CN1742059A - 片状颜料 - Google Patents
片状颜料 Download PDFInfo
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- CN1742059A CN1742059A CNA2004800025747A CN200480002574A CN1742059A CN 1742059 A CN1742059 A CN 1742059A CN A2004800025747 A CNA2004800025747 A CN A2004800025747A CN 200480002574 A CN200480002574 A CN 200480002574A CN 1742059 A CN1742059 A CN 1742059A
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- Prior art keywords
- layer
- sio
- pigment
- metal
- tio
- Prior art date
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-M oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC([O-])=O ZQPPMHVWECSIRJ-KTKRTIGZSA-M 0.000 description 1
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- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 125000000913 palmityl 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])[H] 0.000 description 1
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- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 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
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- 150000002989 phenols Chemical class 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 1
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- 239000011669 selenium Substances 0.000 description 1
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- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- LUPNKHXLFSSUGS-UHFFFAOYSA-M sodium;2,2-dichloroacetate Chemical compound [Na+].[O-]C(=O)C(Cl)Cl LUPNKHXLFSSUGS-UHFFFAOYSA-M 0.000 description 1
- NGSFWBMYFKHRBD-UHFFFAOYSA-N sodium;2-hydroxypropanoic acid Chemical compound [Na+].CC(O)C(O)=O NGSFWBMYFKHRBD-UHFFFAOYSA-N 0.000 description 1
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- 229920005613 synthetic organic polymer Polymers 0.000 description 1
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- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 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
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
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- AFCAKJKUYFLYFK-UHFFFAOYSA-N tetrabutyltin Chemical compound CCCC[Sn](CCCC)(CCCC)CCCC AFCAKJKUYFLYFK-UHFFFAOYSA-N 0.000 description 1
- PEQHIRFAKIASBK-UHFFFAOYSA-N tetraphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 PEQHIRFAKIASBK-UHFFFAOYSA-N 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
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- 239000010496 thistle oil Substances 0.000 description 1
- 230000002992 thymic effect Effects 0.000 description 1
- 239000001585 thymus vulgaris Substances 0.000 description 1
- 229940098465 tincture Drugs 0.000 description 1
- 229910021341 titanium silicide 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
- 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 1
- 229930003799 tocopherol Natural products 0.000 description 1
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- 239000011732 tocopherol Substances 0.000 description 1
- 235000010384 tocopherol Nutrition 0.000 description 1
- 230000000699 topical effect Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000001069 triethyl citrate Substances 0.000 description 1
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 1
- 235000013769 triethyl citrate Nutrition 0.000 description 1
- BYMUNNMMXKDFEZ-UHFFFAOYSA-K trifluorolanthanum Chemical compound F[La](F)F BYMUNNMMXKDFEZ-UHFFFAOYSA-K 0.000 description 1
- XRADHEAKQRNYQQ-UHFFFAOYSA-K trifluoroneodymium Chemical compound F[Nd](F)F XRADHEAKQRNYQQ-UHFFFAOYSA-K 0.000 description 1
- SLGBZMMZGDRARJ-UHFFFAOYSA-N triphenylene Chemical compound C1=CC=C2C3=CC=CC=C3C3=CC=CC=C3C2=C1 SLGBZMMZGDRARJ-UHFFFAOYSA-N 0.000 description 1
- LZTRCELOJRDYMQ-UHFFFAOYSA-N triphenylmethanol Chemical compound C=1C=CC=CC=1C(C=1C=CC=CC=1)(O)C1=CC=CC=C1 LZTRCELOJRDYMQ-UHFFFAOYSA-N 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- ORHBXUUXSCNDEV-UHFFFAOYSA-N umbelliferone Chemical compound C1=CC(=O)OC2=CC(O)=CC=C21 ORHBXUUXSCNDEV-UHFFFAOYSA-N 0.000 description 1
- HFTAFOQKODTIJY-UHFFFAOYSA-N umbelliferone Natural products Cc1cc2C=CC(=O)Oc2cc1OCC=CC(C)(C)O HFTAFOQKODTIJY-UHFFFAOYSA-N 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 235000011912 vitamin B7 Nutrition 0.000 description 1
