,1−フェニレン)ヘキサトリデシルホスファイト、2,2’−メチレンビス(4,6−第三ブチルフェニル)−2−エチルヘキシルホスファイト、2,2’−メチレンビス(4,6−ジ−第三ブチルフェニル)−オクタデシルホスファイト、2,2’−エチリデンビス(4,6−ジ−第三ブチルフェニル)フルオロホスファイト、4,4’−ブチリデンビス(3−メチル−6−第三ブチルフェニルジトリデシル)ホスファイト、トリス(2−〔(2,4,8,10−テトラキス−第三ブチルジベンゾ〔d,f〕〔1,3,2〕ジオキサホスフェピン−6−イル)オキシ〕エチル)アミン、3,9−ビス(4−ノニルフェノキシ)−2,4,8,10−テトラオキサ−3,9−ジホスフェススピロ[5,5]ウンデカン、2,4,6−トリ−第三ブチルフェニル−2−ブチル−2エチル−1,3−プロパンジオールホスファイト、ポリ4,4’−イソプロピリデンジフェノールC12−15アルコールホスファイト、2−エチル−2−ブチルプロピレングリコールと2,4,6−トリ−第三ブチルフェノールのホスファイト等が挙げられる。 Examples of the phosphorus antioxidant include triphenyl phosphite, diisooctyl phosphite, heptakis triphosphite, triisodecyl phosphite, diphenylisooctyl phosphite, diisooctylphenyl phosphite, diphenyltridecyl phosphite. Phyto, triisooctyl phosphite, trilauryl phosphite, diphenyl phosphite, tris (dipropylene glycol) phosphite, diisodecyl pentaerythritol diphosphite, dioleyl hydrogen phosphite, trilauryl trithiophosphite, bis (tridecyl) Phosphite, tris (isodecyl) phosphite, tris (tridecyl) phosphite, diphenyldecylphosphite, dinonylphenylbis (nonylphenyl) phospho Phyto, poly (dipropylene glycol) phenyl phosphite, tetraphenyldipropyl glycol diphosphite, trisnonylphenyl phosphite, tris (2,4-di-tert-butylphenyl) phosphite, tris (2,4-di Tert-butyl-5-methylphenyl) phosphite, tris [2-tert-butyl-4- (3-tert-butyl-4-hydroxy-5-methylphenylthio) -5-methylphenyl] phosphite, tris Decyl phosphite, octyl diphenyl phosphite, di (decyl) monophenyl phosphite, distearyl pentaerythritol diphosphite, a mixture of distearyl pentaerythritol and calcium stearate, alkyl (C10) bisphenol A phosphite, di (tridecyl) ) Intererythritol diphosphite, di (nonylphenyl) pentaerythritol diphosphite, bis (2,4-di-tert-butylphenyl) pentaerythritol diphosphite, bis (2,6-di-tert-butyl-4- Methylphenyl) pentaerythritol diphosphite, bis (2,4,6-tri-tert-butylphenyl) pentaerythritol diphosphite, bis (2,4-dicumylphenyl) pentaerythritol diphosphite, tetraphenyl-tetra (Tridecyl) pentaerythritol tetraphosphite, bis (2,4-di-tert-butyl-6-methylphenyl) ethyl phosphite, tetra (tridecyl) isopropylidenediphenol diphosphite, tetra (tridecyl) -4,4 '-N-butylidenebis (2-th Tributyl-5-methylphenol) diphosphite, hexa (tridecyl) -1,1,3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butanetriphosphite, tetrakis (2,4-di-) Tert-butylphenyl) biphenylenediphosphonite, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, (1-methyl-1-propanyl-3-ylidene) tris (2-1 , 1-dimethylethyl) -5-methyl-4,1-phenylene) hexatridecyl phosphite, 2,2′-methylenebis (4,6-tert-butylphenyl) -2-ethylhexyl phosphite, 2,2 ′ -Methylenebis (4,6-di-tert-butylphenyl) -octadecyl phosphite, 2,2'-ethylidenebis (4,6 Di-tert-butylphenyl) fluorophosphite, 4,4′-butylidenebis (3-methyl-6-tert-butylphenylditridecyl) phosphite, tris (2-[(2,4,8,10-tetrakis- Tert-butyldibenzo [d, f] [1,3,2] dioxaphosphin-6-yl) oxy] ethyl) amine, 3,9-bis (4-nonylphenoxy) -2,4,8, 10-tetraoxa-3,9-diphosphasspiro [5,5] undecane, 2,4,6-tri-tert-butylphenyl-2-butyl-2ethyl-1,3-propanediol phosphite, poly-4 , 4'-isopropylidenediphenol C12-15 alcohol phosphite, 2-ethyl-2-butylpropylene glycol and 2,4,6-tri-tert-butylphenol phosphat Doors and the like.
