CN103502364B - 镀银颜料及其生产方法 - Google Patents
镀银颜料及其生产方法 Download PDFInfo
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- CN103502364B CN103502364B CN201280020690.6A CN201280020690A CN103502364B CN 103502364 B CN103502364 B CN 103502364B CN 201280020690 A CN201280020690 A CN 201280020690A CN 103502364 B CN103502364 B CN 103502364B
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- silver
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- 239000000049 pigment Substances 0.000 title claims abstract description 66
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000000034 method Methods 0.000 claims abstract description 43
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 35
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000012895 dilution Substances 0.000 claims abstract description 26
- 238000010790 dilution Methods 0.000 claims abstract description 26
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 239000011159 matrix material Substances 0.000 claims description 36
- 239000000725 suspension Substances 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 13
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 12
- 239000008103 glucose Substances 0.000 claims description 12
- 239000001509 sodium citrate Substances 0.000 claims description 8
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 8
- 229940038773 trisodium citrate Drugs 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000007772 electroless plating Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 239000002966 varnish Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 21
- 150000003606 tin compounds Chemical class 0.000 abstract description 13
- 238000002360 preparation method Methods 0.000 description 19
- 229910052709 silver Inorganic materials 0.000 description 12
- 239000004332 silver Substances 0.000 description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 11
- 239000002245 particle Substances 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 101150003085 Pdcl gene Proteins 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000007747 plating Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000000845 anti-microbial effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 3
