JP5726164B2 - 成形金属粒子の製造およびその使用 - Google Patents
成形金属粒子の製造およびその使用 Download PDFInfo
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- JP5726164B2 JP5726164B2 JP2012501247A JP2012501247A JP5726164B2 JP 5726164 B2 JP5726164 B2 JP 5726164B2 JP 2012501247 A JP2012501247 A JP 2012501247A JP 2012501247 A JP2012501247 A JP 2012501247A JP 5726164 B2 JP5726164 B2 JP 5726164B2
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- acid
- particles
- groups
- transition metal
- copolymers
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- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- JCBJVAJGLKENNC-UHFFFAOYSA-M potassium ethyl xanthate Chemical compound [K+].CCOC([S-])=S JCBJVAJGLKENNC-UHFFFAOYSA-M 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- ZTHBGWDIOJXYNC-UHFFFAOYSA-M potassium;hexoxymethanedithioate Chemical compound [K+].CCCCCCOC([S-])=S ZTHBGWDIOJXYNC-UHFFFAOYSA-M 0.000 description 1
- PEEXCRJDFUVJRT-UHFFFAOYSA-M potassium;methoxymethanedithioate Chemical compound [K+].COC([S-])=S PEEXCRJDFUVJRT-UHFFFAOYSA-M 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- MCSINKKTEDDPNK-UHFFFAOYSA-N propyl propionate Chemical compound CCCOC(=O)CC MCSINKKTEDDPNK-UHFFFAOYSA-N 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
- 239000003009 skin protective agent Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000012419 sodium bis(2-methoxyethoxy)aluminum hydride Substances 0.000 description 1
- BEOOHQFXGBMRKU-UHFFFAOYSA-N sodium cyanoborohydride Chemical compound [Na+].[B-]C#N BEOOHQFXGBMRKU-UHFFFAOYSA-N 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- 239000012321 sodium triacetoxyborohydride Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 125000004079 stearyl 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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920000638 styrene acrylonitrile Polymers 0.000 description 1