上記チオエーテル系酸化防止剤としては、例えば、テトラキス[メチレン−3−(ラウリルチオ)プロピオネート]メタン、ビス(メチル−4−[3−n−アルキル(C12/C14)チオプロピオニルオキシ]5−第三ブチルフェニル)スルファイド、ジトリデシル−3,3’−チオジプロピオネート、ジラウリル−3,3’−チオジプロピオネート、ジミリスチル−3,3’−チオジプロピオネート、ジステアリル−3,3’−チオジプロピオネート、ラウリル/ステアリルチオジプロピオネート、4,4’−チオビス(6−第三ブチル−m−クレゾール)、2,2’−チオビス(6−第三ブチル−p−クレゾール)、ジステアリル−ジサルファイドが挙げられる。 Examples of the thioether-based antioxidant include tetrakis [methylene-3- (laurylthio) propionate] methane, bis (methyl-4- [3-n-alkyl (C12 / C14) thiopropionyloxy] 5-tert-butyl. Phenyl) sulfide, ditridecyl-3,3′-thiodipropionate, dilauryl-3,3′-thiodipropionate, dimyristyl-3,3′-thiodipropionate, distearyl-3,3′-thiodipro Pionate, lauryl / stearyl thiodipropionate, 4,4'-thiobis (6-tert-butyl-m-cresol), 2,2'-thiobis (6-tert-butyl-p-cresol), distearyl- Disulfide is mentioned.
上記紫外線吸収剤としては、例えば、2,4−ジヒドロキシベンゾフェノン、2−ヒドロキシ−4−メトキシベンゾフェノン、2−ヒドロキシ−4−オクトキシベンゾフェノン、5,5’−メチレンビス(2−ヒドロキシ−4−メトキシベンゾフェノン)等の2−ヒドロキシベンゾフェノン類;2−(2−ヒドロキシ−5−メチルフェニル)ベンゾトリアゾール、2−(2−ヒドロキシ−5−第三オクチルフェニル)ベンゾトリアゾール、2−(2−ヒドロキシ−3,5−ジ第三ブチルフェニル)−5−クロロベンゾトリアゾール、2−(2−ヒドロキシ−3−第三ブチル−5−メチルフェニル)−5−クロロベンゾトリアゾール、2−(2−ヒドロキシ−3,5−ジクミルフェニル)ベンゾトリアゾール、2,2’−メチレンビス(4−第三オクチル−6−ベンゾトリアゾリルフェノール)、2−(2−ヒドロキシ−3−第三ブチル−5−カルボキシフェニル)ベンゾトリアゾールのポリエチレングリコールエステル、2−〔2−ヒドロキシ−3−(2−アクリロイルオキシエチル)−5−メチルフェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−3−(2−メタクリロイルオキシエチル)−5−第三ブチルフェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−3−(2−メタクリロイルオキシエチル)−5−第三オクチルフェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−3−(2−メタクリロイルオキシエチル)−5−第三ブチルフェニル〕−5−クロロベンゾトリアゾール、2−〔2−ヒドロキシ−5−(2−メタクリロイルオキシエチル)フェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−3−第三ブチル−5−(2−メタクリロイルオキシエチル)フェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−3−第三アミル−5−(2−メタクリロイルオキシエチル)フェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−3−第三ブチル−5−(3−メタクリロイルオキシプロピル)フェニル〕−5−クロロベンゾトリアゾール、2−〔2−ヒドロキシ−4−(2−メタクリロイルオキシメチル)フェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−4−(3−メタクリロイルオキシ−2−ヒドロキシプロピル)フェニル〕ベンゾトリアゾール、2−〔2−ヒドロキシ−4−(3−メタクリロイルオキシプロピル)フェニル〕ベンゾトリアゾール等の2−(2−ヒドロキシフェニル)ベンゾトリアゾール類;2−(2−ヒドロキシ−4−メトキシフェニル)−4,6−ジフェニル−1,3,5−トリアジン、2−(2−ヒドロキシ−4−ヘキシロキシフェニル)−4,6−ジフェニル−1,3,5−トリアジン、2−(2−ヒドロキシ−4−オクトキシフェニル)−4,6−ビス(2,4−ジメチルフェニル)−1,3,5−トリアジン、2−〔2−ヒドロキシ−4−(3−C12〜13混合アルコキシ−2−ヒドロキシプロポキシ)フェニル〕−4,6−ビス(2,4−ジメチルフェニル)−1,3,5−トリアジン、2−〔2−ヒドロキシ−4−(2−アクリロイルオキシエトキシ)フェニル〕−4,6−ビス(4−メチルフェニル)−1,3,5−トリアジン、2−(2,4−ジヒドロキシ−3−アリルフェニル)−4,6−ビス(2,4−ジメチルフェニル)−1,3,5−トリアジン、2,4,6−トリス(2−ヒドロキシ−3−メチル−4−ヘキシロキシフェニル)−1,3,5−トリアジン等の2−(2−ヒドロキシフェニル)−4,6−ジアリール−1,3,5−トリアジン類;フェニルサリシレート、レゾルシノールモノベンゾエート、2,4−ジ第三ブチルフェニル−3,5−ジ第三ブチル−4−ヒドロキシベンゾエート、オクチル(3,5−ジ第三ブチル−4−ヒドロキシ)ベンゾエート、ドデシル(3,5−ジ第三ブチル−4−ヒドロキシ)ベンゾエート、テトラデシル(3,5−ジ第三ブチル−4−ヒドロキシ)ベンゾエート、ヘキサデシル(3,5−ジ第三ブチル−4−ヒドロキシ)ベンゾエート、オクタデシル(3,5−ジ第三ブチル−4−ヒドロキシ)ベンゾエート、ベヘニル(3,5−ジ第三ブチル−4−ヒドロキシ)ベンゾエート等のベンゾエート類;2−エチル−2’−エトキシオキザニリド、2−エトキシ−4’−ドデシルオキザニリド等の置換オキザニリド類;エチル−α−シアノ−β,β−ジフェニルアクリレート、メチル−2−シアノ−3−メチル−3−(p−メトキシフェニル)アクリレート等のシアノアクリレート類;各種の金属塩、又は金属キレート、特にニッケル、クロムの塩、又はキレート類等が挙げられる。 