- 238000007781 pre-processing Methods 0.000 description 3
- 238000002203 pretreatment Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229960001866 silicon dioxide Drugs 0.000 description 2
- -1 silver ions Chemical class 0.000 description 2
- HEUBDYLTIBJGRL-UHFFFAOYSA-N 1-triethoxysilyldecan-1-one Chemical compound CCCCCCCCCC(=O)[Si](OCC)(OCC)OCC HEUBDYLTIBJGRL-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910002666 PdCl2 Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- HSMXEPWDIJUMSS-UHFFFAOYSA-K aluminum;tetradecanoate Chemical compound [Al+3].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O HSMXEPWDIJUMSS-UHFFFAOYSA-K 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 230000003412 degenerative effect Effects 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
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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
- C09C1/0078—Pigments consisting of flaky, non-metallic substrates, characterised by a surface-region containing free metal
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
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- A61Q1/10—Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
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- A61Q3/00—Manicure or pedicure preparations
- A61Q3/02—Nail coatings
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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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- C09C1/407—Aluminium oxides or hydroxides
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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- C01P2004/00—Particle morphology
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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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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
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- Chemically Coating (AREA)
Abstract
本发明公开了一种用于生产镀银(Ag)颜料的方法。根据本发明的用于生产镀银颜料的所述方法包括:在所述基质表面形成锡化合物预处理层的步骤;和使用稀释的硝酸银溶液、氨水、柠檬酸溶液和稀释的氢氧化钾溶液通过回流和无电镀过程在所述锡化合物预处理层的下面部分形成镀银层的步骤。
Description
发明领域
本发明涉及镀银颜料(Ag coating pigment)及其制备方法,以及更具体地,涉及通过提高不使用昂贵化合物如PdCl2作为预处理材料的无电镀的镀层效率而具有改良的经济可行性的能够容易地生产高亮度镀银颜料的技术。
背景技术
珠光颜料用粉末形成,其具有在所述粉末的透明基质上形成的镀层。在这里,代表性地,使用高折射率金属氧化物如TiO2、Fe2O3等等和低折射率材料如SiO2、MgO·SiO2镀所述透明基质。这样的材料以单层或多层镀到所述透明基质上,从而制备各种颜色的珠光颜料。
然而,所述珠光颜料的问题在于不容易进行使用金属盐(其在制备金属氧化物的过程中为起始材料)制备初反应溶液的过程,以及由于所述金属氧化物的光学性质所述颜料不具有不同于金属的高光泽。
发明内容
技术问题
本发明的一个方面提供制备镀银颜料的方法,其具有提高的效率并能够在具有预处理层和银(Ag)镀层的堆叠结构的颜料的制备中通过排除预处理层的形成中的昂贵的金属化合物如PdCl2和镀银过程中的昂贵的装置如溅镀机、微波辐照器等降低生产成本。
本发明的另一个方面提供制备镀银颜料的方法,其能够通过在银(Ag)镀层的形成中将传统的清洁、敏化作用和活化作用过程集成化和简化至单一的回流过程降低用于过程和设施的成本。
技术方案
根据本发明的一个实施方案,用于制备镀银(Ag)颜料的方法包括:在基质表面形成锡化合物预处理层;和使用硝酸银稀释溶液、氨水、柠檬酸溶液和稀释的氢氧化钾溶液通过回流和无电镀在所述锡化合物预处理层上形成银镀层。
更具体地,制备镀银(Ag)颜料的方法包括:(a)通过将基质与盐酸溶液混合制备浆体;(b)通过回流所述浆体从所述基质的表面除去杂质;(c)通过向(b)的所述浆体加入SnCl2·2H2O和回流所述浆体在所述基质的表面形成SnCl2预处理层;(d)通过所述浆体的脱水和水洗形成镀有SnCl2预处理层的颜料粉末;(e)通过混合硝酸银、纯水、氨水和柠檬酸钠形成稀释的硝酸银溶液,以及通过将所述镀有SnCl2预处理层的颜料粉末与所述稀释的硝酸银溶液混合形成悬浮液;(f)将所述悬浮液与稀释的葡萄糖溶液混合并回流所述混合物;(g)将(f)的所述悬浮液与稀释的氢氧化钾(KOH)溶液混合并另外回流所述混合物;(h)向(g)的所述悬浮液加柠檬酸溶液,并通过回流和无电镀在所述预处理层形成镀银(Ag)层;以及(i)进行(h)的所述悬浮液的脱水和水洗,并干燥所产生的悬浮液。
有益效果
根据本发明,所述制备镀银(Ag)颜料的方法可以通过不使用昂贵金属化合物如PdCl2的形成预处理层降低生产成本和用于设施的投资成本。
另外,所述制备镀银(Ag)颜料的方法可以通过集成化和简化传统过程为单一的回流过程、不使用传统的溅镀或微波辐照过程而降低过程成本和提高生产效率。
而且,根据本发明,所述镀银(Ag)颜料具有优异的抗菌性质和电磁波屏蔽效应。
附图简介
图1描绘了根据本发明的实施方案的颜料粉末的电磁波屏蔽效应。
最佳实施方式
下列实施方案的具体描述连同附图将使本发明的上述和其它方面、特征及优势变得很明显。然而,应当理解,本发明不限于下列实施方案并且可以以不同的方式体现,以及为了充分公开和本领域技术人员彻底理解本发明而提供所述实施方案。本发明的范围应当仅由所附权利要求及其等同物限定。
在下文中,将具体描述根据本发明的实施方案的镀银(Ag)颜料及其制备方法。
根据本发明的一个实施方案,颜料包括:在基质表面形成的促进镀层的预处理层;和在所述预处理层上形成的镀银层。
传统的预处理过程具有低的经济可行性因为所述预处理过程使用昂贵的化合物如PdCl2或通过几个过程进行。然而,如果进行预处理,存在问题即溅镀装置或微波辐照器被用于镀银,从而增加设备成本。
因此,根据本发明,使用盐酸(HCl)和锡化合物(SnCl2·2H2O)制备浆体,然后回流,从而在所述基质上形成所述锡化合物的预处理层。
预处理
首先,使用基质、优选为平坦基质的小薄片制备包含按重量计算(wt%)10%到20wt%的固形物和稀释到1wt%到10wt%的浓度的盐酸溶液的浆体。
在这里,所述基质包括选自玻璃鳞片、云母、镀二氧化钛的玻璃鳞片、镀二氧化钛的云母、镀氧化铁的云母、镀氧化铁的玻璃鳞片、板状氧化铁、板状氧化铝和板状二氧化硅中的至少一种。
另外,如果所述盐酸溶液具有小于1wt%的浓度,那么随后的杂质去除可能是困难的,以及如果所述盐酸溶液具有大于10wt%的浓度,那么由于所述基质表面的过度蚀刻,随后的形成镀层的过程可能不正常地进行。
而且,如果所述浆体有少于10wt%的固形物在浆体中,那么由于所述基质的数量不足,生产率可能会下降,以及如果所述浆体具有大于20wt%的固形物,那么形成所述镀层需要的时间增加,退化过程效率。
在制备所述浆体后,将所述浆体回流1小时到3小时,以便从所述基质的表面去除所有杂质。