- 229920006132 styrene block copolymer Polymers 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- VSJBBIJIXZVVLQ-UHFFFAOYSA-N tert-butyl 3,5,5-trimethylhexaneperoxoate Chemical compound CC(C)(C)CC(C)CC(=O)OOC(C)(C)C VSJBBIJIXZVVLQ-UHFFFAOYSA-N 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- XKXIQBVKMABYQJ-UHFFFAOYSA-M tert-butyl carbonate Chemical compound CC(C)(C)OC([O-])=O XKXIQBVKMABYQJ-UHFFFAOYSA-M 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 125000003718 tetrahydrofuranyl group Chemical group 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- WJCNZQLZVWNLKY-UHFFFAOYSA-N thiabendazole Chemical compound S1C=NC(C=2NC3=CC=CC=C3N=2)=C1 WJCNZQLZVWNLKY-UHFFFAOYSA-N 0.000 description 1
- 239000004308 thiabendazole Substances 0.000 description 1
- 235000010296 thiabendazole Nutrition 0.000 description 1
- 229960004546 thiabendazole Drugs 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229960002663 thioctic acid Drugs 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- 235000010384 tocopherol Nutrition 0.000 description 1
- 229930003799 tocopherol Natural products 0.000 description 1
- 229960001295 tocopherol Drugs 0.000 description 1
- 239000011732 tocopherol Substances 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- DBGVGMSCBYYSLD-UHFFFAOYSA-N tributylstannane Chemical compound CCCC[SnH](CCCC)CCCC DBGVGMSCBYYSLD-UHFFFAOYSA-N 0.000 description 1
- 150000003627 tricarboxylic acid derivatives Chemical class 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 229960003500 triclosan Drugs 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
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- SCHZCUMIENIQMY-UHFFFAOYSA-N tris(trimethylsilyl)silicon Chemical compound C[Si](C)(C)[Si]([Si](C)(C)C)[Si](C)(C)C SCHZCUMIENIQMY-UHFFFAOYSA-N 0.000 description 1
- QUTYHQJYVDNJJA-UHFFFAOYSA-K trisilver;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Ag+].[Ag+].[Ag+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QUTYHQJYVDNJJA-UHFFFAOYSA-K 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229920001862 ultra low molecular weight polyethylene Polymers 0.000 description 1
- 238000001392 ultraviolet--visible--near infrared spectroscopy Methods 0.000 description 1