Examples of the ultraviolet absorber include 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-octoxybenzophenone, and 5,5′-methylenebis (2-hydroxy-4-methoxybenzophenone). 2-hydroxybenzophenones such as 2- (2-hydroxy-5-methylphenyl) benzotriazole, 2- (2-hydroxy-5-tert-octylphenyl) benzotriazole, 2- (2-hydroxy-3, 5-di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2-hydroxy-3-tert-butyl-5-methylphenyl) -5-chlorobenzotriazole, 2- (2-hydroxy-3,5 -Dicumylphenyl) benzotriazole, 2,2'-methylenebis (4-th Octyl-6-benzotriazolylphenol), polyethylene glycol ester of 2- (2-hydroxy-3-tert-butyl-5-carboxyphenyl) benzotriazole, 2- [2-hydroxy-3- (2-acryloyloxy) Ethyl) -5-methylphenyl] benzotriazole, 2- [2-hydroxy-3- (2-methacryloyloxyethyl) -5-tert-butylphenyl] benzotriazole, 2- [2-hydroxy-3- (2- Methacryloyloxyethyl) -5-tert-octylphenyl] benzotriazole, 2- [2-hydroxy-3- (2-methacryloyloxyethyl) -5-tert-butylphenyl] -5-chlorobenzotriazole, 2- [2 -Hydroxy-5- (2-methacryloyloxyethyl) phenyl] benzene Zotriazole, 2- [2-hydroxy-3-tert-butyl-5- (2-methacryloyloxyethyl) phenyl] benzotriazole, 2- [2-hydroxy-3-tert-amyl-5- (2-methacryloyloxy) Ethyl) phenyl] benzotriazole, 2- [2-hydroxy-3-tert-butyl-5- (3-methacryloyloxypropyl) phenyl] -5-chlorobenzotriazole, 2- [2-hydroxy-4- (2- Methacryloyloxymethyl) phenyl] benzotriazole, 2- [2-hydroxy-4- (3-methacryloyloxy-2-hydroxypropyl) phenyl] benzotriazole, 2- [2-hydroxy-4- (3-methacryloyloxypropyl) 2- (2-hydroxypheny) such as phenyl] benzotriazole B) benzotriazoles; 2- (2-hydroxy-4-methoxyphenyl) -4,6-diphenyl-1,3,5-triazine, 2- (2-hydroxy-4-hexyloxyphenyl) -4,6 -Diphenyl-1,3,5-triazine, 2- (2-hydroxy-4-octoxyphenyl) -4,6-bis (2,4-dimethylphenyl) -1,3,5-triazine, 2- [ 2-hydroxy-4- (3-C12-13 mixed alkoxy-2-hydroxypropoxy) phenyl] -4,6-bis (2,4-dimethylphenyl) -1,3,5-triazine, 2- [2- Hydroxy-4- (2-acryloyloxyethoxy) phenyl] -4,6-bis (4-methylphenyl) -1,3,5-triazine, 2- (2,4-dihydroxy-3-allylphenyl) -4,6-bis (2,4-dimethylphenyl) -1,3,5-triazine, 2,4,6-tris (2-hydroxy-3-methyl-4-hexyloxyphenyl) -1,3 2- (2-hydroxyphenyl) -4,6-diaryl-1,3,5-triazines such as 5-triazine; phenyl salicylate, resorcinol monobenzoate, 2,4-ditert-butylphenyl-3,5- Di-tert-butyl-4-hydroxybenzoate, octyl (3,5-di-tert-butyl-4-hydroxy) benzoate, dodecyl (3,5-di-tert-butyl-4-hydroxy) benzoate, tetradecyl (3,5- Ditert-butyl-4-hydroxy) benzoate, hexadecyl (3,5-ditert-butyl-4-hydroxy) benzoate, octadecyl (3,5-ditert Benzoates such as butyl-4-hydroxy) benzoate, behenyl (3,5-ditert-butyl-4-hydroxy) benzoate; 2-ethyl-2′-ethoxyoxanilide, 2-ethoxy-4′-dodecyloxy Substituted oxanilides such as zanilides; cyanoacrylates such as ethyl-α-cyano-β, β-diphenyl acrylate and methyl-2-cyano-3-methyl-3- (p-methoxyphenyl) acrylate; various metal salts Or metal chelates, especially nickel, chromium salts, or chelates.
