CN106661341A - 用于给漆料调色的固体着色剂 - Google Patents
用于给漆料调色的固体着色剂 Download PDFInfo
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- CN106661341A CN106661341A CN201580028190.0A CN201580028190A CN106661341A CN 106661341 A CN106661341 A CN 106661341A CN 201580028190 A CN201580028190 A CN 201580028190A CN 106661341 A CN106661341 A CN 106661341A
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- 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
- C09B67/0084—Dispersions of dyes
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- C09B67/009—Non common dispersing agents polymeric dispersing agent
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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
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- 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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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- 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
- C09B67/0095—Process features in the making of granulates
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic pigment
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D5/031—Powdery paints characterised by particle size or shape
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/41—Organic pigments; Organic dyes
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D7/47—Levelling agents
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
- F26B5/065—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing the product to be freeze-dried being sprayed, dispersed or pulverised
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- G—PHYSICS
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- G01F—MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
- G01F13/00—Apparatus for measuring by volume and delivering fluids or fluent solid materials, not provided for in the preceding groups
- G01F13/006—Apparatus for measuring by volume and delivering fluids or fluent solid materials, not provided for in the preceding groups measuring volume in function of time
Landscapes
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- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Molecular Biology (AREA)
- Health & Medical Sciences (AREA)
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Abstract
本发明涉及一种固体着色剂,其包含:a.30‑97重量%的颜料;b.小于5重量%的溶剂;c.3‑40重量%的表面活性剂,并且其中所述固体着色剂的比例S/A[颗粒尺寸分布的标准偏差/平均颗粒尺寸]<25%,优选<22%,且更优选<20%,其中重量%是相对于固体着色剂的总重量,并且其中颗粒尺寸分布是通过使用OCCHIO ZEPHYR ESR分析仪根据ISO 13322‑1静态图像分析第一版2004‑12‑01采用全自动图像分析的光散射测定的。本发明还涉及制备固体着色剂的方法,以及所述固体着色剂用于通过将固体着色剂体积计量给基础漆料来给该基础漆料调色的用途。
Description
本发明涉及用于给漆料组合物着色的固体着色剂、制备固体着色剂的方法以及固体着色剂的用途。
建筑漆料和色料制造商通常提供具有少量流行色的预混漆料和色料。为了满足消费者的要求并且为了能够与现有经涂漆或经着色的表面相匹配,制造商通常还提供一组可调色的漆料以及若干浓缩着色剂。在销售网点利用着色剂分配和摇动混合设备组合它们,从而以远远多于在预混产品中可得的有限颜色的颜色系列制造小批量的定制调色的漆料或色料。