- 125000002948 undecyl 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])[H] 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 229920001866 very low density polyethylene Polymers 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 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
- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
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Description
a)遷移金属塩およびポリマー分散剤を含む水性混合物に還元剤を添加する工程と、続いて、
b)得られたコロイド分散体を過酸化物で処理する工程と
を含み、工程a)の水性混合物が、2mmol毎リットルより高い濃度の遷移金属塩を含む方法に関する。
a)還元剤の溶液と、遷移金属塩およびポリマー分散剤ならびに場合により添加剤を含む水性混合物とを混合して、球状金属粒子の分散体を形成する工程と、続いて、
b)前記分散体を過酸化物で処理する工程とを含み、前記球状粒子の制御的凝集を誘導してプレートレット成形金属粒子を形成させる方法である。
CH2=C(R2)−(C=O)−R3(I)
[式中、
R2は、水素またはCH3であり、
R3は、NH2、OH、O-(M+)、グリシジル、非置換C1〜C18アルコキシ、少なくとも1つのNR4および/またはO原子によって分断されたC2〜C1000アルコキシ、またはヒドロキシ置換C1〜C18アルコキシ、非置換C1〜C18アルキルアミノ、ジ(C1〜C18アルキル)アミノ、C5〜C11ヘテロシクロアルキル、ヒドロキシ置換C1〜C18アルキルアミノまたはヒドロキシ置換ジ(C1〜C18アルキル)アミノ、−O−CH2−CH2−N(CH3)2または−O−CH2−CH2−N+H(CH3)2An-または二環式もしくは三環式炭化水素の残基であり、
R4は、HまたはC1〜C18アルキルであり、
An-は、一価の有機酸または無機酸の陰イオンであり、
M+は、金属陽イオン、あるいは1つ以上のC1〜C4アルキルによって置換されていてもよいアンモニウムイオンである]のアクリレートから誘導することができる。
R5は、C1〜C25アルキル、フェニル、またはC1〜C18アルキルによって置換されたフェニルであり、
R6は、H、メチル、エチルまたはプロピルであり、
vは、1から1000の整数である]の基である。
R7−(OCH2CH2)xO−L−CO2M
[式中、
R7は、C8〜C24アルキルまたはC8〜C24アルケニル基であり、
xは、2から8であり、
Lは、−O−、−CO−、−COO−、−OCNR8、−NR8−、−CR9=CR10−もしくは−C≡C−によって分断され、かつ/またはケトン、エステルもしくはアミド基によって置換されていてもよいC1〜C12アルキレン基であり、R8、R9およびR10はH、C1〜C12アルキル、C5〜C12シクロアルキルまたはフェニルであり、
Mは、H、C1〜C4アルキルによって置換されていてもよいアンモニウムイオン、または金属陽イオンである]に対応する他のアルキルエーテルカルボキシレート。
R7−CO−[O−CH(CH3)−CO]y−CO2M
[式中、
R7は、C8〜C24アルキルまたはC8〜C24アルケニル基であり、
yは3から10であり、
Mは、H、C1〜C4アルキルによって置換されていてもよいアンモニウムイオン、または金属陽イオンである]に対応するアシルラクチレートであってもよい。例はナトリウムココイルラクチレートである。
Aは、R7−(OCH2CH2)x−O−およびアシルラクチレートであり、
AはR7−CO−[O−CH(CH3)−CO]y−であり、
nは1または2である]の有機ホスフェートも、上記アルキルエーテルカルボキシレートから誘導することができる好適なポリマー分散剤である。対応する塩も使用可能である。
R14−X−SH
[式中、
R14はC1〜C25アルキル、特にメチルもしくはエチル、フェニル、またはC1〜C18アルキルによって置換されたフェニルであり、
Xは、平均分子量が約1000から約6000、好ましくは約5000であるポリエチレングリコールまたはポリプロピレングリコールである]のチオールである。少なくとも部分的に水溶性の好適なチオールの例は、2−メルカプトエタノール、メルカプトブタノール、メルカプトヘキサノール、3−メルカプトプロピオン酸、11−メルカプトウンデカン酸、システインおよびホモシステイン等である。
R15、R16およびR17は、互いに独立して、H、C1〜C18アルキル、C2〜C18アルケニル、C2〜C18アルキニル、フェニル、C1〜C18アルキルによって置換されたフェニル、ポリエチレングリコールの基、ポリプロピレングリコールの基またはポリブチレングリコールの基である]のアミンである。好ましくは、アミンは、アンモニア、メチルアミン、ジメチルアミン、ジエチルアミン、アリルアミン、ブチルアミンまたはヘキシルアミン、より好ましくはアンモニアである。