上記難燃剤としては、例えば、トリフェニルホスフェート、トリクレジルホスフェート、トリキシレニルホスフェート、クレジルジフェニルホスフェート、クレジル−2,6−キシレニルホスフェート及びレゾルシノールビス(ジフェニルホスフェート)等の芳香族リン酸エステル、フェニルホスホン酸ジビニル、フェニルホスホン酸ジアリル及びフェニルホスホン酸(1−ブテニル)等のホスホン酸エステル、ジフェニルホスフィン酸フェニル、ジフェニルホスフィン酸メチル、9,10−ジヒドロ−9−オキサ−10−ホスファフェナントレン−10−オキシド誘導体等のホスフィン酸エステル、ビス(2−アリルフェノキシ)ホスファゼン、ジクレジルホスファゼン等のホスファゼン化合物、リン酸メラミン、ピロリン酸メラミン、ポリリン酸メラミン、ポリリン酸メラム、ポリリン酸アンモニウム、リン含有ビニルベンジル化合物及び赤リン等のリン系難燃剤、水酸化マグネシウム、水酸化アルミニウム等の金属水酸化物、臭素化ビスフェノールA型エポキシ樹脂、臭素化フェノールノボラック型エポキシ樹脂、ヘキサブロモベンゼン、ペンタブロモトルエン、エチレンビス(ペンタブロモフェニル)、エチレンビステトラブロモフタルイミド、1,2−ジブロモ−4−(1,2−ジブロモエチル)シクロヘキサン、テトラブロモシクロオクタン、ヘキサブロモシクロドデカン、ビス(トリブロモフェノキシ)エタン、臭素化ポリフェニレンエーテル、臭素化ポリスチレン及び2,4,6−トリス(トリブロモフェノキシ)−1,3,5−トリアジン、トリブロモフェニルマレイミド、トリブロモフェニルアクリレート、トリブロモフェニルメタクリレート、テトラブロモビスフェノールA型ジメタクリレート、ペンタブロモベンジルアクリレート、及び、臭素化スチレン等の臭素系難燃剤等が挙げられる。 Examples of the flame retardant include aromatic phosphoric acid such as triphenyl phosphate, tricresyl phosphate, trixylenyl phosphate, cresyl diphenyl phosphate, cresyl-2,6-xylenyl phosphate, and resorcinol bis (diphenyl phosphate). Phosphonates such as esters, divinyl phenylphosphonate, diallyl phenylphosphonate and phenylphosphonic acid (1-butenyl), phenyl diphenylphosphinate, methyl diphenylphosphinate, 9,10-dihydro-9-oxa-10-phospha Phosphonic acid esters such as phenanthrene-10-oxide derivatives, phosphazene compounds such as bis (2-allylphenoxy) phosphazene and dicresyl phosphazene, melamine phosphate, melamine pyrophosphate, Melamine phosphate, melam polyphosphate, ammonium polyphosphate, phosphorus-containing vinylbenzyl compounds and phosphorus-based flame retardants such as red phosphorus, metal hydroxides such as magnesium hydroxide and aluminum hydroxide, brominated bisphenol A type epoxy resin, bromine Phenol novolac epoxy resin, hexabromobenzene, pentabromotoluene, ethylenebis (pentabromophenyl), ethylenebistetrabromophthalimide, 1,2-dibromo-4- (1,2-dibromoethyl) cyclohexane, tetrabromocyclo Octane, hexabromocyclododecane, bis (tribromophenoxy) ethane, brominated polyphenylene ether, brominated polystyrene and 2,4,6-tris (tribromophenoxy) -1,3,5-triazine, tribromophenyl Reimido, tribromophenyl acrylate, tribromophenyl methacrylate, tetrabromobisphenol A type dimethacrylate, pentabromobenzyl acrylate, and include brominated flame retardants such as brominated styrene and the like.