- 239000011735 vitamin B7 Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 239000007762 w/o emulsion Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical group [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0051—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating low and high refractive indices, wherein the first coating layer on the core surface has the low refractive index
- C09C1/0057—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating low and high refractive indices, wherein the first coating layer on the core surface has the low refractive index comprising at least one light-absorbing layer
- C09C1/0066—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating low and high refractive indices, wherein the first coating layer on the core surface has the low refractive index comprising at least one light-absorbing layer consisting of at least one coloured inorganic material
- C09C1/0069—Sub-stoichiometric inorganic materials
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/62—L* (lightness axis)
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/63—Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
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- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
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- C01P2006/65—Chroma (C*)
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- C01P2006/66—Hue (H*)
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/302—Thickness of a layer with high refractive material
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/30—Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle
- C09C2200/303—Thickness of a layer with low refractive material
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- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/20—PVD, CVD methods or coating in a gas-phase using a fluidized bed
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Cosmetics (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Paints Or Removers (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
本发明涉及一种片状颜料,其包括(a)一个由煅烧含有SiOz和一种金属的层而得到的层,其中0.03≤z≤2.0;该产品的制备方法;及其在油漆、纺织品、喷墨打印、化妆品、涂料组合物、塑料、打印墨水以及瓷器和玻璃的珐琅方面的用途。上述方法使片状颜料获得了高度的面平行度以及使得规定厚度在平均厚度的±10%范围内,优选±5%。
Description
本发明涉及一种片状颜料,其包括(a)一个由煅烧含有SiOz和一种金属的层而得到的层,其中0.03≤z≤2.0;该产品的制备方法;及其在油漆、纺织品、喷墨打印、化妆品、涂料组合物、塑料、打印墨水以及瓷器和玻璃的珐琅方面的用途。上述方法使片状颜料获得了高度的平面平行度以及使得规定厚度在平均厚度的±10%范围内,优选±5%。
WO93/19131公开了一种片状有色颜料,其包含二氧化钛,一种或多种钛的低价氧化物和钛以外的一种或多种金属或非金属的氧化物,其中在涂层中钛氧化物的浓度在基体表面附近最大并且向着颜料表面逐渐减少。
WO00/34395,WO00/69975和WO02/31058描述了亮金属薄片,SiOy1/Al/SiOy1,其中y1为约1至约2。铝层的厚度为至少约40nm并且SiOy1层的厚度为至少10nm。
WO03/68868描述了制备SiOy薄片的方法。可以在500-1500℃,优选500-1000℃下用含碳气体,优选排除氧气处理SiOy薄片,其中在SiOy薄片上形成SiC层。另一选择,则是在含氧空气中加热它,使SiOy薄片转化成SiO2薄片。该SiO2薄片可以用作干扰色颜料的基质。
PCT/EP03/09296公开了片状颜料,其包含由煅烧TiO2/SiO2所获得的层,其中0.03≤z≤2.0,及其在油漆、纺织品、喷墨打印、化妆品、涂料、塑料材料、打印墨水、在瓷器和玻璃的珐琅方面以及在安全打印方面的用途。
EP-A-803549公开了有色颜料,其包含(a)由基本上透明或金属的反射材料组成的内核,和(b)至少一种基本上由一种或多种硅氧化物组成的涂层,氧与硅的分子比率为0.25-0.95。
本发明涉及一种片状颜料,其颗粒大体上具有2μm-5mm的长度,2μm-2mm的宽度和20nm-1.5μm的厚度,以及长度和厚度之比至少2∶1,其包括(a)一个由煅烧含有SiOz和一种金属的层而得到的层,其中0.03≤z≤2.0。
煅烧优选于600℃以上在非氧化氛中进行。
该片状颜料的颗粒大体上具有2μm-5mm的长度,2μm-2mm的宽度和20nm-1.5μm的厚度,以及长度和厚度之比至少2∶1,优选至少6.5∶1,特别是从50∶1至500∶1。该颗粒具有两个大体上平行的面,其间的距离是内核的最短的轴。该颜料(薄片)并不是规则的形状。即便如此,为了简而言之,将该薄片称为具有“直径”。该薄片具有高的面平行度以及具有在平均厚度的±10%范围内,优选±5%内的规定厚度。该薄片具有20-2000nm的厚度,特别优选100-350nm。目前优选薄片的直径的优选范围为约1-60μm,更加优选的范围为约5-40μm。这样,本发明的薄片的长宽比的优选范围为约14-400。
片状颜料可以由以下方法制备,包括:
a)将分离剂层蒸汽沉积至载体上,
b)然后,同时将金属和SiOz蒸汽沉积在分离剂层上,其中0.03≤z≤2.0,
c)将分离剂溶解于溶剂中,
d)从溶剂中分离出产品,和
e)在非氧化气氛中煅烧产品。
进一步的,还涉及该方法所获得的片状颗粒。
新的颜料能够尤其用于汽车的面漆、工业涂料组合物、塑料、打印墨水和化妆品制剂中。
颜料颗粒优选具有5-50μm的宽度和长度,尤其是5-25μm,以及60nm-1.0μm的厚度。
SiOz其中0.03≤z≤2.0,意味着氧与硅的分子比率平均为0.03-2.0。
相应的,SiOy其中0.70≤z≤1.80,意味着氧与硅的分子比率平均为0.70-1.80。
按照本发明,术语一个包含SiOz和一种金属的层意味着一个包含SiOz基体和植入其中的金属的复合物层,但不包含SiOz和Al的清晰层的复合层状结构,如SiOz/Al/SiOz。
层(a)的金属主要可以为在燃烧步骤与SiOz反应的任何金属。优选Al、Cu、Mo、V、Ag、Cr、Zr、Nb、Ni、Fe、Co、Ti或其合金,如铬-镍、铁-镍、铁-铬和镍-钴,其中最优选铝。
按照本发明,术语“铝”包含铝和铝合金。铝合金可以举例为在G.Wassermann in Ullmanns Enzyklopdie der IndustriellenChemie,4.Auflage,Verlag Chemie,Weinheim,Band 7,S.281-292中所描述的。尤其合适的是腐蚀稳定的铝合金,其描述于WO00/12634的10-12页,除铝硅之外其包括镁、锰、铜、锌、镍、钒、铅、锑、锡、镉、铋、钛、铬和/或铁,其用量低于20重量%,优选低于10重量%。