a)遷移金属塩およびポリマー分散剤を含む水性混合物に還元剤を添加する工程と、続いて、
b)得られたコロイド分散体を過酸化物で処理する工程と
を含む(ただし、過酸化物の添加後に水溶性アミンを添加しない)方法に関する。
a)遷移金属塩の水溶液にアクリレートもしくはメタクリレートモノマーまたはオリゴマー、あるいはポリアクリレートもしくはポリメタクリレートおよび還元剤を添加する工程と、
b1)コロイド溶液を過酸化物で処理する工程、または
b2)コロイド溶液をUVまたは可視光に曝露する工程と、
c)水溶性アミンを添加する工程と、
d)ナノ成形遷移金属粒子を単離する、またはナノ成形遷移金属粒子を分散剤とともに液体アクリレートまたはメタクリレートモノマーに再分散する工程と
を含む方法を排除する。
a)以上に記載されているように製造された成形遷移金属粒子と、
b)熱可塑性または架橋性ポリマーと
からなる組成物に関する。
−60%未満の全太陽放射線透過率(340〜1800nm)、
−低い曇り度値、および
−60%超の全可視光透過率(400〜750nm)。
1.1.アルキル化モノフェノール、例えば、2,6−ジ−tert−ブチル−4−メチルフェノール、
1.2.アルキルチオメチルフェノール、例えば、2,4−ジオクチルチオメチル−6−tert−ブチルフェノール、
1.3.ヒドロキノンおよびアルキル化ヒドロキノン、例えば、2,6−ジ−tert−ブチル−4−メトキシフェノール、2,5−ジ−tert−ブチルヒドロキノン、
1.4.トコフェロール、例えば、α−トコフェロール、
1.5.ヒドロキシル化チオジフェニルエーテル、例えば、2,2’−チオビス(6−tert−ブチル−4−メチルフェノール)、
1.6.アルキリデンビスフェノール、例えば、2,2’−メチレンビス(6−tert−ブチル−4−メチルフェノール)、
1.7.O−、N−およびS−ベンジル化合物、例えば、3,5,3’,5’−テトラ−tert−ブチル−4,4’−ジヒドロキシジベンジルエーテル、
1.8.ヒドロキシベンジル化マロネート、例えば、ジオクタデシル−2,2−ビス(3,5−ジ−tert−ブチル−2−ヒドロキシベンジル)マロネート、
1.9.芳香族ヒドロキシベンジル化合物、例えば、1,3,5−トリス(3,5−ジ−tert−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、
1.10.トリアジン化合物、例えば、2,4−ビス(オクチルメルカプト)−6−(3,5−ジ−tert−4−ブチル−ヒドロキシアニリノ)−1,3,5−トリアジン、
1.11.ベンジルホスホネート、例えば、ジメチル−2,5−ジ−tert−ブチル−4−ヒドロキシベンジルホスホネート、
1.12.アシルアミノフェノール、例えば、4−ヒドロキシラウラニリド、
1.13.β−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオン酸と一価または多価アルコールとのエステル、
1.14.β−(5−tert−ブチル−4−ヒドロキシ−3−メチルフェニル)プロピオン酸と一価または多価アルコールとのエステル、
1.15.β−(3,5−ジシクロヘキシル−4−ヒドロキシフェニル)プロピオン酸と一価または多価アルコールとのエステル、
1.16.3,5−ジ−tert−ブチル−4−ヒドロキシフェニル酢酸と一価または多価アルコールとのエステル、
1.17.β−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオン酸のアミド、例えば、N,N’−ビス(3,5−ジ−tert−ブチル−4−ヒドロキシフェニルプロピオニル)ヘキサメチレンジアミド、
1.18.アスコルビン酸(ビタミンC)、
1.19.アミン系抗酸化剤、例えば、N,N’−ジ−イソプロピル−p−フェニレンジアミン。
2.1.2−(2’−ヒドロキシフェニル)ベンゾトリアゾール、例えば、2−(2’−ヒドロキシ−5’−メチルフェニル)−ベンゾトリアゾール、
2.2.2−ヒドロキシベンゾフェノン、例えば、4−ヒドロキシ誘導体、
2.3.置換および非置換安息香酸のエステル、例えば、サリチル酸4−tert−ブチル−フェニル、
2.4.アクリル酸、例えば、α−シアノ−β,β−ジフェニルアクリル酸エチル、
2.5.ニッケル化合物、例えば、2,2’−チオ−ビス[4−(1,1,3,3−テトラメチルブチル)フェノール]のニッケル化合物、
2.6.立体阻害アミン、例えば、ビス(2,2,6,6−テトラメチル−4−ピペリジル)セバケート、
2.7.オキサミド、例えば、4,4’−ジオクチルオキシオキサニリド、