因此,如果回流时间小于1小时,那么所述杂质可能去除得不充分,以及如果所述回流时间超过3小时,所述基质的表面可能被过度蚀刻,据此随后的镀层过程可能不正常地进行。
在完成所述基质表面的预处理后,向所述浆体中加入锡化合物如SnCl2·2H2O,然后回流1小时到3小时,从而在所述基质的表面形成锡化合物预处理层,例如1重量份到10重量份的SnCl2基于100重量份的所述基质。
在这里,如果所述锡化合物预处理层以基于100重量份所述基质小于1重量份的量形成,那么所述锡化合物预处理层具有非常小的厚度并因此不能胜任预处理层的功能。相反地,如果所述锡化合物预处理层以基于100重量份所述基质大于10重量份的量形成,那么由于增加的厚度,在随后的镀层过程中可能发生破裂,以及所述颜料的性能如光泽度和亮度可能退化。
另外,如果回流时间小于1小时,那么所述锡化合物预处理层可能以基于100重量份所述基质小于1重量份的量不充分地形成。而且,如果回流时间超过3小时,那么所述锡化合物预处理层以基于100重量份所述基质大于10重量份的量形成,从而导致所述预处理层的过大的厚度。
在完成如上文描述的预处理过程后,将所述浆体脱水并用纯水洗涤,从而完成镀有所述预处理层的颜料粉末的制备。
接下来,为了保护根据本发明的所述颜料的高亮度,在所述颜料粉末的表面形成镀银层。
在这里,为了镀银,制备下列三种类型的溶液。接下来,将所述预处理的颜料粉末加入将制备的溶液在其中混合的悬浮液,然后回流,从而进行镀银。
同样地,根据本发明的所述镀银过程可以通过消除传统的电镀过程而简化制备过程,并且由于不使用非常昂贵的PdCl2可以提高经济可行性。
镀银
1)稀释的硝酸银溶液
通过向基于100重量份基质的10重量份到70重量份的硝酸银加入纯水、氨水和柠檬酸钠,制备稀释的硝酸银溶液。
在这里,硝酸银的量可以根据所述基质的颗粒尺寸而变化。如果所述基质具有大的颗粒尺寸,那么基于100重量份的所述基质、硝酸银的加入量可以减少至10重量份,以及如果所述基质具有小的颗粒尺寸,那么基于100重量份的所述基质、硝酸银的加入量可以增加至70重量份。
然而,如果基于100重量份的所述基质、硝酸银的量小于10重量份,那么镀银的作用将变得不重要,以及如果基于100重量份的所述基质、硝酸银的量超过70重量份,那么所述镀银层具有过大的厚度,从而导致经济可行性方面的问题。
接下来,基于100重量份的硝酸银,所述氨水优选以50重量份到150重量份的量存在。
如果基于100重量份的硝酸银、所述氨水的加入量小于50重量份,那么银可能被部分氧化,这样使得所述稀释的银溶液具有非透明色,也就是说,半透明的或不透明的颜色。结果,在所述镀层的形成中,晶体生长和黏附可能劣化。相反地,如果基于100重量份的硝酸银、所述氨水的加入量超过150重量份,那么由于还原成银的能力的退化,反应效率可能降低以及由于氨水的恶臭,设施条件可能被损害。
接下来,基于100重量份的硝酸银,将15重量份到100重量份的柠檬酸钠加入所述稀释的硝酸银溶液,然后回流。
在这里,如果基于100重量份的硝酸银、柠檬酸钠的量小于15重量份,那么镀银层的黏附可能减少,从而使其难以形成致密的晶体。相反地,如果基于100重量份的硝酸银、柠檬酸钠的量超过100重量份,那么由于增加的阳离子浓度,可能发生镀银颗粒的凝聚。
2)稀释的葡萄糖溶液
基于100重量份的硝酸银,将100重量份到200重量份的葡萄糖用纯水稀释。稀释的葡萄糖溶液可能包含约5wt%到约30wt%的葡萄糖,但并不限于此。
在这里,如果葡萄糖的加入量小于100重量份,那么由于反应完成后银离子在溶液中的存在,经济可行性劣化。如果葡萄糖的加入量超过200重量份,那么可能显现不出葡萄糖加入的效果。
3)稀释的氢氧化钾溶液
基于100重量份的硝酸银,将100重量份到200重量份的氢氧化钾用纯水稀释。稀释的氢氧化钾溶液可能包含约5重量份到约30重量份的氢氧化钾,但并不限于此。
在这里,基于100重量份的硝酸银,稀释的氢氧化钾溶液优选包含100重量份到200重量份的氢氧化钾。如果基于100重量份的硝酸银、氢氧化钾的量小于100重量份,那么镀银层的黏附可能劣化,从而抑制致密晶体的形成。相反地,如果基于100重量份的硝酸银、氢氧化钾的量超过200重量份,那么可能发生镀银颗粒的凝聚,导致非均匀镀层。
如上文描述的,在完成用于镀银的主要溶液的制备后,通过向稀释的硝酸银溶液加入所述预处理的颜料粉末制备悬浮液。接下来,将稀释的葡萄糖溶液加入所述悬浮液,接下来将其立即回流。
接下来,使用计量泵在30分钟到3小时的时间内将所述稀释的氢氧化钾溶液缓慢加入所述悬浮液。
在这里,如果所述稀释的氢氧化钾溶液加入时间不充分少于30分钟,那么用于随后镀银的晶体生长可能会变差,并且回流可能被不充分地进行。相反地,如果所述稀释的氢氧化钾溶液的加入时间超过30分钟,那么银从硝酸银转化为氧化银,导致镀层过程的异常进行,并且由于制备时间的增加,经济可行性可能劣化。
