JP6144331B2 - 固溶体顔料ナノ粒子分散液 - Google Patents
固溶体顔料ナノ粒子分散液 Download PDFInfo
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- JP6144331B2 JP6144331B2 JP2015257232A JP2015257232A JP6144331B2 JP 6144331 B2 JP6144331 B2 JP 6144331B2 JP 2015257232 A JP2015257232 A JP 2015257232A JP 2015257232 A JP2015257232 A JP 2015257232A JP 6144331 B2 JP6144331 B2 JP 6144331B2
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- 150000002739 metals Chemical class 0.000 description 1
- 229940098779 methanesulfonic acid Drugs 0.000 description 1
- 229940057867 methyl lactate Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- QJQAMHYHNCADNR-UHFFFAOYSA-N n-methylpropanamide Chemical compound CCC(=O)NC QJQAMHYHNCADNR-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229940116315 oxalic acid Drugs 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 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
- 239000003973 paint Substances 0.000 description 1
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000001054 red pigment Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229940079101 sodium sulfide Drugs 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- ZGHLCBJZQLNUAZ-UHFFFAOYSA-N sodium sulfide nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[S-2] ZGHLCBJZQLNUAZ-UHFFFAOYSA-N 0.000 description 1
- 229940048181 sodium sulfide nonahydrate Drugs 0.000 description 1
- WBQTXTBONIWRGK-UHFFFAOYSA-N sodium;propan-2-olate Chemical compound [Na+].CC(C)[O-] WBQTXTBONIWRGK-UHFFFAOYSA-N 0.000 description 1
- WMDLZMCDBSJMTM-UHFFFAOYSA-M sodium;sulfanide;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[SH-] WMDLZMCDBSJMTM-UHFFFAOYSA-M 0.000 description 1
- 238000000371 solid-state nuclear magnetic resonance spectroscopy Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- PWEBUXCTKOWPCW-UHFFFAOYSA-N squaric acid Chemical compound OC1=C(O)C(=O)C1=O PWEBUXCTKOWPCW-UHFFFAOYSA-N 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- LBMZLLXZMSMJPJ-UHFFFAOYSA-N thiepane 1-oxide Chemical compound O=S1CCCCCC1 LBMZLLXZMSMJPJ-UHFFFAOYSA-N 0.000 description 1
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
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- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/06—Zinc compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0269—Solid material in other moving receptacles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic Table
- C07F1/08—Copper compounds
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0014—Influencing the physical properties by treatment with a liquid, e.g. solvents
- C09B67/0016—Influencing the physical properties by treatment with a liquid, e.g. solvents of phthalocyanines
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0017—Influencing the physical properties by treatment with an acid, H2SO4
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0017—Influencing the physical properties by treatment with an acid, H2SO4
- C09B67/0019—Influencing the physical properties by treatment with an acid, H2SO4 of phthalocyanines