上記充填剤としては、例えば、タルク、マイカ、炭酸カルシウム、酸化カルシウム、水酸化カルシウム、炭酸マグネシウム、水酸化マグネシウム、酸化マグネシウム、硫酸マグネシウム、水酸化アルミニウム、硫酸バリウム、ガラス粉末、ガラス繊維、クレー、ドロマイト、マイカ、シリカ、アルミナ、チタン酸カリウムウィスカー、ワラステナイト、繊維状マグネシウムオキシサルフェート等が好ましい。これらの充填剤において、平均粒径(球状乃至平板状のもの)又は平均繊維径(針状乃至繊維状)が5μm以下のものが好ましい。 Examples of the filler include talc, mica, calcium carbonate, calcium oxide, calcium hydroxide, magnesium carbonate, magnesium hydroxide, magnesium oxide, magnesium sulfate, aluminum hydroxide, barium sulfate, glass powder, glass fiber, clay, Dolomite, mica, silica, alumina, potassium titanate whisker, wollastonite, fibrous magnesium oxysulfate and the like are preferable. Among these fillers, those having an average particle diameter (spherical or flat) or an average fiber diameter (needle or fiber) of 5 μm or less are preferable.
上記滑剤は、成形体表面に滑性を付与し傷つき防止効果を高める目的で加えられる。滑剤としては、例えば、オレイン酸アミド、エルカ酸アミド等の不飽和脂肪酸アミド;ベヘン酸アミド、ステアリン酸アミド等の飽和脂肪酸アミド等が挙げられる。これらは1種を用いてもよく、2種以上を併用して用いてもよい。 The above-mentioned lubricant is added for the purpose of imparting lubricity to the surface of the molded body and enhancing the effect of preventing damage. Examples of the lubricant include unsaturated fatty acid amides such as oleic acid amide and erucic acid amide; saturated fatty acid amides such as behenic acid amide and stearic acid amide. These may be used alone or in combination of two or more.
上記帯電防止剤は、成形品の帯電性の低減化や、帯電による埃の付着防止の目的で加えられる。帯電防止剤としては、カチオン系、アニオン系、非イオン系の帯電防止剤等が挙げられる。好ましい例としては、ポリオキシエチレンアルキルアミンやポリオキシエチレンアルキルアミドが挙げられる。これらは1種を用いてもよく、2種以上を併用して用いてもよい。 The antistatic agent is added for the purpose of reducing the chargeability of the molded product and preventing dust from adhering due to charging. Examples of the antistatic agent include cationic, anionic and nonionic antistatic agents. Preferable examples include polyoxyethylene alkylamine and polyoxyethylene alkylamide. These may be used alone or in combination of two or more.
上記結晶核剤としては、例えば、安息香酸ナトリウム、4−第三ブチル安息香酸アルミニウム塩等の安息香酸金属塩、アジピン酸ナトリウム、ナトリウムビス(4−第三ブチルフェニル)ホスフェート、リチウム−2,2’−メチレンビス(4,6−ジ第三ブチルフェニル)ホスフェート等のリン酸エステル金属塩、N,N’,N”−トリス[2−メチルシクロヘキシル]―1,2,3−プロパントリカルボキサミド(RIKACLEAR PC1)、N,N’,N”−トリシクロヘキシルー1,3,5−ベンゼントリカルボキミド、N,N’−ジシクロヘキシル−ナフタレンジカルボキサミド、1,3,5−トリ(ジメチルイソプロポイルアミノ)ベンゼン等のアミド化合物、N,N’,N”−トリス(2−メチルシクロヘキシル)−1,2,3−プロパントリカルボキシアミド、シス−エンド−ビシクロ[2.2.1]ヘプタン−2,3−ジカルボン酸ナトリウム塩、(N−[3,5−ビス(2,2−ジメチルプロピオニルアミノ)−フェニル]−2,2−ジメチルプロピオンアミド)、N,N’(メチレンビス(2,6−ジエチル−4,1−フェニレン))ビス(2−(オルト−トルイル)アセトアミド)、2,2−メチレンビス−(4,6−ジ−第三ブチルフェニル)ホスフェート、ビス((4−第三ブチル)ベンゾイル)オキシ)ヒドロキシ)アルミニウム、2,4,8,10−テトラ−第三ブチル−6−ヒドロキシ−12H−ジベンゾ[d.g][1,3,2]ジオキサホスホシン6−オン、ヒドロキシアルミニウム(1R,4S)−ビシクロ[2.2.1]ヘプタン−2,3−ジカルボキシレート、(1R、4S)−ビシクロ[2.2.1]ヘプタン−2,3−ジカルボン酸、ヒドロキシビス((2,4,8,10−テトラ−第三ブチル−6−オキシド−12H−ジベンゾ[d,g][1,3,2]ジオキサホスホシン−6−イル)オキシ)アルミニウム]等が挙げられる。 Examples of the crystal nucleating agent include benzoic acid metal salts such as sodium benzoate and aluminum 4-tert-butylbenzoate, sodium adipate, sodium bis (4-tert-butylphenyl) phosphate, lithium-2,2 Phosphoric acid ester metal salts such as '-methylenebis (4,6-ditert-butylphenyl) phosphate, N, N', N "-tris [2-methylcyclohexyl] -1,2,3-propanetricarboxamide (RIKACLEAR) PC1), N, N ′, N ″ -tricyclohexyl 1,3,5-benzenetricarboximide, N, N′-dicyclohexyl-naphthalenedicarboxamide, 