如上文描述的,在向所述悬浮液加入所述稀释的氢氧化钾溶液后,将所产生的悬浮液另外回流约30分钟到约3小时。
接下来,基于100重量份的硝酸银,在完成所述另外的回流过程后向所述悬浮液加入50重量份到200重量份的柠檬酸溶液,并最后进行50分钟到70分钟的回流和无电镀,从而制备颜料,在其上,基于100重量份的所述基质形成10重量份到35重量份的镀银层。
在这里,如果基于100重量份的硝酸银、所述柠檬酸溶液的加入量小于50重量份,或者所述回流时间少于50分钟,那么在所述溶液内的部分团聚的颗粒的可分散性可能劣化。相反地,如果基于100重量份的硝酸银、所述柠檬酸溶液的加入量超过200重量份,或者所述回流时间超过70分钟,那么所述镀银可能重新溶入水溶液。
接下来,在将所产生的悬浮液脱水并用纯水洗涤后,将所述悬浮液在30℃到100℃干燥,从而制备在其上形成所述镀银层的颜料粉末。在这里,如果所述干燥温度低于30℃,那么由于过长的干燥时间,经济可行性可能劣化,以及如果所述干燥温度超过100℃,那么可能存在损害具有扩大的比表面积的镀银颗粒的可能性,并且所述镀银颗粒的凝聚可能增加。
同样地,根据本发明的具有镀银层的颜料粉末可以容易地制备,并且具有高亮度和通过消除作为预处理材料的昂贵化合物如PdCl2和低镀层效率的无电镀而提高的经济可行性。
因此,由于所加入金属——银(Ag)的高亮度,所述颜料粉末具有提高的亮度。
另外,使用所述悬浮液通过涂覆法可能提高银的抗菌性能以及增加银的比表面积,这样使得所述颜料可能具有与所述银的比表面积增加相称的提高的亮度和抗菌性能。也就是说,所述颜料可能在亮度、光泽度和色度方面具有比由传统无电镀方法生产的镀层颜料更高的性能。接下来,将根据一些实施例更详细地解释本发明。
测量结果
表1显示取决于基于100重量份的基质的镀银层和柠檬酸钠的重量份的色度计测量值。所述基质由玻璃鳞片组成,并且在镀银层形成之前,基于100重量份的所述基质形成5重量份的SnCl2预处理层。
在所述样品在暗度表上减少至PC6%(用NC树脂)后,在黑色背景进行实施例和比较实施例的样品测量。
1)色度测量值(在75度使用MINOLTA cm-512m3测量)
表1
参阅表1,能够看出实施例1到6的所有样品具有比比较实施例1到2的那些更高的光度(L)值。另外,能够看出当实施例1到6的a和b值在靠近无色的区域分布时,比较实施例1和2的a和b值向有色区域加重。因此,能够看出根据本发明的镀银层具有提高的亮度和色度。
2)光泽计测量值(在60度使用DENSHOKU PG-1M测量)
表2
参阅表2,能够看出实施例1到6的所有样品具有比比较实施例1到2优秀的光泽性能。
根据本发明,所述镀银(Ag)颜料除了优异的光泽性能之外还提供优异的抗菌性能和电磁波屏蔽效应。
接下来,将根据试验结果更详细地描述根据本发明的所述颜料粉末的抗菌性能。
将试验外包给FITI试验研究院(FITI Testing&Research Institute),并且依照KS4206:2008,SHAKE FLASK METHOD进行抗菌活性试验。
使用实施例1和2中制备的颜料作为样品,以及使用比较实施例3和4中制备的颜料作为样品,其中仅将镀银层从实施例1和2的颜料中排除。
随着在各个样品中放相同量的细菌,在24小时后测量试验结果。结果在表3中显示。
表3
比较实施例3 | 实施例1 | 比较实施例4 | 实施例2 | |
初始瞬间 | 1.7*104 | 1.7*104 | 1.5*104 | 1.5*104 |
24小时后 | 9.3*106 | <10 | 1.3*105 | <10 |
去除率(%) | - | 99.9 | - | 99.9 |
从表3可以看出,实施例1和2的样品具有比比较实施例3和4的那些高得多的细菌去除率。
接下来,为了调查根据本发明的颜料粉末的电磁波屏蔽效应,使用实施例1和2的颜料进行电磁波屏蔽试验。
依照关于国际标准的框架法第23条、执行法令第16条和KS A ISO/IEC17025:2006(Article23of the Framework Act on international standards,Enforcement decree Article16,and KS A ISO/IEC17025:2006),由忠清北道科技园IT聚集中心(韩国)[Chungbuk TechnoPark IT Convergence Center(Korea)]进行试验。
另外,结果如表4所示,图表显示于图1。在图1中,10%镀层意味着基于100重量份的基质、所述镀银层以10重量份的量存在,以及15%镀层意味着基于100重量份的基质、所述镀银层以15重量份的量存在。
表4
从表4和图1可以看出,根据本发明的所有颜料粉末具有10dB或更高的电磁波屏蔽率。由这个结果可以看出,根据本发明的颜料粉末具有优异的电磁波屏蔽功效。
如上文所述,根据本发明,基于所述预处理层的形成,所述制备镀银(Ag)颜料的方法能够通过消除昂贵的金属化合物如PdCl2和昂贵的装置如溅镀装置、微波辐照器等降低生产成本和设施投资成本。