混合层的厚度依赖所用的金属。在铝和SiOz(0.03≤z≤2.0)共升华的情况下,其中铝和SiOz的混合层形成干扰色颜料的内核,另外的金属氧化物层沉积于其上,厚度大体上为5-100nm,优选30-60nm。
优选层(a)形成颜料的内核。进一步的层可位于内核的只一个平行表面上。然而,更优选将进一步的层对称地安排在内核的周围。只由由煅烧一个含有SiOz(其中0.03≤z≤2.0)和金属(尤其是铝)的层而得到的层组成的片状结构尤其适合作干扰色颜料的基质并且形成了本发明的一个优选的实施方案(A)。
本发明进一步的主题是该颜料在喷墨打印(PCT/EP03/11189),染色的纺织品(PCT/EP03/11188),颜料涂料,打印墨水,塑料,化妆品(PCT/EP03/09296),瓷器和玻璃的珐琅以及安全打印方面的应用。
在优选的实施方案(B)中,片状颜料包括
(b1)一个SiOz层,
(a)一个由煅烧含有SiOz和一种金属,尤其是铝,的层而得到的层,和
(b2)一个SiOz层,其中0.03≤z≤2.0。
在这个实施方案中,层(a)优选形成颜料的内核,其中层(b1)和(b2)只存在于内核的平行表面上。
SiOz层的厚度依赖于所需要的颜色,但大体上是10-1000nm。大于500nm的厚度会导致无光泽的颜色。
在本发明的一个优选实施方案中,干扰色颜料包含具有“高”折射指数的材料,在此将其定义为折射指数大于约1.65,并任选含有具有“低”折射指数的材料,在此将其定义为折射指数约1.65或更低。可以利用的各种(电介质)材料包括无机材料如金属氧化物、金属低价氧化物、金属氟化物、金属氧卤化物、金属硫化物、金属硫属元素化物、金属氮化物、金属氧氮化物、金属碳化物、其结合等等,以及有机电介质材料。这些材料容易获得并且容易通过物理或化学蒸汽沉积方法,或湿化学涂覆方法来应用。
具有“高”折射指数的电介质材料的例子为硫化锌(ZnS)、氧化锌(ZnO)、氧化锆(ZrO2)、二氧化钛(TiO2)、碳、氧化铟(In2O3)、氧化铟锡(ITO)、五氧化钽(Ta2O5)、氧化铬(Cr2O3)、氧化镉(CeO2)、氧化钇(Y2O3)、氧化铕(Eu2O3)、铁氧化物如铁(II)/铁(III)氧化物(Fe3O4)和铁(III)氧化物(Fe2O3)、氮化铪(HfN)、碳化铪(HfC)、氧化铪(HfO2)、氧化镧(La2O3)、氧化镁(MgO)、氧化钕(Nd2O3)、氧化镨(Pr6O11)、氧化钐(Sm2O3)、氧化锑(Sb2O3)、单氧化硅(SiO)、氧化硒(Se2O3)、氧化锡(SnO2)、氧化钨(WO3)或其结合。电介质材料优选金属氧化物。金属氧化物很可能是单一氧化物或氧化物的混合物,带有或不带有吸收性能,例如,TiO2、ZrO2、Fe3O4、Fe2O3、Cr2O3、钛酸铁、氧化铁的水合物、氧化低价钛或ZnO,特别优选TiO2。
在具有“高”折射指数的电介质材料的层,尤其是TiO2层的顶部应用低折射指数的金属氧化物,有可能获得色彩更强和更透明的颜料。可以使用的合适的低指数电介质材料的非限制性例子包括二氧化硅(SiO2)、氧化铝(Al2O3)以及金属氟化物如氟化镁(MgF2)、氟化铝(AlF3)、氟化铈(CeF3)、氟化镧(LaF3)、氟化铝钠(例如Na3AlF6或Na5Al3F14)、氟化钕(NdF3)、氟化钐(SmF3)、氟化钡(BaF2)、氟化钙(CaF2)、氟化锂(LiF)、其结合或任意其他具有约1.65或更低的折射指数的低指数材料。例如,有机单体和聚合物可以用作低指数材料,包括二烯烃或烯烃如丙烯酸酯(如甲基丙烯酸酯),全氟烯烃聚合物,聚四氟乙烯(TEFLON),氟化乙烯丙烯聚合物(FEP),聚对亚苯基二甲基,对二甲苯,其结合,等等。另外,前述材料包含浓缩的、挥发的和交联的透明丙烯酸酯层,其可用在U.S.专利5,877,895中所描述的方法沉积,其所公开的内容在此合并作为参考。优选SiO2、Al2O3、AlOOH、B2O3或其混合物。最优选SiO2。
特别优选的基于实施方案(A)或(B)的干扰色颜料进一步优选在颜料的整个表面上包括高折射指数的金属氧化物,特别是TiO2或Fe2O3,以及任选地、另外地在高折射指数的金属氧化物层上包括低折射指数的金属氧化物,尤其是SiO2。
相应的,本发明还涉及片状颜料,其包括:
(c1)一个高折射指数的金属氧化物的层,尤其是TiO2或Fe2O3,
(b1)任选的,一个SiOz层,
(a)一个由煅烧含有SiOz和一种金属的层而得到的层,
(b2)任选的,一个SiOz层,其中0.03≤z≤2.0,和
(c2)一个高折射指数的金属氧化物的层,优选TiO2或Fe2O3。
在这个实施方案中,优选层(a)形成颜料的内核,其中优选(b1)和(b2)存在于内核的平行表面。高折射指数材料的层(c1)和(c2),特别是TiO2,可以只存在于层(c1)和(c2)上,但优选存在于颜料的整个表面上。
高折射指数的金属氧化物优选选自TiO2、ZrO2、Fe2O3、Cr2O3、Fe3O4、ZnO及这些氧化物的混合物,和钛酸铁、氧化铁水合物、氧化低价钛,和这些化合物的混合物或混合相,尤其是Fe2O3和TiO2。低折射指数金属氧化物优选选自SiO2、Al2O3、AlOOH、B2O3和其混合物,有可能的话,任选的加入碱金属氧化物或碱土金属氧化物作为附加组分。
包含由煅烧含有SiOz和一种金属,优选铝,的层而得到的层的新颜料可以获得的性能概括如下:
提高的基体性质
可精确控制均匀的基体厚度,
光滑均匀的基体表面,
不含固有颜色的透明基体,
提高的光的反射和折射,
提高的颜色强度和纯度,
新的颜色变化效果。
进一步优选的基于实施方案(A)和(B)的干扰色颜料可被涂覆一层或多层金属或金属合金,所述金属或金属合金例如选自铬、镍、银、铋、铜、锡和哈斯特洛伊镍基耐蚀耐热合金(镍基合金),或被涂覆一种金属硫化物,后者举例为,钨、钼、铈、镧或稀土金属的金属硫化物。
当进一步的层是金属或金属合金层时,内核厚度为10-1000nm,其要依赖所用金属和所需颜色,且优选低于500nm。可用湿化学方法或PVD或CVD方法应用该进一步的层。
特别优选的干扰色颜料是,基于具体方式(A)或(B)、且任选地以湿化学方法按所述顺序涂覆TiO2(内核:SiOz/Al;层:TiO2),(SnO2)TiO2,Fe2O3,Fe2O3·TiO2(内核:SiOz/Al;Fe2O3和TiO2的混合层),TiO2/Fe2O3(内核:SiOz/Al;第一层:TiO2;第二层:Fe2O3),TiO2/普鲁士蓝,TiO2/Cr2O3,TiO2/FeTiO3,TiO2/SiO2/TiO2,(SnO2)TiO2/SiO2/TiO2,TiO2/SiO2/TiO2/SiO2/TiO2或TiO2/SiO2/Fe2O3。
可以将TiO2用以下常用方法任选进行还原:US-B-4948631(NH3,750-850℃),WO93/19131(H2,>900℃)或DE-A-19843014(固态还原剂,例如硅,>600℃)。
可用CVD(化学汽相沉积,chemical vapour deposition)法或湿化学涂覆法应用金属氧化物层。可通过在水蒸气存在下分解羰基络金属获得金属氧化物层(相对低分子量的金属氧化物如磁铁矿),或在合适的情况下在氧气和水蒸气存在下进行(如氧化镍和氧化钴)。很可能涂覆操作在流化床反应器中进行(EP-A-045851和EP-A-106235),金属氧化物层尤其通过羰基络金属(如,五羰基合铁、六羰基合铬;EP-A-45851)的氧化气体相分解的方式施用,通过金属醇化物(如,钛和锆的四正-和四异-丙醇化物DE-A-41 40 900)或金属卤化物(如,四氯化钛,EP-A-338428)的水解气体相分解的方式施用,通过有机锡化合物(特别是烷基锡化合物如四丁基锡和四甲基锡,DE-A-4403678)的氧化分解的方式施用,或通过在EP-A-668329中描述的有机硅化合物(特别是二-叔-丁氧基乙酸基硅烷)的气相水解的方式施用。在铝涂覆的颜料的冷却过程中控制氧化可有益地获得Al2O3层(B),否则其需在惰性气体下进行(DE-A-19516181)。
可能合适的情况下对于需还原的金属氧化物来说,优选以湿化学法析出的方式应用金属锆、钛、铁和锌的氧化物、这些金属的氧化物水合物、钛酸铁、氧化低价钛或其混合物的层。在湿化学涂覆的情况下,可以使用为制备珠光颜料而发展的湿化学涂覆方法,其被描述在例如DE-A-1467468,DE-A1959988,DE-A-2009566,DE-A-2214545,DE-A-2215191,DE-A-2244298,DE-A-2313331,DE-A-2522572,DE-A-3137808,DE-A-3137809,DE-A-3151343,DE-A-3151354,DE-A-3151355,DE-A-3211602和DE-A-3235017,DE1959988,WO93/08237,WO98/53001和WO03/6558中。
高折射指数的金属氧化物优选TiO2,低折射指数的金属氧化物优选SiO2。TiO2层可以为金红石型或锐钛矿型的,其中优选金红石型的。也可用已知方式还原TiO2层,例如氨、氢、烃蒸汽或其混合物、或金属粉末,其描述于EP-A-735114,DE-A-3433657,DE-A-4125134,EP-A-332071,EP-A-707050或WO93/19131中。
