JP4140729B2 - チタニア/粘土複合多孔体の製造方法 - Google Patents
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- JP4140729B2 JP4140729B2 JP2005172517A JP2005172517A JP4140729B2 JP 4140729 B2 JP4140729 B2 JP 4140729B2 JP 2005172517 A JP2005172517 A JP 2005172517A JP 2005172517 A JP2005172517 A JP 2005172517A JP 4140729 B2 JP4140729 B2 JP 4140729B2
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 370
- 239000004927 clay Substances 0.000 title claims description 103
- 239000002131 composite material Substances 0.000 title claims description 44
- 238000004519 manufacturing process Methods 0.000 title claims description 17
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- 238000001179 sorption measurement Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 230000002378 acidificating effect Effects 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
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- 229910021647 smectite Inorganic materials 0.000 claims description 2
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
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- 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
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 1
- ZOSIIFOALXTYQY-UHFFFAOYSA-M C(CCCCCCCCCCCCCCCCC)(=O)[O-].C(CCC)O[Ti+] Chemical compound C(CCCCCCCCCCCCCCCCC)(=O)[O-].C(CCC)O[Ti+] ZOSIIFOALXTYQY-UHFFFAOYSA-M 0.000 description 1
- DIICDKVONBLTBM-UHFFFAOYSA-L CC(C)O[Ti++]OC(C)C.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O Chemical compound CC(C)O[Ti++]OC(C)C.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O DIICDKVONBLTBM-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-L Oxalate Chemical compound [O-]C(=O)C([O-])=O MUBZPKHOEPUJKR-UHFFFAOYSA-L 0.000 description 1
- 101100258086 Postia placenta (strain ATCC 44394 / Madison 698-R) STS-01 gene Proteins 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
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- 150000001450 anions Chemical class 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
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- 231100000507 endocrine disrupting Toxicity 0.000 description 1
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- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 description 1
- 229910000271 hectorite Inorganic materials 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
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- 229910001410 inorganic ion Inorganic materials 0.000 description 1
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- 239000011812 mixed powder Substances 0.000 description 1
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- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
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- 229960005235 piperonyl butoxide Drugs 0.000 description 1
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- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- WSNJABVSHLCCOX-UHFFFAOYSA-J trilithium;trimagnesium;trisodium;dioxido(oxo)silane;tetrafluoride Chemical compound [Li+].[Li+].[Li+].[F-].[F-].[F-].[F-].[Na+].[Na+].[Na+].[Mg+2].[Mg+2].[Mg+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O WSNJABVSHLCCOX-UHFFFAOYSA-J 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Description
<実施形態>
本発明により結晶質チタニアと粘土が複合されたチタニア/粘土複合多孔体を、以下のような手順で調製することができる。
(実施例1)
結晶質チタニアと粘土が複合されたチタニア/粘土複合多孔体の調製を以下のように行った。すなわち、アナターゼを含有する強酸性チタニアゾル(テイカ株式会社製 TKS−202、pH値:1.1)を水で20倍に希釈した希釈液89mlに、ナトリウム−モンモリロナイト(クニミネ工業株式会社製 クニピア−F)2gを含む水懸濁液200mlを加え、室温で3時間攪拌した。この混合液中の配合比は粘土分に対するチタニア分の重量配合比で1:1にあたる。その後、遠心分離により固液分離を行い、得られた固形生成物の水洗をくり返し、その後、室温で自然乾燥し、さらに120℃の加熱を加えた。乾燥物の粉砕を行い、結晶質チタニアと粘土が複合されたチタニア/粘土複合多孔体粉末を得た。
実施例1におけるナトリウム−モンモリロナイトをナトリウム−合成フッ素マイカ(トピー工業株式会社製 Na−TS)に替え、他の条件は実施例1と同様にして、結晶質チタニアと粘土が複合されたチタニア/粘土複合多孔体粉末を調整した。この配合比は実施例1と同様に粘土分に対するチタニア分の重量配合比で1:1にあたる。
実施例1におけるチタニアゾルを中性のペルオキソチタン水溶液(株式会社鯤コーポレーション製 PTA85)に替え、ペルオキソチタン水溶液118mlを、ナトリウム−モンモリロナイト(クニミネ工業株式会社製 クニピア−F)1gを含む水懸濁液100mlと混合し、他の条件は実施例1と同様にして、チタニア/粘土複合体粉末を調整した。この配合比は粘土分に対するチタン化合物固形分の重量配合比で1:1にあたる。
実施例1におけるチタニアゾルをアナターゼを含有する中性のペルオキソチタン改質ゾル(株式会社鯤コーポレーション製 TO85)に替え、ペルオキソチタン改質ゾル118mlを、ナトリウム−モンモリロナイト(クニミネ工業株式会社製 クニピア−F)1gを含む水懸濁液100mlと混合し、他の条件は実施例1と同様にして、チタニア/粘土複合体粉末を調整した。この配合比は粘土分に対するチタン化合物固形分の重量配合比で1:1にあたる。
実施例1におけるチタニアゾルに替えて、光触媒チタニア微粉末(日本アエロジル株式会社製 P−25)2gを水200mlに分散したチタニア懸濁液を、ナトリウム−モンモリロナイト(クニミネ工業株式会社製 クニピア−F)2gを含む水懸濁液200mlと混合し、他の条件は実施例1と同様にして、チタニア/粘土混合粉末を調整した。この配合比は実施例1と同様に粘土分に対するチタニア分の重量配合比で1:1にあたる。
以上のようにして得られた実施例1〜2及び比較例1〜3の粉末について、蛍光X線分析法によるチタニア含有量測定、X線回折法による含有チタニアの結晶相の判定、窒素吸着法によるBET法比表面積測定を行った。
実施例1〜2及び比較例1〜3の粉末の蛍光X線分析法によるチタニア含有量測定、X線回折法による含有チタニアの結晶相の判定、窒素吸着法によるBET法比表面積測定の結果を表1に示す。
Claims (5)
- チタニア分散液またはチタニアゾルを膨潤性粘土に作用させてチタニア/粘土複合多孔体とするチタニア/粘土複合多孔体の製造方法であって、該チタニア分散液または該チタニアゾルのpHが0〜1.5の強酸性でありかつ該チタニア分散液または該チタニアゾル中に含有されるチタニアが結晶質であることを特徴とするチタニア/粘土複合多孔体の製造方法。
- 前記チタニア分散液または前記チタニアゾルを20倍までの倍率で水で希釈した希釈液を膨潤性粘土に作用させてチタニア/粘土複合多孔体とすることを特徴とする請求項1に記載のチタニア/粘土複合多孔体の製造方法。
- 前記チタニア分散液または前記チタニアゾル、あるいは前記希釈液中に含有されるチタニアの結晶相がアナターゼ、ブルッカイト、ルチルのいずれかであるかまたはこれらの混合であることを特徴とする請求項1または2のいずれかに記載のチタニア/粘土複合多孔体の製造方法。
- 製造される前記チタニア/粘土複合多孔体の窒素ガス吸着法によるBET法比表面積が70m2/g以上であることを特徴とする請求項1から3のいずれかに記載のチタニア/粘土複合多孔体の製造方法。
- 前記膨潤性粘土はスメクタイト、バーミキュライト、合成マイカおよびフッ素置換せしめたこれらの類似体の1種または2種以上の混合物であることを特徴とする請求項1から4のいずれかに記載のチタニア/粘土複合多孔体の製造方法。
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