另外,所述制备镀银(Ag)颜料的方法能够通过集成化和简化传统过程为单一的回流过程、不使用传统的无电镀从而降低过程成本和提高生产效率。
根据本发明,所述镀银颜料可作为化妆品的颜料使用,如口红、眼影、指甲油等。
表5到7显示包括实施例2所制备颜料和MC2080PS(Nippon sheet glass Co.,Ltd.)的口红(表5)、眼影(表6)和指甲油(表7)的组成成分。
表5显示使用实施例2所制备颜料的口红1和使用颜料MC2080PS的口红2的组成成分。
表5(单位:wt%)
表6显示使用实施例2制备的颜料的眼影1和使用颜料MC2080PS的眼影2的组成成分。
表6(单位:wt%)
成分 | 眼影1 | 眼影2 |
颜料 | 10.0 | 10.0 |
滑石 | 68.40 | 68.40 |
云母 | 7.20 | 7.20 |
硬脂酸锌 | 5.40 | 5.40 |
二氧化硅 | 4.50 | 4.50 |
聚甲基丙烯酸甲酯 | 2.88 | 2.88 |
二氧化钛 | 1.44 | 1.44 |
肉豆蔻酸铝 | 0.09 | 0.09 |
三乙氧基辛酰硅烷 | 0.05 | 0.05 |
二甲聚硅氧烷 | 0.04 | 0.04 |
总计 | 100.00 | 100.00 |
表7显示使用实施例2制备的颜料的指甲油1和使用颜料MC2080PS的指甲油2的组成成分。
表7(单位:wt%)
根据表5到7所列组成成分制备的口红、眼影和指甲油的性能如应用等级、隐蔽、颜色和哑光性能如表8所示。
为了评估各个产品的应用等级、隐蔽、颜色和哑光性能,由年龄在20岁到40岁的40个女性进行感官评价(0分到100分)如所述产品作为化妆品使用后的意见等,根据平均值提供和评定得分,如下:
X(低于60分):坏的
Δ(60分到69分):中等
O(70分到79分):比较好
◎(80分到89分):优异(Excellent)
(90分到100分):极其优异(Extremely Excellent)
表8
参阅表8,当使用实施例2制备的颜料作为化妆品颜料时,证实所述化妆品在应用等级、隐蔽、透明性和颜色方面表现出优异的性能。这意味着根据本发明的所述镀银颜料能够表现出高亮泽的颜色同时保持等于或优于典型化妆品颜料的功能。
尽管已根据一些实施方案描述了本发明,但是应当理解的是,本领域技术人员可以不脱离本发明的精神和范围地做出各种修饰、变化、改变和等价的实施方案。因此,本发明的范围应当仅由所附权利要求及其等同物来限定。
Claims (8)
1.一种制备镀银(Ag)颜料的方法包括:
(a)通过混合基质与盐酸溶液制备浆体;
(b)通过回流所述浆体从所述基质的表面去除杂质;
(c)通过向(b)的所述浆体加入以所述基质为100重量份计1-10重量份的SnCl2·2H2O并回流所述浆体在所述基质的表面形成SnCl2预处理层;
(d)通过所述浆体的脱水和水洗形成用所述SnCl2预处理层镀层的颜料粉末;
(e)通过混合硝酸银、纯水、氨水和柠檬酸钠形成稀释的硝酸银溶液,和通过混合所述用所述SnCl2预处理层镀层的颜料粉末与所述稀释的硝酸银溶液形成悬浮液;
(f)混合所述悬浮液与稀释的葡萄糖溶液并回流所述混合物;
(g)混合(f)的所述悬浮液与稀释的氢氧化钾(KOH)溶液并另外回流所产生的悬浮液;
(h)向(g)的所述悬浮液加入柠檬酸溶液,并通过回流和无电镀所述悬浮液在所述预处理层上形成以所述基质为100重量份计10-35重量份的镀银(Ag)层;以及
(i)进行脱水和用(h)的所述悬浮液的水进行洗涤,以及干燥所述悬浮液;
其中,在(a)中,所述盐酸溶液包括1wt%到10wt%的盐酸,以及所述浆体具有10wt%到20wt%的固形物。
2.根据权利要求1所述的方法,其中,在(b)和(c)中,回流进行1小时到3小时。
3.根据权利要求1所述的方法,其中,在(e)中,基于100重量份的所述基质,所述稀释的硝酸银溶液包括10重量份到70重量份的硝酸银;基于100重量份的所述硝酸银,所述氨水以50重量份到150重量份的量存在;以及基于100重量份的所述硝酸银,所述柠檬酸钠以15重量份到100重量份的量存在。
4.根据权利要求1所述的方法,其中,基于100重量份的所述硝酸银,(f)的所述稀释的葡萄糖溶液包括100重量份到200重量份的葡萄糖。
5.根据权利要求1所述的方法,其中,基于100重量份的所述硝酸银,所述稀释的氢氧化钾(KOH)溶液包括100重量份到200重量份的氢氧化钾,并使用计量泵加入30分钟到3小时。
6.根据权利要求1所述的方法,其中,在(h)中,基于100重量份的所述硝酸银,所加入的柠檬酸溶液以50重量份到200重量份的量加入。
7.根据权利要求1所述的方法,其中,在(i)中,在30℃到100℃进行干燥。
8.包括通过根据权利要求1到7的任一项的所述方法制备的镀银颜料的口红、眼影或指甲油。
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