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0025—Crystal modifications; Special X-ray patterns
- C09B67/0026—Crystal modifications; Special X-ray patterns of phthalocyanine pigments
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0033—Blends of pigments; Mixtured crystals; Solid solutions
- C09B67/0034—Mixtures of two or more pigments or dyes of the same type
- C09B67/0035—Mixtures of phthalocyanines
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
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- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0092—Dyes in solid form
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
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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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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Description
この鏡面研磨の面粗度は、特に限定されないが、好ましくはRa0.01〜1.0μm、より好ましくはRa0.03〜0.3μmとする。
このように、3次元的に変位可能に保持するフローティング機構によって、第2処理用部20を保持することが望ましい。
P=P1×(K−k)+Ps
なお、図示は省略するが、近接用調整面24を離反用調整面23よりも広い面積を持ったものとして実施することも可能である。
この凹部13の先端と第1処理用面1の外周面との間には、凹部13のない平坦面16が設けられている。
例えば、上記の複数の顔料溶液を処理用面1,2間に導入する場合、それぞれの顔料溶液の顔料濃度を一定としてそのうちの少なくとも何れか1種類の顔料溶液の処理用面1,2間への導入速度を変化させてもよく、2種類以上の顔料を溶媒に溶解して調整した1種類の顔料溶液を処理用面1,2間に導入する場合、処理用面1,2間への顔料溶液の導入速度を一定として、顔料溶液の顔料濃度を変化させてもよい。
その他、顔料溶液を処理用面1,2間に導入する直前もしくは、顔料析出用溶媒と混合する直前にて希釈して顔料濃度を変更するなどの方法が挙げられる。
実施例1〜5として、図1に示すように、対向して配設された接近・離反可能な処理用面をもつ、少なくとも一方が他方に対して回転する処理用面1,2の間にできる薄膜流体中で、均一に拡散・攪拌・混合する反応装置を用いて、顔料溶液と顔料析出用溶媒とを混合し、薄膜流体中で析出反応を行う。
吐出された固溶体顔料ナノ粒子分散液中より不純物を除去するために、固溶体顔料ナノ粒子を緩く凝集させ、凝集された固溶体顔料ナノ粒子を濾集し、純水にて洗浄して固溶体顔料ナノ粒子ペーストを得た。
得られた固溶体顔料ナノ粒子ペーストの一部を60℃、−0.01MPaGの条件で乾燥し、固溶体顔料ナノ粒子粉体を得た。また、得られた固溶体顔料ナノ粒子ペーストの一部に純水及びドデシル硫酸ナトリウム(SDS)を加え、超音波分散機にて分散処理し、固溶体顔料ナノ粒子分散液を作製した。
比較例として、ビーカーを用いて実験を行った。ビーカー中で純水を攪拌しながら、銅フタロシアニン及び臭素化塩素化亜鉛フタロシアニングリーンの異なる2種の顔料を発煙硫酸(SO3濃度:30%)に溶解した顔料溶液を投入した。
中央から第1流体の顔料析出用溶媒として、9.5wt%の硫化ナトリウム九水和物(Na2S・9H2O)を純水に溶解した硫化ナトリウム水溶液(Na2S aq)を供給圧力/背圧力=0.50MPaG / 0.10MPaG、回転数1700rpmで送液し、硝酸亜鉛六水和物(Zn(NO3)2・6H2O)及び硝酸マンガン六水和物(Mn(NO3)2・6H2O)の異なる2種類の顔料を純水に溶解した顔料溶液を第2流体として処理用面1,2間に導入した。第1流体と第2流体を薄膜流体中で混合し、白色顔料である硫化亜鉛(ZnS)と淡紅色顔料である硫化マンガン(MnS)の固溶体顔料ナノ粒子分散液として処理用面1,2間より吐出された。
吐出された固溶体顔料ナノ粒子分散液中より不純物を除去するために、固溶体顔料ナノ粒子を緩く凝集させ、凝集された固溶体顔料ナノ粒子を濾集し、純水にて洗浄して固溶体顔料ナノ粒子ペーストを得た。
得られた固溶体顔料ナノ粒子ペーストの一部を60℃、−0.01MPaGの条件で乾燥し、固溶体顔料ナノ粒子粉体を得た。また、得られた固溶体顔料ナノ粒子ペーストの一部にメタノール及び分散剤(チオカルコール08:花王製)を加え、超音波分散機にて分散処理し、固溶体顔料ナノ粒子分散液を作製した。
比較例3として、ビーカーを用いて実験を行った。ビーカー中で純水を攪拌しながら、硝酸亜鉛六水和物(Zn(NO3)2・6H2O)及び硝酸マンガン六水和物(Mn(NO3)2・6H2O)の異なる2種類の顔料を純水に溶解した顔料溶液を投入した。
2 第2処理用面
10 第1処理用部
11 第1ホルダ
20 第2処理用部
21 第2ホルダ
d1 第1導入部
d2 第2導入部
d20 開口部
Claims (2)
- 銅フタロシアニン及び臭素化塩素化亜鉛フタロシアニンからなる固溶体顔料ナノ粒子を分散させた顔料分散液であって、
上記固溶体顔料ナノ粒子は、
体積平均粒子径が100nm以下であり、
観測条件25万倍以上のTEM−EDS測定を用いて求めた、上記固溶体顔料ナノ粒子の一次粒子中の固溶比が5.19〜0.42であり、
上記固溶体顔料ナノ粒子についてICP発光分光分析によって求められた固溶比に対するTEM−EDS測定によって求められた上記固溶比の精度が20%以内であることを特徴とする、固溶体顔料ナノ粒子分散液。 - 350nm〜800nmの波長領域における、透過スペクトル測定における最大透過率の波長(Tλmax)が、471nm〜511nmの範囲にあることを特徴とする、請求項1に記載の固溶体顔料ナノ粒子分散液。
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