JPS6327294B2 - - Google Patents

Info

Publication number

JPS6327294B2

JPS6327294B2 JP7888381A JP7888381A JPS6327294B2 JP S6327294 B2 JPS6327294 B2 JP S6327294B2 JP 7888381 A JP7888381 A JP 7888381A JP 7888381 A JP7888381 A JP 7888381A JP S6327294 B2 JPS6327294 B2 JP S6327294B2

Authority

JP

Japan

Prior art keywords

earth metal

alkaline earth

reaction

tio

oxyalkoxide

Prior art date

1981-05-25

Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)

Expired

Links

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• 239000010936 titanium Substances 0.000 claims description 32
• -1 titanium alkoxide Chemical class 0.000 claims description 23
• 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 16
• 229910052719 titanium Inorganic materials 0.000 claims description 13
• 238000004519 manufacturing process Methods 0.000 claims description 12
• 150000001342 alkaline earth metals Chemical group 0.000 claims description 7
• 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims description 5
• 150000002430 hydrocarbons Chemical group 0.000 claims description 5
• XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
• 239000004215 Carbon black (E152) Substances 0.000 claims description 4
• 125000000217 alkyl group Chemical group 0.000 claims description 4
• 229910052788 barium Inorganic materials 0.000 claims description 4
• 229930195733 hydrocarbon Natural products 0.000 claims description 4
• 125000004432 carbon atom Chemical group C* 0.000 claims description 3
• 238000005979 thermal decomposition reaction Methods 0.000 claims description 3
• 229910052712 strontium Inorganic materials 0.000 claims description 2
• 238000000354 decomposition reaction Methods 0.000 claims 1
• 238000006243 chemical reaction Methods 0.000 description 28
• 239000000243 solution Substances 0.000 description 18
• 239000003960 organic solvent Substances 0.000 description 15
• 238000000034 method Methods 0.000 description 14
• 239000000047 product Substances 0.000 description 13
• 239000002131 composite material Substances 0.000 description 11
• RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 10
• 239000002245 particle Substances 0.000 description 10
• 229910010413 TiO 2 Inorganic materials 0.000 description 9
• 238000000921 elemental analysis Methods 0.000 description 7
• 239000000463 material Substances 0.000 description 7
• 239000002994 raw material Substances 0.000 description 7
• 239000010419 fine particle Substances 0.000 description 6
• 239000007787 solid Substances 0.000 description 6
• LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
• KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
• 239000007789 gas Substances 0.000 description 5
• 239000000203 mixture Substances 0.000 description 5
• 239000000843 powder Substances 0.000 description 5
• 239000000126 substance Substances 0.000 description 5
• KVNYFPKFSJIPBJ-UHFFFAOYSA-N 1,2-diethylbenzene Chemical compound CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 4
• CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
• 238000005481 NMR spectroscopy Methods 0.000 description 4
• MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 4
• URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 4
• 238000009835 boiling Methods 0.000 description 4
• 150000001875 compounds Chemical class 0.000 description 4
• NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 4
• 238000009826 distribution Methods 0.000 description 4
• 230000007062 hydrolysis Effects 0.000 description 4
• 238000006460 hydrolysis reaction Methods 0.000 description 4
• LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
• 229910003514 Sr(OH) Inorganic materials 0.000 description 3
• JAWMENYCRQKKJY-UHFFFAOYSA-N [3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-ylmethyl)-1-oxa-2,8-diazaspiro[4.5]dec-2-en-8-yl]-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone Chemical compound N1N=NC=2CN(CCC=21)CC1=NOC2(C1)CCN(CC2)C(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F JAWMENYCRQKKJY-UHFFFAOYSA-N 0.000 description 3
• 238000004821 distillation Methods 0.000 description 3
• 239000003495 polar organic solvent Substances 0.000 description 3
• 238000010992 reflux Methods 0.000 description 3
• 150000003839 salts Chemical class 0.000 description 3
• 238000003756 stirring Methods 0.000 description 3
• YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
• XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
• 238000002441 X-ray diffraction Methods 0.000 description 2
• 239000012298 atmosphere Substances 0.000 description 2
• 125000004429 atom Chemical group 0.000 description 2
• AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
• FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
• 229910002092 carbon dioxide Inorganic materials 0.000 description 2
• 239000001569 carbon dioxide Substances 0.000 description 2
• 239000000470 constituent Substances 0.000 description 2