为了进行涂覆,将基体颗粒分散于水或HCl中,在适合水解的pH值下向其中加入一种或多种可水解的金属盐,选择这样的pH值以使金属氧化物或金属氧化物的水合物直接沉淀到这些颗粒上,而不会发生二次沉淀。通过同时计量加入一种碱,pH值可以保持恒定。然后将颜料分离、洗涤和干燥,以及任选地煅烧,对于特别的涂层将煅烧温度最优化是可能的。如果需要,在应用每个涂层之后,在为了沉积另外一些层而进行再次分散之前,可以将颜料分离、干燥以及选择地煅烧。此外,涂覆还可以气相涂覆的方式在流化床反应器中进行,对此,例如,可以相应地使用公开于EP-A-0045851和EP-A-0106235中的生产珠光颜料的方法。
在复合层颜料的情况下,可以通过扩大特定波长的方式确定干扰色,当在复合层颜料中许多层具有相同的光学厚度时,层的数目越大则反射光的颜色变得更强更加饱和。此外,通过适当的选择层厚,可以获得依靠视角而产生的特别大的颜色变化。形成明显的颜色下落,这是本发明的颜料所需的。因此,不管其折射指数,单独的金属氧化物层的厚度为20-500nm,优选50-300nm。
对于二氧化钛层的应用,优先考虑在US-B-3553001中描述的方法。
将钛盐水溶液缓慢地加入被涂覆材料的悬浮液中,该悬浮液已经被加热至约50-100℃,优选70-80℃,以及并具有基本上恒定的pH值约0.5-5,优选约1.5-2.5,其通过同时计量加入一种碱,例如氨水溶液或碱金属氢氧化物水溶液而维持。一旦沉积的TiO2达到了所需层厚,即可以停止钛盐溶液和碱的添加。该方法也称为滴定法,其以避免钛盐过量为特征。这是靠针对水解如下投料而获得的,即在每单位时间内,投料量只是用水合TiO2均匀涂覆所必须的量,以及在每单位时间内可以覆盖被涂覆颗粒有效表面的量。相应的,水合二氧化钛颗粒并没有在被涂覆表面形成并沉积。用该方法获得了TiO2的锐钛矿形式。在沉积TiO2层之前沉积SnO2层并在约700-900℃燃烧该颜料则可以获得TiO2的金红石形式。在0-60℃的温度下用盐酸进行TiCl4水解的方法,也有可能沉淀具备1-50nm粒径的金红石形纳米TiO2(Lit:R.J.Nussbaumer,W.Caseri,T.Tervoort和P.Smith,Journal ofManoparticle Research 2002,4,319-323;Anpo等J.Phys.Chem.1987,91,4305)。在0-50℃的温度下用水进行的Ti(Oipr)4(四异丙醇钛)的水解以及接下来在50-100℃以及轻度真空(p约200torr)条件下分离所得到的异丙醇,同样可能沉淀具有10-40nm粒径(晶粒<10nm)的锐钛矿形纳米TiO2(Lit:K.l.Gnanasekar等,Journal ofMaterials Research 2002,17(6),1507-1512)。同样很可能将用氢氧化铵水解和接下来用H2O2氧化TiCl4所制备的钛酸溶液添加至Al/SiOz薄片的水溶液中,在100-250℃加热的情况下,会从该溶液中自发形成具有约10nm粒径的锐钛矿形纳米TiO2颗粒(Lit:H.Ichinose,M.Terasaki和H.Katsuki,Journal of the CeramicSociety of Japan,Int.Edition 1996,104(8),715-718)。这种溶液和分散体现在已经成为商业上可以获得的(Kon Corporation,91-115Miyano Yamauchi,Kishimagun Saga-prefecture,Japan 849-2305)。涂覆了钛、锆或铁的Al/SiOz薄片接下来可用已知的方法涂覆有机或无机的化合物。
对于二氧化硅层的实施,可以使用下述方法:将苏打水玻璃溶液计量加入被涂覆材料的悬浮液中,该悬浮液已经被加热至50-100℃,尤其是70-80℃。
通过同步添加10%的盐酸溶液,pH值于4-10,优选6.5-8.5保持恒定。在添加水玻璃溶液之后,再进行30分钟的搅拌。
为了加强复合层薄片的耐候和耐光稳定性,依据应用的领域,可以对其进行表面处理。有用的表面处理方法可以举例为,在DE-C-2215191,DE-A-3151354,DE-A-3235017,DE-A-3334598,DE-A-4030727,EP-A-649886,WO97/29059,WO99/57204和US-A-5759255中所描述的方法。所述表面处理还可以使颜料处理变得容易,特别是易于使其引入各种各样的应用介质。
进一步的,基于实施方案(A)或(B)的干扰色颜料可以在一个平行面上,优选在两个平行面上,具有薄的半透明金属层。该金属层典型的是5-25nm厚,尤其是5-15nm厚,并且由例如Cr,Ti,Mo,W,Al,Cu,Ag,Au或Ni组成。
半透明金属层可以由PVD法施用。另一选择,由湿化学涂覆法或化学蒸汽沉积法获得金属层,例如金属羰基化合物的气相沉积法。在金属化合物存在的情况下,将基体分散于含有介质的含水的和/或有机溶剂中,并通过添加还原剂将其沉积在基体上。例如,该金属化合物为硝酸银和乙酰丙酮镍(WO03/37993)。
按照US-B-3536520,氯化镍可用作金属化合物,次磷酸盐可用作还原剂。按照EP-A-353544,在湿化学涂覆法中以下化合物可以用作还原剂:醛(甲醛、乙醛、亚苄基醛),酮(丙酮),羧酸及其盐(酒石酸、抗坏血酸),还原酮(异抗坏血酸、丙糖还原酮、还原酸)和还原糖(葡萄糖)。
颜料的煅烧包括颜料在非氧化气氛中,如果合适的话在含氧空气中,煅烧颜料。在非氧化气体的气氛中,例如Ar和/或He煅烧颜料,是在超过600℃,优选700-1100℃的温度下进行超过10分钟,优选几个小时,合适的话在减压下,优选低于0.9333105N/m2(700torr)下进行。可以在用高折射指数金属氧化物涂覆之后进行煅烧,但优选在用高折射指数金属氧化物涂覆之前进行煅烧。
通过仅仅改变两个工艺参数:金属和SiOz混合层的真空涂层的厚度,和混合层中植入的金属的百分比,层状材料就可以以可变和可重现的变体的多重态方式生产。
用蒸汽沉积法施用混合层和分离剂层,通过在真空中同步汽化的方式将金属与SiOz混合。金属,尤其是铝,与SiOz的比率大体上低于60重量%,优选低于或等于50重量%。当将Al和SiOz同时汽化时,优先用煅烧的方式将所有的铝转化为Al3+:
假设在非氧化空气中煅烧金属/SiOz可以获得复合层,因此会产生折射指数的变化。假设,折射指数的变化是基于金属被SiOz氧化。例如,已知在650℃加热SiO和铝可以形成Si和Al2O3,在900℃加热SiO和钛可以形成硅化钛(New J.Chem.,2001,25,994-998)。
当由蒸汽喷发重叠以至于混合层在重叠区域生产的两个汽化器生产混合层时,该生产尤其简单。作为备选方案,还可以通过单汽化器进行汽化,该汽化器同时或交替地汽化两个组分。
用在1-10-3Pa的压力下加热和汽化要在真空中被汽化的物质的真空沉积法制备材料。蒸汽凝结在冷的基质表面以形成所需的薄层。汽化可以在通过电流通过而直接加热的金属容器(钨皿,钼或钽盘)中进行,或靠电子束轰击进行。
在溅射法或阴极雾化的情况下,在载体和涂覆材料之间引发气体放电(等离子体),涂覆材料呈盘的形式(目标)。用来自等离子体的高能离子,例如氩离子,轰击涂覆材料,结果其被移下并雾化。雾化的涂覆材料的原子或分子沉积于载体上并形成所需薄层。
金属或合金尤其适于溅射法。尤其在所谓的DC磁控管法中,它们可以被高速雾化。诸如氧化物或低价氧化物或氧化物的混合物的化合物还可以用高频溅射雾化。层的化学组成由涂覆材料(目标)的组成控制,但还是会被向形成等离子的气体进行添加的影响。特别是,由向气体空间中加入氧或氮制备氧化物或亚硝酸盐层(参见,例如,US-A-5 440 446和EP-A-0 733 919)。
优选使用耐热汽化器、电子束加热的汽化器、感应加热的汽化器或电弧操控的汽化器。
为了简化操作,载体材料应具有光滑或结构化(structured)的表面。已经发现,聚酰亚胺膜或金属箔片或其结合是尤其合适的载体材料。优选载体材料为循环带的形式,其描述于US-B-6270840中,这样使材料的连续生产成为可能。
冷凝在载体上的分离剂可以为涂层,聚合物如在US-B-6398999中描述的(热塑性)聚合物,例如丙烯酸或苯乙烯聚合物或其混合物,溶于有机溶剂或水并在真空中汽化的有机物,如蒽、蒽醌、乙酰氨基苯酚、乙酰水杨酸、樟脑酸酐、苯并咪唑、苯-1,2,4-三羧酸,联苯-2,2-二羧酸,二(4-羟苯基)砜,二羟基蒽醌,乙内酰脲,3-羟基苯甲酸,8-羟基喹啉-5-磺酸一水合物,4-羟基香豆素,7-羟基香豆素,3-羟基萘-2-羧酸,间苯二甲酸,4,4-亚甲基-二-3-羟基萘-2-羧酸,萘-1,8-二羧酸酐,邻苯二甲酰亚胺及其钾盐,酚酞,吩噻嗪,糖精及其盐,四苯基甲烷,苯并菲,三苯基甲醇或其中至少两种的混合物。分离剂优选能在真空汽化的水溶性无机盐(参见,例如,DE19844357),例如氯化钠、氯化钾、氯化锂、氟化钠、氟化钾、氟化锂、氟化钙、氟化钠铝或四硼酸二钠。
本发明优选的实施例将在以下更清楚的描述。
在按照本发明方法的优选实施例中,通过按照PVD法的热力学汽化,在真空中逐一施用以下层,优选在1-10-3Pa的压力下:
分离剂层,和
混合层,置于分离剂层的顶部,该层含有金属和可自由选择比例的SiOz,其通过异源或同源的同步汽化引入。
按照本发明的方法,原则上,可能使用任何在煅烧过程中能与混合层中所存在的SiOz反应的无机金属。优选镍、铁、钴、银、铬、锆、铌、钼、钒、钛或其合金,例如铬-镍、铁-镍、铁-铬和镍-钴;特别优选使用铝。合金的汽化可从具备所需的摩尔比的分开的源有利地进行。
本发明的一个特别优选的实施方案在于SiOy/Al薄片的制备,其中0.70≤y≤1.8优选1.0≤y≤1.8。