1,3,5-tri (dimethylisopropoylamino) Amide compounds such as benzene, N, N ′, N ″ -tris (2-methylcyclohexyl) -1, , 3-propanetricarboxamide, cis-endo-bicyclo [2.2.1] heptane-2,3-dicarboxylic acid sodium salt, (N- [3,5-bis (2,2-dimethylpropionylamino)- Phenyl] -2,2-dimethylpropionamide), N, N ′ (methylenebis (2,6-diethyl-4,1-phenylene)) bis (2- (ortho-toluyl) acetamide), 2,2-methylenebis- (4,6-di-tert-butylphenyl) phosphate, bis ((4-tert-butyl) benzoyl) oxy) hydroxy) aluminum, 2,4,8,10-tetra-tert-butyl-6-hydroxy-12H -Dibenzo [d.g] [1,3,2] dioxaphosphocin 6-one, hydroxyaluminum (1R, 4S) -bicyclo [2.2.1] heptane- 2,3-dicarboxylate, (1R, 4S) -bicyclo [2.2.1] heptane-2,3-dicarboxylic acid, hydroxybis ((2,4,8,10-tetra-tert-butyl-6 -Oxide-12H-dibenzo [d, g] [1,3,2] dioxaphosphocin-6-yl) oxy) aluminum] and the like.
また、ポリマーを含まず、添加剤の組合せからなる添加剤組成物において、一成分の添加剤の融点以上の温度で混練したものを乾燥させる場合も、本発明の撹拌装置を利用することができる。 The stirring device of the present invention can also be used for drying an additive composition that does not contain a polymer and is a combination of additives and kneaded at a temperature equal to or higher than the melting point of the one-component additive. .
本発明で製造されるものは、球状、円柱状(ペレット状)、顆粒状等の任意の形状又は無定形状であってもよい。平均粒子径は特に制限されないが、1μm〜10mm程度のものは、取扱性がよく好ましく用いることができる。 What is manufactured by this invention may be arbitrary shapes, such as spherical shape, cylindrical shape (pellet shape), and granular shape, or indefinite shape. The average particle diameter is not particularly limited, but those having a particle size of about 1 μm to 10 mm can be preferably used because of good handleability.
また、特開昭63−264547号公報、特開平9−100253号公報、特開平10−147550号公報で提案されているように、脂肪酸と金属酸化物及び/又は金属水酸化物を反応させて金属石けんを製造する場合において、脂肪酸と金属酸化物及び/又は金属水酸化物を融点以上の温度で溶融反応させる製造方法、又は、脂肪酸と金属酸化物又は金属水酸化物のスラリーを、生成する脂肪酸金属塩の融点以下で半溶融させる製造方法においても、本発明の撹拌装置を利用することができる。 Further, as proposed in JP-A-63-264547, JP-A-9-100253, and JP-A-10-147550, a fatty acid is reacted with a metal oxide and / or metal hydroxide. When producing metal soap, a production method in which a fatty acid and a metal oxide and / or a metal hydroxide are melt-reacted at a temperature equal to or higher than the melting point, or a slurry of a fatty acid and a metal oxide or metal hydroxide is produced. The stirrer of the present invention can also be used in a production method in which the fatty acid metal salt is semi-molten below the melting point.
上記脂肪酸としては、例えば、炭素数8〜24の飽和又は不飽和脂肪酸(カプリル酸、カプリン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキン酸、ベヘン酸等の飽和脂肪酸、オクテン酸、テトラデセン酸、ヘキサデセン酸、オレイン酸、エルカ酸、リノール酸、リノレイン酸等の不飽和脂肪酸等)、オキシ脂肪酸(12−ヒドロキシステアリン酸、リシノール酸等の水酸基を有する脂肪酸)等が好ましく用いられ、これらは、単独であってもよく二種以上を混合したものであってもよい。 Examples of the fatty acid include saturated or unsaturated fatty acids having 8 to 24 carbon atoms (saturated fatty acids such as caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, and behenic acid, octenoic acid, Tetradecenoic acid, hexadecenoic acid, oleic acid, erucic acid, linoleic acid, unsaturated fatty acids such as linolenic acid, etc.), oxy fatty acids (fatty acids having a hydroxyl group such as 12-hydroxystearic acid, ricinoleic acid), etc. are preferably used. May be single or a mixture of two or more.