• 238000007796 conventional method Methods 0.000 description 2
• 230000003301 hydrolyzing effect Effects 0.000 description 2
• 239000012535 impurity Substances 0.000 description 2
• 238000002156 mixing Methods 0.000 description 2
• 239000000178 monomer Substances 0.000 description 2
• 239000012299 nitrogen atmosphere Substances 0.000 description 2
• 230000000704 physical effect Effects 0.000 description 2
• 239000011541 reaction mixture Substances 0.000 description 2
• 230000035484 reaction time Effects 0.000 description 2
• 239000002002 slurry Substances 0.000 description 2
• VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
• PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 2
• KTXWGMUMDPYXNN-UHFFFAOYSA-N 2-ethylhexan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCCC(CC)C[O-].CCCCC(CC)C[O-].CCCCC(CC)C[O-].CCCCC(CC)C[O-] KTXWGMUMDPYXNN-UHFFFAOYSA-N 0.000 description 1
• NVJALIGNTUTVQO-UHFFFAOYSA-N CCCCO[Ti](OCC)(OCC)OCCCC Chemical compound CCCCO[Ti](OCC)(OCC)OCCCC NVJALIGNTUTVQO-UHFFFAOYSA-N 0.000 description 1
• MCALDHMLXICSKJ-UHFFFAOYSA-N CCO[Ti](OCC)(OC(C)C)OC(C)C Chemical compound CCO[Ti](OCC)(OC(C)C)OC(C)C MCALDHMLXICSKJ-UHFFFAOYSA-N 0.000 description 1
• CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
• VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
• 229910002367 SrTiO Inorganic materials 0.000 description 1
• 229910010252 TiO3 Inorganic materials 0.000 description 1
• 150000001242 acetic acid derivatives Chemical class 0.000 description 1
• 239000002253 acid Substances 0.000 description 1
• 239000000654 additive Substances 0.000 description 1
• 238000005054 agglomeration Methods 0.000 description 1
• 230000002776 aggregation Effects 0.000 description 1
• 125000003158 alcohol group Chemical group 0.000 description 1
• 230000001476 alcoholic effect Effects 0.000 description 1
• 239000007864 aqueous solution Substances 0.000 description 1
• 229910052786 argon Inorganic materials 0.000 description 1
• RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
• 229910001863 barium hydroxide Inorganic materials 0.000 description 1
• 229910001422 barium ion Inorganic materials 0.000 description 1
• GXUARMXARIJAFV-UHFFFAOYSA-L barium oxalate Chemical compound [Ba+2].[O-]C(=O)C([O-])=O GXUARMXARIJAFV-UHFFFAOYSA-L 0.000 description 1
• 229940094800 barium oxalate Drugs 0.000 description 1
• 238000007664 blowing Methods 0.000 description 1
• 239000006227 byproduct Substances 0.000 description 1
• 239000003054 catalyst Substances 0.000 description 1
• 239000003795 chemical substances by application Substances 0.000 description 1
• 238000011109 contamination Methods 0.000 description 1
• RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
• 239000013078 crystal Substances 0.000 description 1
• 238000007598 dipping method Methods 0.000 description 1
• XGZNHFPFJRZBBT-UHFFFAOYSA-N ethanol;titanium Chemical compound [Ti].CCO.CCO.CCO.CCO XGZNHFPFJRZBBT-UHFFFAOYSA-N 0.000 description 1
• 238000001704 evaporation Methods 0.000 description 1
• 239000000835 fiber Substances 0.000 description 1
• 239000010408 film Substances 0.000 description 1
• 238000001914 filtration Methods 0.000 description 1
• 238000007710 freezing Methods 0.000 description 1
• 230000008014 freezing Effects 0.000 description 1
• 239000011521 glass Substances 0.000 description 1
• 238000010438 heat treatment Methods 0.000 description 1
• 239000012456 homogeneous solution Substances 0.000 description 1
• XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
• 150000004679 hydroxides Chemical class 0.000 description 1
• 239000011261 inert gas Substances 0.000 description 1
• 150000002500 ions Chemical class 0.000 description 1
• 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
• 239000007788 liquid Substances 0.000 description 1
• 238000005259 measurement Methods 0.000 description 1
• ZEIWWVGGEOHESL-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC.OC.OC.OC ZEIWWVGGEOHESL-UHFFFAOYSA-N 0.000 description 1
• 239000011859 microparticle Substances 0.000 description 1
• 238000002715 modification method Methods 0.000 description 1
• 235000006408 oxalic acid Nutrition 0.000 description 1
• 229920000642 polymer Polymers 0.000 description 1
• 229910052573 porcelain Inorganic materials 0.000 description 1
• 239000002244 precipitate Substances 0.000 description 1
• 238000011160 research Methods 0.000 description 1
• 238000004626 scanning electron microscopy Methods 0.000 description 1
• 238000000926 separation method Methods 0.000 description 1
• 238000007086 side reaction Methods 0.000 description 1
• 238000005245 sintering Methods 0.000 description 1
• 238000003746 solid phase reaction Methods 0.000 description 1
• 239000002904 solvent Substances 0.000 description 1
• 238000005507 spraying Methods 0.000 description 1
• 239000007858 starting material Substances 0.000 description 1
• 239000010409 thin film Substances 0.000 description 1
• 239000008096 xylene Substances 0.000 description 1