具体的说,将一种盐,例如NaCl,随后是硅的低价氧化物和铝的层蒸汽沉积在一个载体上,其可以是一个连续的金属带,在<0.5Pa的真空下通过汽化器。通过两个汽化器获得硅的低价氧化物(SiOy)和铝的混和层,每一个汽化器装有两种材料之一,并且两个汽化器的汽化圆锥区域重叠,金属以占混和层1-50%的比率混合。分离剂(尤其是盐)的蒸汽沉积厚度约20-100nm,优选30-60nm,而取决于该产品的用途,混和层的蒸汽沉积厚度为10-1000nm。进一步的进程,形成一个环路的带形载体通过由已知方式(参见US-B-6270840)构造的动态真空锁室,进入一个1-5×104Pa压力、优选600-109压力、更优选103-5×103压力的区域,在这儿浸入一个溶解槽。选择此处的溶剂温度使得其蒸汽压应在指示压力的范围内。在机械协助下,分离剂层迅速溶解,产品层碎裂成薄片,然后其以悬浮体的方式存在于溶剂中。在优选的实施方案中,NaCl用作分离剂层的分离剂,该NaCl溶于水中。在接下来的进程中,将该带干燥并脱除任何仍然粘附于其上的污染物。它运行通过第二组动态真空锁室,进入汽化室,在这重复进行分离剂和SiOy/分离剂的混和层的涂覆过程。
然后将包含溶于其中的产品结构、溶剂和分离剂的悬浮液根据已知技术在接下来的操作中分离。为了这个目的,将产品结构首先浓缩至液体中,并用新鲜溶剂漂洗数次以洗去溶解的分离剂。以固态形式的产品仍旧是湿的,将其通过过滤、沉淀、离心过滤、倾析或蒸发来分离。
按照另一个优选的具体实施例,通过按照PVD方法的热力学气化,在真空中,优选在1-10-3Pa的压力下逐一施用如下各层:
分离剂层,
在分离剂层上面的SiOy层,
混和层,置于SiOy层之上,该层包含铝与可自由选择百分比的SiOz,该SiOz由从异源或同源的同步汽化所引入,和
在混和层上面的SiOy层。
优选由Si和SiO2的混合物在大于1300℃的温度下在汽化器中反应生产的单氧化硅形成SiO1.00-1.8层。优选在大于1300℃的温度下蒸发含有最高达20重量%的硅的单氧化硅形成SiO0.70-0.99层。
如果在几个10-2Pa的工业真空下,硅取代SiO被汽化,刚获得小于等摩尔数的氧含量的氧化硅,这也就是说,在SiOx中,0.03≤x≤0.95,优选0.05≤x≤0.5。
在这个实施方案中每一个SiOy层的厚度从10-1000nm不等。可按照所需颜色来优选厚度。大于约500nm的SiOy层厚会导致无光泽的颜色。
本发明进一步优选的主题包括按照上面所述方法获得的颗粒,其具有如下层结构:SiOy/(SiOy和铝的混和层=内核)/SiOy,其可以在非氧化气氛中燃烧。这些薄片的煅烧是在保护气体,例如氦或氩,的气氛下,适合的话在减压(<0.93 105Pa)下,在大于600℃,优选700-1100℃的温度下进行大于10分钟,优选大于2小时。
煅烧之后,将该产品进行氧化热处理。为达到该目的,可使用已知方法。在大于200℃,优选大于400℃,特别优选500-1000℃的温度下,将空气或其它含氧气体通过平行面结构,该结构是松散材料的形式或是流化床的形式。然后可用如下方式使得产品达到所需颗粒尺寸,通过超声处理或在液体介质中使用高速搅拌机的机械法,或在具有螺旋式分粒器的空气喷射磨中干燥碎片之后,研磨或空气筛分法,然后将其传送至进一步的使用。
对于涂覆了SiOy的薄片的进一步操作,不同的变体都是合理的。
变体(1)(TiO2/SiOz/内核’/SiOz/TiO2,其中内核’是煅烧由SiOy和铝组成的层而得到的层):
在高于600℃的温度下,优选700-1100℃的温度下,将SiOy涂覆的片(SiOy/(SiOy和Al的混和层=内核)/SiOy)在非氧化气氛中煅烧超过10分钟,优选几个小时。任选地在降低的压强下,优选在低于700Torr(0.9333 105N/m2)的压强下,煅烧在非氧化气氛中进行,如Ar和/或He,其中优选Ar。
将所得片进行氧化热处理。例如,在大于200℃,优选大于400℃,特别优选500-1000℃的温度下,将氧气或其它含氧气体通过片,该片是松散材料的形式或是流化床的形式,其中将SiOy氧化为SiOz。
用物理或化学蒸汽沉积法或湿化学涂覆法,可简单地将TiO2涂层施用到SiOy涂覆的金属片上。
为了涂覆的目的,将基体颗粒分散于水中,并在适于水解的pH值将一种或多种可水解钛盐加入,pH值的选择使得金属氧化物或金属氧化物水合物直接沉淀颗粒上而不会发生二次沉淀。通过同时计量加入一种碱,pH通常保持恒定。然后将颜料分离,洗涤,干燥且如果需要的话,煅烧,可以针对目标涂层优化煅烧温度。如果需要,在施用每个涂层后,将颜料分离,干燥且如果需要的话,煅烧,然后为了沉积接下来的层将其再次分散。
按照本发明的具体方式,可使用在US-B-3553001中描述的方法施用TiO2层。
将钛盐水溶液慢慢地加入被涂覆材料的分散液中,该分散液已经被加热至约50-100℃,优选70-80℃,并通过同时计量加入一种碱,例如氨水溶液或碱金属氢氧化物水溶液,保持基本上恒定的约0.5-5的pH值,尤其是约1.2-2.5的pH值。一旦沉淀的TiO2达到了所需层厚,则停止添加钛盐和碱。
该方法也称为滴定法,其以避免钛盐过量为特征。这是靠针对水解如下投料而获得的,即在每单位时间内,投料量只是用水合TiO2均匀涂覆所必须的量,以及在每单位时间内可以覆盖被涂覆颗粒有效表面的量。大体上,在初始颜料的表面上形成了TiO2的锐钛矿形式。然而,通过添加少量的SnO2,很可能促使形成金红石结构。例如,如在WO93/08237中所描述的,二氧化锡可在二氧化钛之前沉积,并且涂覆着二氧化钛的产品可以在800-900℃煅烧。
通过附加涂层有可能提高其耐候性,同时,可导致其对于结合体系的最佳适应(EP-A-268918和EP-A-632109)。
变体(2)(TiO2/层(E)/内核’/SiOz/层(E)/TiO2:
如上所述,SiOz涂覆的片(SiOy/(SiOy和Al的混和层=内核)/SiOy)用TiO2涂覆,然后在非氧化气氛中煅烧。用这种方式,在层(a)之外制备附加层(E),该层由TiO2/SiOz的煅烧形成。假设在非氧化气氛中煅烧TiO2/SiOz生产的中间层导致了折射指数的变化。然而,很可能中间层并不是连续的层,并且不能排除,在TiO2和SiOz界面处只有部分区域经历了导致折射指数变化的转化。进一步假设,折射指数的变化是由于SiOy将TiO2还原。
因此,本发明的原理是基于通过SiOy还原TiO2而产生导致折射指数变化的中间层。
相应的,本发明进一步优选的技术方案涉及具有以下层结构的颜料,TiO2/SiOz/内核/SiOz/TiO2,其中SiOz层只存在于平行面表面上,而不是侧面,TiO2施加于整个表面;还涉及具备以下层结构的颜料,TiO2/层(E)/SiOz/内核/SiOz/层(E)/TiO2,其中SiOz层和层(E)只存在于平行面表面上,而不是侧面,TiO2施加于整个表面。
二者择一地,颜料可用以下方法获得:
变体(3):在非氧化气氛下煅烧(→层(a)),用TiO2涂覆所得颜料(TiO2/SiOy/内核’/SiOy/TiO2),并且任选地在氧气存在下煅烧(SiOy→SiOz)(TiO2/SiOz/内核’/SiOz/TiO2)。
变体(4):在非氧化气氛下煅烧(→层(a)),用TiO2涂覆所得颜料(TiO2/SiOy/内核’/SiOy/TiO2),在非氧化气氛下煅烧(→层(E))(TiO2/层(E)/SiOy/内核’/SiOy/层(E)/TiO2),并且任选地在氧气存在下煅烧(SiOy→SiOz)(TiO2/层(E)/SiOz/内核’/SiOz/层(E)/TiO2)。
如果需要可用常规方法将TiO2还原为钛的低价氧化物,例如在US-A-4948 631,JP H4-20031,DE-A-19618562和DE-A-198 43 014中所描述的。
在TiO2层的上面施加“低”折射指数,也就是说折射指数小于约1.65的金属氧化物,如SiO2,Al2O3,AlOOH,B2O3或其混合物,优选SiO2,并且在该金属氧化物层上进一步施加Fe2O3和/或TiO2层,就可能获得颜色更强烈以及更透明的颜料。这样的多层涂覆的干扰色颜料包括硅氧化物基层和任选的高和低折射指数的金属氧化物层,其可用类似于WO98/53011和WO99/20695中所描述的方法制备。
合适的情况下,可将SiO2(保护)层施加于二氧化钛层的上面,其可使用以下方法:将苏打水玻璃溶液计量加入被涂覆材料的分散液中,该分散液已被加热至约50-100℃,优选70-80℃。通过同步添加10%的盐酸,将pH维持在4-10,优选6.5-8.5。添加水玻璃溶液之后,进行搅拌30分钟。
此外,通过施加进一步的层,如有色金属氧化物或柏林蓝,过渡金属如Fe,Cu,Ni,Co,Cr的化合物或有机化合物如染色或色淀,就可能改善颜料的粉末颜色。
此外,还可能将成品颜料进行随后的涂覆或后处理,其进一步提高耐光、耐候和耐化学稳定性,或者,其使颜料容易处理,尤其是易于将其引入不同的介质中。例如,在DE-A-22 15 191,DE-A-31 51 354,DE-A-32 35 017,DE-A-3334598,DE-A-4030727,EP-A-649886,WO97/29059,WO99/57204和US-A-5759255中所描述的步骤适用作后处理或后涂覆。
此外,按照本发明的颜料可用难溶、牢固黏附、无机或有机着色剂涂覆。优选使用色淀,尤其是铝色淀。为此目的,沉淀氢氧化铝层,在第二步使用色淀对其进行装饰(DE-A-24 29762和DE 29 28 287)。
此外,按照本发明的颜料还可具有带复合盐颜料的附加涂层,复合盐尤其指青色高铁酸盐复合物(EP-A-141 173和DE-A-23 13332)。