上記脂肪酸は、天然油脂から得られる脂肪酸であってもよい。天然油脂としては、例えば、アマニ油、オリーブ油、カカオ油、ゴマ油、コメヌカ油、サフラワー油、大豆油、椿油、コーン油、菜種油、パーム油、パーム核油、ひまし油、ひまわり油、綿実油、ヤシ油等の植物性油脂、牛脂、豚脂、乳脂、魚油、鯨油等の動物性油脂が挙げられる。 The fatty acid may be a fatty acid obtained from natural fats and oils. Examples of natural fats and oils include linseed oil, olive oil, cacao oil, sesame oil, rice bran oil, safflower oil, soybean oil, cocoon oil, corn oil, rapeseed oil, palm oil, palm kernel oil, castor oil, sunflower oil, cottonseed oil, and palm oil. And vegetable oils such as beef fat, pork fat, milk fat, fish oil, whale oil and the like.
上記金属酸化物又は金属水酸化物の金属源としては、カルシウム、マグネシウム、亜鉛、鉛、錫、鉄、カドミウム、バリウム、コバルト、ニッケル、マンガン、ストロンチウム、チタン、バナジウム、銅、リチウム、ナトリウム等が挙げられ、より具体的には、酸化亜鉛、生石灰、酸化マグネシウム、消石灰、水酸化バリウム等が挙げられる。 Examples of the metal source of the metal oxide or metal hydroxide include calcium, magnesium, zinc, lead, tin, iron, cadmium, barium, cobalt, nickel, manganese, strontium, titanium, vanadium, copper, lithium, sodium, and the like. More specifically, zinc oxide, quick lime, magnesium oxide, slaked lime, barium hydroxide and the like can be mentioned.
以下、本発明を実施例及び比較例により、更に具体的に説明するが、本発明はこれらによって限定されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further more concretely, this invention is not limited by these.
<棒状の冶具を用いた実施例>
図1に示す撹拌装置において、図2に示すように、径3mmのステンレス製(SUS304)の2本の金属の棒42で形成された冶具4を、図3に示すように羽根21を挟むように設置し、下記実施例1及び2の製造を行った。尚、図4に示すように、冶具4は、羽根21及び回転軸2の形状に沿って設置されているが、これらと接触しないように、冶具4と羽根21及び回転軸2とは0.1〜5mm程度の空間を設けた。
<Example using a rod-shaped jig>
In the stirring device shown in FIG. 1, as shown in FIG. 2, the jig 4 formed of two metal rods 42 made of stainless steel (SUS304) having a diameter of 3 mm is sandwiched between the blades 21 as shown in FIG. The following Examples 1 and 2 were produced. As shown in FIG. 4, the jig 4 is installed along the shapes of the blades 21 and the rotating shaft 2, but the jig 4, the blades 21, and the rotating shaft 2 are not more than 0. A space of about 1 to 5 mm was provided.
〔実施例1〕
オルトリン酸−メラミンを、加熱しながら、回転速度5(min-1)で撹拌し、200〜260℃で脱水縮合反応させる連続運転を行った。
[Example 1]
The ortho-phosphoric acid-melamine was stirred at a rotational speed of 5 (min −1 ) while being heated and subjected to a dehydration condensation reaction at 200 to 260 ° C.
〔実施例2〕
ポリフェニレンエーテル10kgと無水マレイン酸200gを撹拌装置中に投入し、内容物を撹拌しなから窒素置換した。窒素置換後、撹拌装置を密封し、内容物を回転速度5(min-1)で撹拌しながら、室温から180℃まで1時間かけて昇温した。5分間180℃を保持したあと、1時間かけて室温まで冷却した。
[Example 2]
10 kg of polyphenylene ether and 200 g of maleic anhydride were put into a stirrer, and the contents were replaced with nitrogen without stirring. After purging with nitrogen, the stirring apparatus was sealed, and the contents were heated from room temperature to 180 ° C. over 1 hour while stirring at a rotational speed of 5 (min −1 ). After maintaining at 180 ° C. for 5 minutes, it was cooled to room temperature over 1 hour.
<板状の冶具を用いた実施例>
図1に示す撹拌装置において、図5に示すように、幅30mm、厚さ3mmのステンレス製(SUS304)の2枚の金属の板43で形成され、下端部が屈曲して16mmの長さでL字状を形成する冶具4を、図6に示すように羽根21を挟むように設置し、実施例3の製造を行った。尚、冶具4は、羽根21及び回転軸2の形状に沿って設置されているが、これらと接触しないように、冶具4と羽根21及び回転軸2とは0.1〜5mm程度の空間を設けた。
<Example using a plate-shaped jig>
In the stirring apparatus shown in FIG. 1, as shown in FIG. 5, it is formed of two metal plates 43 made of stainless steel (SUS304) having a width of 30 mm and a thickness of 3 mm, and its lower end is bent to a length of 16 mm. The jig 4 forming an L shape was installed so as to sandwich the blade 21 as shown in FIG. 6, and Example 3 was manufactured. In addition, although the jig 4 is installed along the shape of the blade | wing 21 and the rotating shaft 2, the jig | tool 4, the blade | wing 21, and the rotating shaft 2 have a space of about 0.1-5 mm so that these may not be contacted. Provided.
