JP6076266B2 - ナノ粒子の懸濁液の調製方法及びナノ粒子の懸濁液 - Google Patents
ナノ粒子の懸濁液の調製方法及びナノ粒子の懸濁液 Download PDFInfo
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- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000010951 particle size reduction Methods 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
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- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
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- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910000348 titanium sulfate 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
- 238000012795 verification Methods 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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Description
本実施例では、二酸化チタン粉末が金属酸化物粉末106とされ、水が分散媒102とされる。さらに、 表1に基づき、クエン酸が分散剤104として選択される。前記実施例では、10グラム(gm)のクエン酸ナトリウムを100ミリリットル(ml)の水に溶解し、この溶液に40gmの二酸化チタン、つまりチタニア粉末(Sumitomo Co. Japanから入手される)を加えて一次混合物110を得た。一次混合物110は、磁気撹拌を用いて分散させた。さらに、一次混合物110を磨砕するために、各々容積500mlを有する4つのよく洗浄されたメノウジャーを有するプラネタリーボールミルを用いた。ジャーに、1000gmの0.4〜0.7mmのZirconox磨砕媒体(Jyothi Ceramics、Nasik、Indiaから入手される)を詰め、ジャーの有効容積を総容積の約2/3に対応させた。
さらに、懸濁液の安定性を検査するために、懸濁液を時間に応じて監視した。この目的のために、実施例1に記載された手順によって4時間の磨砕後に得られた一次懸濁液の試料を、室温及び大気圧で30日間保存した。この元の試料中の粒子は80nmのd50径を有し、92.3%の粒子は100nmより微細であった。d50粒径は、体積で測定される粒径分布の中央値又は50パーセンタイルを表す。d50粒径は、粒子の50%がこの値以下の体積を有するような粒径分布に関する値である。保存された試料をクエン酸水で希釈し、4分間超音波処理し、粒径分析にかけた。試料は多少の凝集を示し、41.2%の割合は100nm未満であった。
様々な分散剤の効果を研究して、相互作用エネルギーに基づく分散剤の選択を検証するために、ポリアクリル酸及びカルボキシメチルセルロースを分散剤として、二酸化チタンを金属酸化物粉末として、及び水を分散媒として実施例1を繰り返した。
記載された方法は、分散剤及び分散媒の新たな組合せについても検査された。この目的のために、分散媒102としてエチルアルコールで実施例1を繰り返した。表3に基づき、p-ヒドロキシ安息香酸(SD Fine Chem Ltd. Indiaから入手された)を分散剤104として選択した。
実施例3と同様に、記載された方法は、分散剤及び分散媒の新組合せについて再び検査された。この目的のために、p-Span-80 Fluka USA (SD Fine Chem Ltd. Indiaから入手される)を分散剤104として、n-ブチルアセテートを分散媒102として実施例1を繰り返した。このように得られた非水性チタニアナノ粒子懸濁液の特性を、表5に示す。
102 分散媒
104 分散剤
106 金属酸化物粉末
110 一次混合物
112 ディスパーサー
114 グラインダー
116 懸濁液
118 粒径分析器
Claims (10)
- ナノ粒子の懸濁液の調製方法であって、
分散媒(102)を分散剤(104)及び金属酸化物粉末(106)と混合して一次混合物(110)を形成するステップであって、前記分散剤(104)は前記分散媒(102)の存在下で前記金属酸化物粉末(106)に対する前記分散剤(104)の相互作用エネルギーに基づいて選択される、混合ステップと、
一次混合物(110)を磨砕して懸濁液(116)を得るステップであって、前記分散剤(104)が所定の期間後に磨砕中に一次混合物(110)に加えられる、磨砕ステップと、を有し、
前記金属酸化物粉末(106)が二酸化チタンからなり、
前記懸濁液(116)中の金属酸化物粒子が100nm未満の平均径を有する方法。 - 前記分散媒(102)及び前記金属酸化物粉末(106)に対する複数の見込みがある分散剤の相互作用エネルギーを、分子モデリング技法を用いて計算する計算ステップと、
前記複数の見込みがある分散剤から計算された相互作用エネルギーに基づいて分散剤(104)を選択する選択ステップと、をさらに含む請求項1に記載の方法。 - 前記金属酸化物粉末(106)が、0.1ミクロンから100ミクロンの範囲内の平均粒径を有する少なくとも1種の金属酸化物の粒子を含む、請求項1に記載の方法。
- 前記混合ステップが前記一次混合物(110)を分散させて前記一次混合物(110)のスラリーを形成する分散ステップをさらに含む、請求項1に記載の方法。
- 前記分散剤(104)及び前記分散媒(102)を前記懸濁液(116)に加えて希釈懸濁液を得る追加ステップと、
前記希釈懸濁液を分散させて分散希釈懸濁液を得る分散ステップと、をさらに含む、請求項1に記載の方法。 - 前記分散ステップが超音波処理及び磁気撹拌の1つを用いて行われる、請求項4又は請求項5に記載の方法。
- 前記一次混合物(110)を磨砕する磨砕ステップが前記一次混合物(110)を湿式粉砕して前記懸濁液(116)を得るステップを含む、請求項1に記載の方法。
- 前記一次混合物(110)を磨砕する間、前記一次混合物(110)中の金属酸化物粒子の粒径を定期的に測定する測定ステップをさらに含み、前記一次混合物(110)が、金属酸化物粒子の平均粒径が100nm未満になるまで磨砕される、請求項1に記載の方法。
- 前記分散媒(102)が水、油、グリコール、アルコール及びエステルの少なくとも1つである、請求項1に記載の方法。
- 前記分散剤(104)が、カルボン酸、エステル、エーテル、アルコール、糖、糖誘導体、ホスフェート、及びアミンの少なくとも1つである、請求項1に記載の方法。
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