如在变体(1)中所描述的,将SiOy涂覆的片(SiOy/(SiOy和铝的混合层=内核)/SiOy),于高于600℃,优选在700-1100℃的温度下,在非氧化气氛下已经煅烧超过10分钟,优选几小时之后,还可将其引至可最高加热至约1500℃的气密反应器中,优选为松散材料的形式,于500-1500℃,优选500-1000℃,有利地在排除氧气的情况下,与选自炔烃例如乙炔,烯烃例如甲烷、烯烃、芳香族化合物等等、及其混合物的含碳气体反应,其任选地与含氧化合物混合,如醛、酮、水、一氧化碳、二氧化碳等等,或其混合物。为了调解该反应,可将含碳气体与惰性气体,例如氩或氦混合(WO03/68868)。
在低于1Pa的压力下,反应通常进行得太慢,但是,尤其是当含碳气体反应活性减少或被惰性气体高度稀释时,完全可能在等于4000bar的压力下操作,如例如在HIP(等热压制)体系中同常规使用的。
在这样的碳化中,所有SiOy都有可能反应以形成SiC,优选5-90重量%的SiOy反应形成SiC。SiOy向SiC转化过程的温度为500-1500℃,优选500-1000℃,过程持续时间为约1小时至约20小时。反应从平面结构的表面开始进行,相应地导致梯度变化而不是急剧跃迁。这意味着,在该实施方案中,含SiC层由(SiOy)a和(SiC)b组成,其中0≤a<1,0<b≤1,b为1和a为0时接近于颜料表面,接近于0的SiC的量接近于SiOy基体的边界。对于该反应来说,SiOy的结构足够多孔,使该反应不会只局限于最上层的SiOy分子。
按照该方法,可以获得具有下述层结构的各种颜料,SiC/SiOy/内核’/SiOy/SiC,通过在氧存在下的煅烧,可将其转化为具有下述层结构的颜料,SiC/SiOz/内核’/SiOz/SiC。通过这种方法所获得的颜料是新的,并且是本发明的进一步的主题。
除了具有高折射指数的金属氧化物层,US-B-6524381材料,如钻石状碳和无定形碳,可通过等离子体辅助真空法(使用振动传输机,转鼓涂料器,振动转筒涂料器和自由落体室)将其沉积在SiOz涂覆的基体表面上,如例如在US-B-6524381中所描述的。
所以,本发明还涉及基于SiOz/内核’/SiOz基体的平行面结构(颜料),在其表面上具有碳层,尤其是具有厚度5-150nm,尤其是20-50nm的钻石状碳层。
在例如US-B-6015597所描述的方法中,用等离子体沉积法,将钻石状网络结构(DLN)涂层从含碳气体,如乙炔、甲烷、丁二烯及其混合物和任选的氩,和含有附加组分的任选的气体中沉积于颗粒上。沉积在减压(相对于大气压)和可控的环境下进行。在反应室中,通过对含碳气体施加电场而形成了富碳等离子体。在反应器中将即将被涂覆的颗粒束缚在导管或容器中,并当接近等离子体时进行搅拌。等离子体内的物质在颗粒表面反应以形成共价键,造成在颗粒表面的DLN。
术语“钻石状网络结构”(DLN)是指含有碳并任选含有一个或两个选自氢、氮、氧、氟、硅、硫、钛和铜的附加成分的多孔膜或包衣。钻石状网络结构包含约30-100原子百分数的碳,任选的附加组分补上余下的量。
例如,可将片状的Al/SiOz颗粒用作效颗颜料的基体。可能按照常用方法施加进一步的对干扰效果所必需的层,常用方法已经在此前做过详细的描述,对于包括云母、SiO2或Al2O3内核的效果颜料是已知的。
按照本发明的颜料因高光泽和非常均匀的厚度而区别于其它的,其结果是获得高色彩纯度和色彩强度。按照本发明的颜料可用于各种特定的用途,例如染色纺织品、块状聚合物,涂料(包括效果面漆,包括那些用于汽车界的)、瓷器或玻璃的珐琅和打印墨水(包括安全打印),还有例如在化妆品和喷墨打印方面的应用。该应用在引用文献中是已知的,例如“Industrielle Organische Pigmente”(W.Herbst and K.Hunger,VCH Verlagsgesellschaft mbH,Weinheim/New York,2nd,completely revised edition,1995)。
金属的或非金属的、无机片状颗粒或颜料是效果颜料(尤其是金属效果颜料或干扰色颜料),也就是说,除了赋予应用介质颜色,颜料还赋予了附加的性质,例如,颜色的角度依赖(平视色,flop)、光泽(不是表面光泽)或纹理。对于金属效果颜料,在直接导向的颜料颗粒上会发生大致导向的反射。在干扰色颜料的情况下,赋予颜色的效果要归功于光线在薄的、高折射层的干涉现象。
当按照本发明的颜料为干扰色颜料(效果颜料),他们是因角度变色的(goniochromatic),并能产生极度明亮的、高度饱和的(有光泽的)颜色。他们相应的非常适于与传统的透明颜料联合使用,例如有机颜料如二酮基吡咯并吡咯、喹吖啶酮、二噁嗪类、苝、异吲哚啉酮等,对于透明颜料很可能与效果颜料具有相似的颜色。然而,类似于例如EP 388932和EP402 943,当透明颜料的颜色与效果颜料的颜色互补时,获得了尤其有趣的联合效果。
将按照本发明的颜料用于着色高分子量有机材料会具有优异的效果。
使用按照本发明的颜料或颜料组合物着色的高分子量有机材料可以是天然的或人工合成的。高分子量有机材料通常具有约103-108g/mol或更多的分子量。它们可以是,例如天然树脂、干燥油、橡胶或酪蛋白,或其衍生的天然物质,如氯化橡胶、油改性的醇酸树脂、粘胶、纤维素醚或酯,如乙基纤维素、乙酸纤维素、丙酸纤维素、乙酰丁酸纤维素或硝化纤维,但是优选全部合成的有机聚合物(热固性塑料或热塑性物质),其由聚合、缩聚或加成聚合获得。从这些聚合树脂的种类中可能提及一些化合物,特别是聚烯烃,比如聚乙烯、聚丙烯或聚异丁烯,以及取代聚烯烃,比如氯乙烯、乙酸乙烯酯、苯乙烯、丙烯腈、丙烯酸酯,甲基丙烯酸酯或丁二烯的聚合产物,以及前面提到单体的共聚合产物,特别是ABS或EVA。
从这些加聚反应树脂和缩聚反应树脂系列中,还可提及比如被称为酚醛塑料的甲醛和酚类的缩聚产物,以及被称为氨基塑料的甲醛与尿素、硫脲或三聚氰胺的缩聚产物,还有被当作涂料树脂使用聚酯,饱和的比如醇酸树脂,或不饱和的像顺丁烯二酸树脂,还有线性的聚酯和聚酰胺、聚氨酯或硅氧烷。
前面提到的高分子量化合物可以单独存在,或以塑料固体或熔融物形式以混合物存在。它们也可能是单体形式或溶解的聚合物形式,作为涂料或印刷墨水的成膜物或粘合剂,比如,熟亚麻子油、硝化纤维,醇酸树脂,三聚氰胺树脂,以及脲醛树脂或丙烯酸类树脂。
根据预期用途,使用本发明的颜料或颜料组合物作为调色剂或制剂形式已被证明是有利的。
根据老化(conditioning)方法或预期应用,在老化过程之前或之后,往颜料中加入一定量的质地改良剂,如果这样的操作对效果颜料用于高分子有机材料特别是聚乙烯的着色没有副作用的话,那操作就是有利的。合适的质地改良剂包括,特别是,至少含有18个碳原子的脂肪酸,比如硬脂酸或二十二烷酸,或它们的酰胺或金属盐特别是镁盐,以及增塑剂、蜡、树脂酸,比如松香酸,松香皂,烷基酚或脂肪族醇,比如硬脂醇,或包含8到22个碳原子的1,2-二羟基化合物,比如1,2-十二烷基二醇,以及改性的松香顺-丁烯二酸酯树脂或反-丁烯二酸松香树脂。质地改良剂适宜的加入量为基于最终产品重量的0.1-30%,特别是2-15%。
依照本发明的颜料能以任意的着色有效量加入到被染色的高分子有机材料中。包含高分子有机材料,和基于这种高分子有机材料为0.01到80重量%,优选为0.1到30重量%的本发明颜料的着色物质组合物是有利的。在实践中常用的浓度为1-20重量%,特别是约10重量%。
高浓度,例如那些超过30重量%的具有格外低粘度的本发明的颜料在特定制剂中为浓缩物(“母炼胶(masterbatche)”)的形式,以便仍保持可加工性,其可用作生产具有相对低颜料含量的着色材料所用的着色剂。
为了着色有机材料,基于本发明的颜料可以单独使用。然而,为了尽可能达到不同的色调或颜色效果,除加入基于本发明的效果颜料外,加入任意需要量的其它着色组分比如白色、彩色、黑色或效果颜料到高分子有机材料中也是可行的。当有色颜料与基于本发明的效果颜料一起混合使用时,总量适宜为高分子有机材料重量的0.1到10重量%。通过基于本发明的效果颜料和具有另一种颜色特别是互补色的着色颜料的优选结合而能提供特别高的因角变色差值(goniochromicity),使用上述效果颜料和使用上述着色颜料着色,则在10°测量角下,其色彩差别(ΔH*)为20-340,特别150-210。
优选,按照本发明的效果颜料与透明有色颜料结合,很可能透明有色颜料存在于与本发明的颜料相同的介质中,或存在于相邻的介质中。多层效果涂层是上述效果颜料与有色颜料有利的存在于相邻介质中的一个例子。
用基于本发明的颜料实施对高分子有机基体的着色。比如,通过轧制机或混炼或研磨设备,将该颜料,合适的话以母炼胶的形式与这种基体混合。然后将被着色的材料通过已知方法加工成所需要的最终形式,比如混炼、压模、挤出、涂覆、浇铸或注射成型。在加入颜料之前或之后,塑料工业中所有的常用添加剂,比如增塑剂、填料、稳定剂,都可以以其通常的用量加入到聚合物中。特别的,为了生产非刚性的成型制品,或降低它们的脆性,希望在成型之前向高分子化合物中加入增塑剂,比如磷酸、苯二甲酸或癸二酸的酯。
对于有色涂料和打印墨水,将高分子量有机材料和按照本发明的颜料,适当的情况下与常规试剂如填料、其他颜料、干燥剂或增塑剂一起精细地分散或溶解于同一种有机溶剂或溶剂混合物中,对于将被单独溶解或分散的单独组分或者对于将被一起溶解或分散的一定数量的组分,并且之后对于所有将合并在一起组分,这是可能的。
将基于本发明的颜料分散到要被染色的高分子有机材料中,以及加工基于本发明的颜料组合物的过程,适宜在相对较弱的剪切力条件下实施,这样这些效果颜料不会被分散成更小的部分。
所得的着色,比如在塑料、涂料或打印墨水中,优选是在涂料或打印墨水中,更优选在涂料中,是以极好的性质,特别是极高的饱和度、杰出的不褪色性和高的因角变色差值为特征的。
当被着色的高分子材料是一种涂料时,它尤其是一种特殊涂料,特别是汽车面漆。