2.8.2−(2−ヒドロキシフェニル)−1,3,5−トリアジン、例えば、2,4−ビス(2,4−ジメチルフェニル)−6(2−ヒドロキシ−4−オクチルオキシフェニル[または−4−ドデシル/トリデシルオキシフェニル])−1,3,5−トリアジン。
XaZnbOc (II)
XaYdNe (III)
[式中、
Xは、周期表の第IIIおよび/またはIV主族に属する元素の1種以上であり、
Yは、第III、IV、Vおよび/またはVI族に属する遷移金属であり(これらの族に属する元素の詳細については上記を参照されたい)、
指数a〜eは、成分の存在量をしめし、
式(II)は、a<b<cの条件に従い、
式(III)は、a<d≦eの条件に従う]によって表すことができる。例えばZnOまたはTiNにおけるAl、Gaおよび/またはInのドーピング量は、しばしば最終粒子材料の0.01から約20質量%、特に0.1から10質量%の範囲である。ナノ粒子は、固体であり、結晶質であることが多いが、必ずしもそうではない。それらを当該技術分野で既知の方法により、例えば、スパッタリング、熱蒸着法、化学蒸着(CVD)法、噴霧熱分解法およびゾルゲル法を用いて製造することができる。それらの材料は、しばしば市販されている。
−皮膚および髪の手入れのための化粧品組成物、例えば、ローション、クリーム、オイル、ジェル、パウダー、ワイプ(wipe)、スプレー、スティックおよびロールオンのような脱臭剤、シャワージェルのような磨き粉、入浴剤、(合成界面活性剤ならびに飽和および/または不飽和脂肪酸の塩に基づく)液体石鹸および固体石鹸、水性またはアルコール性溶液、例えば皮膚用洗浄液、湿性洗浄布、手の消毒剤、シャンプー、リンス等、
−例えばゲル、ペースト、クリームまたは水性製剤(洗口液)の形の口腔衛生組成物、
−硬質面洗浄剤、例えば、消毒スプレー、液またはパウダー、食器または洗濯洗剤(液体または固体)、床ワックス、ガラス洗浄剤等、ならびに
−工業および医療用途(例えば、機器、医療器具、手袋、コンタクトレンズ、コンタクトレンズケース、コンタクトレンズ保存液、コンタクトレンズ洗浄液)を含むが、それらに限定されない個人および家庭用手入れ用途、または工業および医療用途の様々な製品形態または組成物に利用することができる。
実施例1から16の一般的な調製手順
能率的撹拌棒を備えた丸底フラスコにおいて、脱イオン水、場合によりキャッピング剤、分散剤および遷移金属塩は、周囲雰囲気下で混合し、混合物を0℃まで冷却する。還元剤の水溶液を添加し、得られた遷移金属粒子の分散体を0℃で1時間撹拌した後、20℃で1時間撹拌する。所望のスペクトルプロファイルに達するまで過酸化物の水溶液を徐々に添加する。
能率的撹拌棒を備えた250mlの丸底フラスコ内の79mlの脱イオン水に1gのEFKA4580(40質量%水溶液)を溶解させる。340mg(2mmol)のAgNO3を添加し、得られた溶液を0℃まで冷却し、新たに調製した20mlのNaBH4(200mM)の氷冷水溶液を、激しく撹拌しながら1回で添加する。得られた褐色分散体を0℃で1時間撹拌し、5分(min)以内で20℃まで加温し、この温度で1時間撹拌する。20mlのH2O2(50%w/w水溶液)を0.1ml/分の量で添加して、濃青色の銀プレートレットの分散体を得る。
WO2004/045755の実施例2に従って調製したコポリマー(40w/w水中分散体)20g、エチレングリコール20gおよびMPEG−5000−チオール6gを、能率的撹拌機を備えた10lの調温器付き反応器内の1950mlの脱イオン水に溶解させる。−1℃まで冷却した後、10.2g(60mmol)のAgNO3を添加し、得られた溶液を15分間静かに撹拌する。4.54g(120mmol)のNaBH4を個別の容器中1lの脱イオン水に溶解させ、0℃まで冷却する。この溶液を、(500rpmで)激しく撹拌しながら、上記AgNO3の溶液に1回で添加する。反応混合物を0℃で5分間(500rpmで)激しく撹拌し、次いで1時間静かに撹拌しながら20℃まで加温する。150mlのH2O2(50%w/w水溶液)を(350rpmで)激しく撹拌しながら3ml/分の量で混合物に添加して、濃青色の銀プレートレットの分散体を得る。
2つの溶液を調製する。
溶液A:WO2004/045755の実施例2に従って調製したコポリマー(40w/w水中分散体)7gおよびMPEG−5000−チオール1.2gを20mlの脱イオン水に溶解させ、0℃まで冷却する。次いで、23mlの脱イオン水中2.04g(12mmol)のAgNO3の溶液を撹拌しながら添加し、得られた混合物を0℃まで冷却する。
2つの溶液を調製する。
溶液A:WO2004/045755の実施例2に従って調製したコポリマー(40w/w水中分散体)12gおよびMPEG−5000−チオール1.0gを15mlの脱イオン水に溶解させ、0℃まで冷却する。次いで、22mlの脱イオン水中3.4g(20mmol)のAgNO3の溶液を撹拌しながら添加し、得られた混合物を0℃まで冷却する。