〔実施例3〕
オルトリン酸−メラミンを、加熱しながら、回転速度5(min-1)で撹拌し、200〜260℃で脱水縮合反応させる連続運転を行った。
Example 3
The ortho-phosphoric acid-melamine was stirred at a rotational speed of 5 (min −1 ) while being heated and subjected to a dehydration condensation reaction at 200 to 260 ° C.
〔比較例1及び比較例2〕
冶具4を取り外した以外は、実施例1又は2と同様な手順にて実施した。
上記実施例1及び2並びに比較例1及び2の結果について、それぞれ下記表1に示す。
[Comparative Example 1 and Comparative Example 2]
The same procedure as in Example 1 or 2 was performed except that the jig 4 was removed.
The results of Examples 1 and 2 and Comparative Examples 1 and 2 are shown in Table 1 below.
比較例1及び2より、8時間の連続運転中に羽根への付着物が多数発生し、付着物を取り除くため運転を中断せざるをえなかった。また、得られた製品をIR分析したところ、未反応の原料の存在が確認された。 From Comparative Examples 1 and 2, many deposits were generated on the blades during continuous operation for 8 hours, and the operation had to be interrupted to remove the deposits. Further, when the obtained product was subjected to IR analysis, the presence of unreacted raw materials was confirmed.
これらに対し、実施例1〜3より、本発明の撹拌装置を用いた製造方法によれば、8時間の連続運転は問題なく行うことができ、安定生産を達成できることが確認できた。また、実施例2で得られた製品をIR分析したところ、原料が反応して所望の製品が得られていることが確認できた。 On the other hand, from Examples 1 to 3, it was confirmed that according to the production method using the stirring apparatus of the present invention, the continuous operation for 8 hours can be performed without any problem and stable production can be achieved. Further, when the product obtained in Example 2 was subjected to IR analysis, it was confirmed that the desired product was obtained by the reaction of the raw materials.
冶具を備えた本発明の撹拌装置を用いることにより、粘着状の物質であっても撹拌装置内部の付着を抑制し、長時間の連続運転を行えることを確認できた。 By using the stirrer of the present invention provided with a jig, it was confirmed that even if it was an adhesive substance, adhesion inside the stirrer was suppressed and continuous operation for a long time could be performed.
1 ケーシング
11 媒体循環路
12 ジャケット
13 熱媒入口
14 熱媒出口
2 回転軸
21 羽根
22 ギア
23 スプロケット
24 スプロケット
25 チェーン
26 ロータリージョイント
27 ロータリージョイント
3 カバー体
31 原料投入口
32 ガス排出口
33 製品排出口
4 冶具
41 支持台
42 金属の棒
43 金属の板
DESCRIPTION OF SYMBOLS 1 Casing 11 Medium circulation path 12 Jacket 13 Heat medium inlet 14 Heat medium outlet 2 Rotating shaft 21 Blade 22 Gear 23 Sprocket 24 Sprocket 25 Chain 26 Rotary joint 27 Rotary joint 3 Cover body 31 Material inlet 32 Gas outlet 33 Product outlet 4 Jig 41 Support stand 42 Metal rod 43 Metal plate
Claims (4)
上記撹拌機が羽根を有する構造であって、該羽根を挟接する冶具を備えることに特徴を有する撹拌装置。 A stirrer, a heating means, and a container for storing them, and the contents put in the container are stirred by the stirrer while being heated by the heating means, whereby the water or solvent contained in the contents or In a stirrer for removing water, alcohol or volatile matter generated by the reaction of the contents,
An agitator having a structure in which the agitator has blades, and includes a jig for sandwiching the blades.
上記撹拌機が羽根を有する構造であって、該羽根を挟接する冶具を備えることに特徴を有するピロリン酸化合物の製造装置。 A stirrer, a heating means, and a container for storing them are provided, and the orthophosphoric acid compound charged in the container is stirred by the stirrer while being heated by the heating means so as to be at a temperature of 120 to 350 ° C. In the production apparatus for removing water, alcohol or volatile matter generated by the reaction of water or a solvent or the orthophosphoric acid compound contained in the orthophosphoric acid compound,
An apparatus for producing a pyrophosphate compound, wherein the agitator has a structure having blades, and includes a jig for sandwiching the blades.
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JP2013020253A JP2014151233A (en) | 2013-02-05 | 2013-02-05 | Agitating device having attachment removing jig |
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