基于本发明的颜料也适于嘴唇或皮肤的化妆以及头发或指甲染色。
本发明相应地涉及化妆品制剂或配方,其含有0.0001-90重量%的硅或氧化硅薄片和/或基于本发明的颜料,以及基于化妆品制剂或配方总重量为10-99.9999%的适合化妆品用的载体材料。
这样的化妆品制剂或配方比如口红、胭脂、粉底、指甲油和洗发剂。
这些颜料可以单独使用或以混合物的形式使用。另外,可以将基于本发明的颜料与其它颜料和/或着色剂一起使用,比如在前文描述过的组合或如化妆品制剂中已知的。
这些基于本发明的化妆品制剂和配方适宜含有占制剂总重量为0.005-50重量%的基于本发明的颜料。
用于基于本发明的化妆品制剂和配方的合适的载体材料包括用于此类组合物的常用材料。
基于本发明的化妆品制剂和配方可以有多种形式,比如条状、软膏、霜、乳液、悬浮液、分散液、粉末或溶液形式。它们可以是例如口红、睫毛膏制剂、胭脂、眼影、粉底、眼线膏、粉或指甲油。
如果该制剂是条状的形式,例如唇膏、眼影、胭脂或粉底,则该制剂包含了相当一部分脂肪组分,其可以包含一种或多种蜡,例如地蜡、羊毛脂、羊毛脂醇、氢化羊毛脂、乙酰化羊毛脂、羊毛脂蜡、蜂蜡、小烛树蜡、微晶蜡、巴西棕榈蜡、鲸蜡基醇、硬脂酰基醇、可可脂、羊毛脂脂肪酸、矿脂、石油冻、在25℃时为固态的单、双或三甘油酯或脂肪酯、硅氧烷蜡例如甲基十八烷氧化聚硅氧烷、聚(二甲基甲硅烷氧基)硬脂氧基聚硅氧烷、硬脂酸单乙醇胺、松香及其衍生物例如乙二醇松香酸酯、甘油松香酸酯、在25℃时为固态的氢化油、糖的甘油酯和钙、镁、锆和铝的油酸盐、肉豆蔻酸盐(myristates)、lanolates、硬脂酸盐和二羟基硬脂酸盐。
脂肪组分还可以包括至少一种蜡和至少一种油的混合物,在这种情况下,例如下面的油是合适的:石蜡油、purcelline油、全氢化角鲨烯、甜杏仁油、鳄梨油、胡桐油、蓖麻油、芝麻油、霍霍巴油、具有约310-410℃的沸点的矿物油、硅油例如二甲基聚硅氧烷、亚油(linoleyl)醇、linoleyl醇、油醇、谷粒油如小麦胚芽油、异丙基lanolate、异丙基十六烷酸酯、豆蔻酸异丙酯,豆蔻酸丁酯、鲸蜡基豆蔻酸酯、鲸蜡基硬脂酸酯、丁基硬脂酸酯、癸基油酸酯、乙酰基甘油酯、醇和多元醇例如乙二醇和甘油的辛酸酯和癸酸酯、醇和多元醇例如鲸蜡基醇、异硬脂基醇、异鲸蜡基lanolate、己二酸异丙酯、己基月桂酸酯和辛基十二烷醇的蓖麻酸酯。
在这种条状形式的制剂中,脂肪组分大体上构成制剂总重的99.91重量%。
按照本发明的化妆品的制剂和配方可附加地包含进一步的组分,例如,二醇、聚乙二醇、聚丙二醇、单烷醇酰胺、无色的聚合的、无机的或有机的填料、防腐剂、UV过滤剂或其它助剂和用于化妆品的常规助剂,例如天然的或合成的或半合成的二或三甘油酯、矿物油、硅油、蜡、脂肪醇、Guerbet醇或其酯、亲油的功能性化妆品活性成分,其包括防晒过滤剂,或这些物质的混合物。
适于皮肤化妆用的亲油的功能性化妆品活性成分、活性成分组合物或活性成分提取物是被允许皮肤或局部应用的一种成分或该成分的组合物。在下面将用举例的方式陈述。
具有对皮肤表面和头发净化作用的活性成分;这包含所有能清洁肌肤的物质,如油、肥皂、合成洗涤剂和固态物质;
具有去臭和抑汗作用的活性成分:它们包括基于铝盐或锌盐的止汗药,包含杀菌或抑菌去臭物质的除臭剂,例如三氯生、六氯酚、醇或阳离子物质,例如,季铵盐,和吸味剂,例如®Grillocin(蓖麻酸锌和不同添加剂的混合物)或柠檬酸三乙酯(任选与抗氧化剂,如丁基羟基甲苯结合)或离子交换树脂;
能够提供阳光防护(UV过滤)的活性成分:适合的活性成分是滤光物质(遮光剂),其能够从阳光中吸收UV辐射并将其转化为热;按照所需的作用,优选以下的光防护剂:能够在约280-315nm的范围内选择性地吸收导致晒斑的高能UV辐射并透射例如315-400nm(UV-A范围)的长波长范围的光防护剂(UV-B吸收剂),以及只吸收315-400nm的UV-A范围的长波长辐射的光防护剂(UV-A吸收剂);
适合的光防护剂为,例如,有机UV吸收剂对氨基苯甲酸衍生物、水杨酸衍生物、二苯甲酮衍生物、联苯酰甲烷衍生物、二苯基丙烯酸酯衍生物、苯并呋喃衍生物、包含一种或多种有机硅自由基的聚合的UV吸收剂、肉桂酸衍生物、樟脑衍生物、三苯氨基-s-三嗪衍生物、苯基苯并咪唑磺酸及其盐、基邻氨基苯甲酸盐、苯并三唑衍生物,和/或选自氧化铝或氧化硅涂覆的TiO2、氧化锌或云母的无机微颜料;
抗昆虫的活性成分(驱虫剂)是一种意图阻止昆虫接触皮肤且在那阻止昆虫变得有活性的试剂;它们将昆虫赶走并慢慢的汽化;最长用的驱虫剂是二乙基甲苯酰胺(DEET);其它普通的驱虫剂。参见例如“Pflegekosmetik”(W.Raab and U.Kindl,Gustav-Fischer-Verlag Stuttgart/New York,1991)中的161页;
抗化学和机械影响的活性成分:这些包括在皮肤和外部有害物质之间形成屏障的所有物质,如,石蜡油、硅油、植物油、PCL产品和为了抵抗水溶液用的羊毛脂、成膜剂如藻酸钠、三乙醇胺藻酸盐、聚丙烯酸酯、聚乙烯醇或为了抵抗有机溶剂的影响用的纤维素醚,或为了抵抗在皮肤上的危险的机械应力而作为润滑剂的基于矿物油、植物油或硅油的物质;
保湿物质:将例如以下物质用作控湿剂(保湿剂):乳酸钠、尿素、醇、山梨糖醇、甘油、丙二醇、胶原蛋白、弹性蛋白和透明质酸;
具有角质成形效果的活性成分:苯甲酰基过氧化物、视黄酸、胶体硫和间苯二酚;
抗菌剂,如,三氯生或季铵化合物;
可皮肤施用的油质的或油溶性维生素或维生素衍生物:例如维生素A(以其游离酸或衍生物形式的视黄醇)、泛醇、泛酸、叶酸、及其结合、维生素E(生育酚)、维生素F;必需脂肪酸、烟酰胺(烟酸酰胺);
基于维生素的胎盘提取物:活性成分组合物,尤其包含维生素A,C,E,B1,B2,B6,B12,叶酸,生物素,氨基酸,酶以及微量元素镁、硅、磷、钙、锰、铁或铜的化合物;
皮肤修复复合物:从失活的和分解的双歧杆菌群的细菌培养物获得;
植物和植物提取物:例如山金车酊、芦荟、须苔藓、常春藤、刺荨麻、人参、散沫花叶、洋柑桔、金盏花、迷迭香、洋苏草、马尾或百里香;
动物提取物:例如蜂王浆、蜂胶、蛋白质或胸腺提取物;
可皮肤施用的化妆品油:Miglyol 812型中性油、杏仁油、鳄梨油、巴巴苏仁油、棉籽油、玻璃苣油、蓟油、花生油、γ-oryzanol、rosehip-seed油、麻油、榛子油、黑醋栗油、霍霍巴油、樱桃-石油、鲑鱼油、亚麻籽油、玉米籽油、澳大利亚坚果油、杏仁油、晚樱草油、貂油、橄榄油、山核桃油、桃核油、阿月浑子果油、油菜油、稻米油、蓖麻油、红花油、芝麻油、大豆油、向日葵油、茶树油、葡萄籽油或小麦胚芽油;
条状制剂优选为无水的,但在特定的情况下可以包含一定量的水,然而,所用水大体上不能超过40重量%,基于化妆品制剂的总重量计。
如果按照本发明的化妆品制剂和配制是半固体产品的形式,也就是说是膏或霜的形式,同样地它们可以是无水的或含水的。例如,这样的制剂和配放是睫毛油、眼线、粉底、胭脂、眼影或用于处理眼下的圈的组合物。
在另一方面,如果这种膏或霜是含水的,它们尤其是水包油型或油包水型乳液,除颜料外,其包括1-98.8重量%的脂肪相,1-98.8重量%的水相和0.2-30重量%的乳化剂。
这些膏和霜还可包含进一步的传统添加剂,例如,香料、抗氧剂、防腐剂、成凝胶剂、UV过滤剂、着色剂、颜料、珠光剂、无色聚合物以及无机或有机填料。
如果制剂是粉末的形式,其基本上由矿物的或无机的或有机的填料,例如,滑石、陶土、淀粉、聚乙烯粉末或聚酰胺粉末以及助剂如粘结剂、着色剂等组成。
在该制剂中同样可以包含各种用于化妆品中的传统助剂,如香味剂、抗氧剂、防腐剂等等。
如果按照本发明的化妆品制剂和配方是指甲油,其基本上由在溶剂体系中的溶液形式的硝化纤维和天然或合成聚合物构成,该溶液很有可能包含其它助剂,例如珠光剂。
在该实施方案中,着色聚合物以约0.1-5重量%的量存在。
按照本发明的化妆品制剂和配方也可用来染发,在此种情况下它们是以香波、霜或凝胶的形式使用,其包含了常用于化妆品工业的基本物质和本发明颜料。
按照本发明的化妆品制剂和配方可用传统方式制备,例如将各种成分混合或搅拌在一起,任选加热以使混合物熔融。
下面的实施例举例说明了本发明而不限制其范围。除非另外明确指出,百分数和份数分别为重量百分数和重量份数。
实施例
实施例1
将一片尺寸为4×4cm的平板玻璃作为目标材料放置于真空室(BAK 600,Balzers AG)中,根据需要,在该真空室中使用电子枪或焦耳加热可汽化各种引入的物质。首先,在1.3310-2Pa的压力下利用引入的铝(焦耳加热,1400-1500℃)和氧化硅(电子枪),其中二者的蒸汽喷射重叠,从而以0.2nm/s的汽化沉积率建立金属铝和SiO的混合层;然后,在该层的上面由引入的二氧化钛汽化沉积(电子枪)成TiO2层。
SiO/Al层和TiO2层的厚度可使用显微扫描设备测定,SiO层的化学计量数由ESCA测定。用D65标准光照明于10°和45°的视角下测量反射光颜色(CIE-L*C*h)。根据实施例1所获得的样品1和2的SiO/Al层和TiO2层的厚度在表1中给出。于10°和45°的视角下样品1和2的反射颜色在表2中给出。
实施例2
重复实施例1,但汽化铝和二氧化硅而不是铝和氧化硅。按照实施例2所获得的样品3的SiO2/Al层和TiO2层的厚度在表1中给出。于10°和45°的视角下样品3的反射颜色在表2中给出。
实施例3
重复实施例2,但汽化二氧化硅,而不是二氧化钛,此外,氧化硅在二氧化硅之后汽化。按照实施例3所获得的样品4的SiO2/Al层、SiO2层和SiO层的厚度在表1中给出。于10°和45°的视角下样品4的反射颜色在表2中给出。
在实施例1-3中,控制汽化使铝与SiO和/或SiO2的重量比约为50∶50。