4gのEFKA4580を実施例1で得られた分散体に添加した後、60mlのジエチレングリコールジメチルエーテル(ジグリム)を添加する。水を蒸発によって除去し、7.7mg/gの銀濃度を有する28gのジグリム中銀プレートレット分散体を得る。
実施例18で得られた分散体2gを98gのメタクリル酸メチルに混入し、100mgのアゾビスイソブチロニトリル(0.1%w/w)を添加し、混合物を、粒子凝集を防止するために連続的な音波処理下で70℃にて重合する。銀/ポリメチルメタクリレート複合体材料を得る。
10gのポリカーボネート(Makrolon(登録商標)を80mlの煮沸トルエンに溶解させる。実施例18で得られた分散体2gを添加し、混合物を周囲温度(20〜25℃)まで急速冷却する。トルエンを蒸発によって除去して、銀/ポリカーボネート複合材料を得る。
2gのポリビニルブチラール(Mn170000〜250000)を16gのエタノールに溶解させた後、実施例18で得られた分散体2gを添加して、銀/ポリビニルブチラール複合材料の粘性溶液を得る。
Claims (11)
- ナノプレートレットの形の成形遷移金属粒子を製造する方法であって、
前記金属は、Cu、Ag、Au、Zn、Cd、Ti、Cr、Mn、Fe、Co、Ni、Ru、Rh、Pd、Os、IrおよびPtからなる群から選択され、最初に、
a)遷移金属塩およびポリマー分散剤を含む水性混合物に還元剤の水溶液を添加する工程と、
b)得られたコロイド分散体を、450から2000nmまでの吸収極大値が達成されるまで過酸化物で処理する工程と
を含み、工程a)の水性混合物が、2mmol毎リットルより高い濃度の遷移金属塩を含み、かつさらなる還元剤を、過酸化物の添加前に添加しない方法。 - 工程a)において、チオール、二硫化物、キサンテート、ジチオカルバメート、アルコール、アミンおよび消泡剤からなる群から選択される少なくとも1つの添加剤が存在する、請求項1に記載の方法。
- 前記遷移金属塩が、特に、AgNO3、AgClO4、Ag2SO4、AgCl、AgBr、AgI、AgOH、Ag2O、AgBF4、AgIO3、AgPF6;R1CO2Ag、R1SO3Ag、ジカルボン酸、トリカルボン酸、ポリカルボン酸、ポリスルホン酸、P含有酸の銀塩、ならびにそれらの混合物からなる群から選択される銀(I)塩であり、
前記R1は、非置換もしくは置換C1〜C18アルキル、非置換もしくは置換C5〜C8シクロアルキル、非置換もしくは置換C7〜C18アラルキル、非置換もしくは置換C6〜C18アリールまたは非置換もしくは置換C2〜C18ヘテロアリールである、請求項1または2に記載の方法。 - 前記分散剤が、極性基を含むポリマーであり、そのポリマーは非イオン性またはイオン性である、請求項1から3までのいずれか1項に記載の方法。
- 前記分散剤が、ポリビニルアルコール、ポリ酢酸ビニル、ポリプロピオン酸ビニル、ポリビニルピロリドン、ポリビニルピロリジン、ポリエステル、ポリエチレンイミン、ポリビニルピリジンおよびそれらのコポリマーまたはブレンド;ポリエーテル、ポリウレタン、ポリアクリル樹脂、ポリエステル、ポリアミド、ポリアルキレングリコール、ビニルポリマー、芳香族ビニルポリマーに基づくポリマー、ランダムコポリマー、ABブロックコポリマー、櫛型コポリマーからなる群から選択され、それらのポリマーまたはコポリマーは、カルボキシレート基、スルホネート基、ホスホネート基、ヒドロキシ基、エーテル基、エステル基および/またはアミン基またはそれらのブレンドから選択される極性基で場合により部分的に中性化、四級化および/または変性されている、請求項1から4までのいずれか1項に記載の方法。
- 前記分散剤が、組成物の全質量に基づいて0.001から10質量%の濃度で工程a)の混合物に存在する、請求項1から5までのいずれか1項に記載の方法。
- 前記還元剤が、ボランおよびその錯体、金属ボラン酸塩、水素化物、アルミン酸塩、アルデヒド、カルボン酸、ヒドラジン、ハイドロサルファイト、スタンナン、スタネート、シラン、ホスフィン、ホスファイトおよびシロキサンからなる群から選択される、請求項1から6までのいずれか1項に記載の方法。
- カルボン酸含有添加剤の不在下で実施される、請求項1から7までのいずれか1項に記載の方法。
- 水を少なくとも部分的に有機媒体に取り替える工程c)をさらに含む、請求項1から8までのいずれか1項に記載の方法。
- 前記有機媒体が、有機溶媒、モノマー、オリゴマー、ポリマー、エマルジョンまたはそれらの組合せを含む、請求項9に記載の方法。
- 前記成形遷移金属粒子が、15から1000nmのエッジ長さの最長寸法および2から100nmの厚さを有するプレートレットの形である、請求項1から10までのいずれか1項に記載の方法。
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