表1
实施例 | 样品 | 载体 | 第一层 | 第二层 | 第三层 |
1 | 1 | 玻璃 | 30nmAl/SiO | 192nm TiO2 | - |
1 | 2 | 玻璃 | 28nmAl/SiO | 192nm TiO2 | - |
2 | 3 | 玻璃 | 118nmAl/SiO2 | 192nm TiO2 | - |
3 | 4 | 玻璃 | 118nmAl/SiO2 | 330nm SiO2 | 50nmSiO |
表2
样品 | 视角[°] | L* | a | b | C* | h |
1 | 10 | 75.4 | -33.5 | -17.2 | 37.6 | 207.2 |
1 | 45 | 69.8 | -14.1 | -29.2 | 32.5 | 244.3 |
2 | 10 | 62.7 | -44.1 | -23.1 | 49.8 | 207.6 |
2 | 45 | 55.8 | -21.2 | -36.5 | 42.2 | 239.9 |
3 | 10 | 99 | -8.7 | 34.3 | 35.4 | 104.2 |
3 | 45 | 98 | -13.5 | 27.4 | 30.6 | 116.3 |
4 | 10 | 82.7 | -42.2 | 13.7 | 44.3 | 162 |
4 | 45 | 78 | 39.3 | -7 | 39.9 | 349.9 |
实施例4
在氩气下将样品2和3在650℃加热2小时。用这种方式所获得的样品2’和3’于10°和45°的视角下的反射颜色在表3中给出。
表3
样品 | 视角[°] | L* | a | b | C* | h |
2’ | 10 | 52.5 | -22.6 | -11.9 | 25.5 | 207.8 |
2’ | 45 | 50.1 | -14 | -20.1 | 24.5 | 235.2 |
3’ | 10 | 56.4 | -33.3 | 11.6 | 35.3 | 160.8 |
3’ | 45 | 57.6 | -38 | -6.9 | 38.7 | 190.3 |
Claims (12)
1.一种片状颜料,其颗粒大体上具有2μm-5mm的长度,2μm-2mm的宽度和20nm-1.5μm的厚度,以及长度和厚度之比至少2∶1,其包括(a)一个由煅烧含有SiOz和一种金属的层而得到的层,其中0.03≤z≤2.0。
2.按照权利要求1的片状颜料,其中层(a)形成颜料的内核。
3.按照权利要求1或2任一项的片状颜料,其包括:
(b1)一个SiOz层,
(a)一个由煅烧含有SiOz和一种金属的层而得到的层,
(b2)一个SiOz层,其中0.03≤z≤2.0。
4.按照权利要求2或3任意一项的片状颜料,其包括:
(c1)一个高折射指数的金属氧化物的层,优选TiO2,
(b1)任选的,一个SiOz层,
(a)一个由煅烧含有SiOz和一种金属的层而得到的层,
(b2)任选的,一个SiOz层,其中0.03≤z≤2.0,和
(c2)一个高折射指数的金属氧化物的层,优选TiO2;或
(c1)一个碳层,
(b1)一个SiOz层,
(a)一个由煅烧含有SiOz和一种金属的层而得到的层,
(b2)一个SiOz层,其中0.03≤z≤2.0,和
(c2)一个碳层;或
(c1)一个含有碳化硅(SiC)的层,
(b1)一个SiOz层,
(a)一个由煅烧含有SiOz和一种金属的层而得到的层,
(b2)一个SiOz层,其中0.03≤z≤2.0,和
(c2)一个含有碳化硅(SiC)的层。
5.按照权利要求1-4任一项的片状颜料,其中0.03≤z≤0.95。
6.按照权利要求1-4任一项的片状颜料,其中0.95≤z≤2.0,优选1.40≤z≤2.0,更优选2.0。
7.按照权利要求1-6任一项的片状颜料,其中金属是Al、Cu、Mo、V、Ag、Cr、Zr、Nb、Ni、Fe、Co、Ti或其合金,如铬-镍、铁-镍、铁-铬和镍-钴,优选铝。
8.按照权利要求1-7任一项的片状颜料的制备方法,包括
a)将分离剂层蒸汽沉积至载体上,
b)然后,同时将金属和SiOz蒸汽沉积在分离剂层上,其中0.03≤z≤2.0,
c)将分离剂溶解于溶剂中,
d)从溶剂中分离出产品,和
e)煅烧产品。
9.按照权利要求8的方法,其中1.0≤z≤1.8。
10.按照权利要求9的方法,其中在步骤(b)中用两个分离的汽化器进行SiOz/金属层的蒸汽沉积,一个汽化器装有包括Si和SiO2、SiOz或其混合物的混合物,其中1.0≤z≤1.8,另一个汽化器装有金属。
11.一种按照权利要求8-10任一项的方法所获得的片状颜料。
12.按照权利要求1-7和11任一项的颜料的用途,用于油漆、纺织品、喷墨打印、化妆品、涂料组合物、塑料、打印墨水以及瓷器和玻璃的珐琅。
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-
2004
- 2004-01-15 EP EP04702292A patent/EP1585792B1/en not_active Expired - Lifetime
- 2004-01-15 KR KR1020057013628A patent/KR101057964B1/ko not_active IP Right Cessation
- 2004-01-15 CA CA002512892A patent/CA2512892A1/en not_active Abandoned
- 2004-01-15 MX MXPA05007871A patent/MXPA05007871A/es not_active Application Discontinuation
- 2004-01-15 CN CNA2004800025747A patent/CN1742059A/zh active Pending
- 2004-01-15 AT AT04702292T patent/ATE359327T1/de not_active IP Right Cessation
- 2004-01-15 JP JP2006500574A patent/JP2006517988A/ja not_active Ceased
- 2004-01-15 US US10/542,036 patent/US7291216B2/en not_active Expired - Fee Related
- 2004-01-15 WO PCT/EP2004/000249 patent/WO2004065492A1/en active IP Right Grant
- 2004-01-15 DE DE602004005817T patent/DE602004005817T8/de active Active
- 2004-01-15 AU AU2004205733A patent/AU2004205733A1/en not_active Abandoned
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101768015B (zh) * | 2009-12-25 | 2012-06-20 | 华南理工大学 | 一种黑色纳米陶瓷颜料及其制备方法 |
CN107567484A (zh) * | 2015-04-15 | 2018-01-09 | 舒伦克金属颜料公司 | 珠光颜料、珠光颜料的制造方法以及该颜料的用途 |
CN107567484B (zh) * | 2015-04-15 | 2021-07-27 | 舒伦克金属颜料公司 | 珠光颜料、珠光颜料的制造方法以及该颜料的用途 |
CN106995660A (zh) * | 2017-06-02 | 2017-08-01 | 中国科学院包头稀土研发中心 | 一种新型稀土油画颜料及其制备方法 |
CN106995660B (zh) * | 2017-06-02 | 2019-04-05 | 中国科学院包头稀土研发中心 | 一种新型稀土油画颜料及其制备方法 |
CN111187527A (zh) * | 2018-11-14 | 2020-05-22 | 丰田自动车株式会社 | 光辉性颜料及其制造方法 |
Also Published As
Publication number | Publication date |
---|---|
ATE359327T1 (de) | 2007-05-15 |
MXPA05007871A (es) | 2005-09-21 |
DE602004005817D1 (de) | 2007-05-24 |
DE602004005817T8 (de) | 2008-04-30 |
KR101057964B1 (ko) | 2011-08-22 |
DE602004005817T2 (de) | 2008-01-10 |
WO2004065492A1 (en) | 2004-08-05 |
CA2512892A1 (en) | 2004-08-05 |
US20060048676A1 (en) | 2006-03-09 |
JP2006517988A (ja) | 2006-08-03 |
AU2004205733A1 (en) | 2004-08-05 |
EP1585792B1 (en) | 2007-04-11 |
EP1585792A1 (en) | 2005-10-19 |
KR20050103908A (ko) | 2005-11-01 |
US7291216B2 (en) | 2007-11-06 |
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