来自不同漆料制造商的定制颜色系统往往具有或多或少类似的组分。例如,典型的定制颜色的漆料系统可以使用若干种(例如2到4种)可调色的基础漆料,范围例如从意欲至多接受少量着色剂的白色基料到意欲接受远远更大量着色剂的相对未经着色的澄清基料。基础漆料可以使用各种粘结剂(例如天然或合成树脂)、各种粘结剂形式(例如溶液状聚合物或胶乳状聚合物)和载体(例如溶剂型或水性的),并且可以提供各种干燥表面面漆(例如无光面漆、半光泽面漆或光泽面漆)。一些制造商还销售有色基础漆料(例如红色基料、蓝色基料和黄色基料),这些基料在深度调色的定制漆料的色调(shade)需要达到一个涂层遮盖力时与额外的着色剂组合。定制颜色的漆料或色料系统中的着色剂可以例如由多着色剂分配站以体积方式计量,其中对于美国市场通常在着色剂分配站中使用12种漆料或色料着色剂,有时在其他市场使用更多(例如16或24种着色剂)。
WO2010091418描述了可用于调色系统中的液体着色剂。液体调色系统的缺点是:难以保持工作位置清洁且难以防止霉菌感染;颜料在液体调色系统中的相分离,这将导致不准确的颜料给料和计量系统的结垢;以及溶剂蒸发的问题,这将改变液体着色剂的浓度和液体着色剂的粘度,使得计量不准确。
WO0047681、EP1474485、US7318864和WO09074576公开了可用于使有色漆料的固体颜料制剂。这些固体颜料制剂是在喷雾干燥过程中制备的。
US2001/0055639描述了制备颗粒状产品的方法。通过双流体喷嘴将颗粒悬浮液喷雾到液氮中。颗粒产品具有宽的或甚至双峰粒度分布。
US2011/0262654描述了一种制备多孔颗粒的方法,其通过电喷雾颗粒的悬浮液,在液氮中收集液滴,然后在真空中干燥。业已得到了不规则的颗粒。
EP0191125描述了通过颗粒的冲击冷却并随后通过升华干燥颗粒来制备固体颗粒的方法。
DE19914329描述了通过喷雾干燥制备固体颗粒的方法。
EP1103173描述了通过喷雾干燥制备固体颜料颗粒的方法。
所有上述方法均制备出具有不规则形状和/或宽颗粒尺寸分布的颗粒。
在喷雾干燥法中制备的颗粒具有许多缺点。它们显示出宽的颗粒尺寸分布,包含相当大量的粉尘并且证明是机械不稳定的。宽的颗粒尺寸分布使得需要在生产颗粒的过程中包括筛分步骤,这使得该方法昂贵并且导致低产率的合适产物。即使在筛分后,颗粒尺寸分布仍然很宽,这导致了若干问题。较小的颗粒(通常具有小于100μm的颗粒尺寸)倾向于团聚成机械不稳定并显示可变堆积密度的聚集体。在团聚之后,堆积密度可能局部增加。同时,小颗粒和大颗粒可以显示渗滤(percolation),这意味着颗粒彼此分离:小颗粒漂移到容器的下部,而较大颗粒倾向于漂浮在较小颗粒的顶部。这种分离导致堆积密度的差异并且给出不规则的颗粒流动行为。此外,在喷雾干燥过程中获得的颗粒不具有规则的圆形形状:许多颗粒具有“甜甜圈”的形状。“甜甜圈”形状导致颗粒之间的内聚力增加,这对颗粒的流动性具有负面影响并影响堆积密度。
由于宽的颗粒尺寸分布和其它性能,现有技术的固体颜料制剂需要以重量方式加入基础漆料组合物中。重量计量通常通过称量包含基础漆料组合物的容器的重量并且确定添加至基础漆料的总重量的颜料制剂来进行。这很复杂,特别是当仅少量的固体颜料制剂应被计量时。在这种情况下,环境中的小变化(例如振动和空气湍流)可能导致大的测量误差,这将产生颜色不合格的着色漆料组合物。颜料的重量测量还意味着所有颜料应以顺序方式加入,因为每种颜料应单独加入。
需要可用于调色系统中,并且可以克服与目前的调色系统相关的一个或多个问题的固体着色剂。
在广泛研究之后,本发明人解决了上述问题并开发了新的固体着色剂,其可有利地用于给基础漆料组合物调色的调色系统中。
发明简述
本发明涉及一种固体着色剂,其包含:
a)30-97wt%的颜料;
b)小于5wt%的溶剂;
c)3-40wt%的表面活性剂;
并且其中固体着色剂的比例S/A[颗粒尺寸分布的标准偏差/平均颗粒尺寸]<25%,优选<22%,且更优选<20%,其中wt%是相对于固体着色剂的总重量,并且其中颗粒尺寸分布是通过使用OCCHIO ZEPHYR ESR分析仪根据ISO 13322-1静态图像分析第一版2004-12-01采用全自动图像分析的光散射测定的。
优选地,固体着色剂的平均颗粒尺寸在400微米和1400微米(μm)之间,优选在500μm和1300μm之间,更优选在600μm和1000μm之间。
颗粒尺寸分布(PSD)、PSD的标准偏差(Std dev)和平均颗粒尺寸(=平均球径)是根据ISO 13322-1静态图像分析第一版2004-12-01,通过使用OCCHIO ZEPHYR ESR分析仪,采用全自动图像分析的光散射测定的。
在一个优选的实施方式中,固体着色剂包含:
a)50-95wt%的颜料;
b)小于3wt%的溶剂;
c)5-30wt%的表面活性剂;
d)0.1-5wt%的添加剂;
e)0-20wt%的无色填料;
f)0-10wt%的粘合剂;
其中固体着色剂的比例S/A[颗粒尺寸分布的标准偏差/平均颗粒尺寸]<25%,优选<22%,且更优选<20%,其中固体着色剂的平均颗粒尺寸在400μm和1400μm之间,优选在500μm和1300μm之间,更优选在600μm和1000μm之间,其中wt%是相对于固体着色剂的总重量。
根据本发明的固体着色剂相对于根据现有技术已知的根据喷雾干燥制备的固体着色剂具有令人惊讶的窄颗粒尺寸分布。此外,着色剂显示出固有着色强度的快速展开,这是快速分散到水性或有机溶剂基的基础漆料中以获得调色的基础漆料的指标。根据本发明的固体着色剂具有高机械稳定性和窄颗粒尺寸分布,这使得可以将固体着色剂以体积方式添加到基础涂料中,而不是将固体着色剂以已知的重量计量到基础涂料组合物中。
固体着色剂中的固体材料的量是使用Kern MLS分析仪设备通过热重分析(TGA)方法测定的。固体含量(%)为100%-水分含量(%)。固体着色剂中的固体材料基本上由颜料、无色填料材料和表面活性剂组成。优选地,固体材料的量相对于固体着色剂的重量为95至99.9wt%,更优选98至99.9wt%。
着色剂是影响颜色或改变某物的色调的任何物质(例如染料、颜料、油墨或漆料)。
固体着色剂是这样的固体组合物,其可以添加到销售点容器中,该容器的内部体积大部分(例如,容器体积的三分之二或更多)但是不完全已经被基础漆料填充了,以便改变这种基础漆料的色调或亮度,并且该组合物含有颜料或染料。
在根据本发明的固体着色剂中,所使用的颜料在性质上可以是无机或有机的,并且可以例如选自由各种金属形成的金属氧化物,例如由铝、锑、铋、硼、铬、钴、镓、铟、铁、镧、锂、镁、锰、钼、钕、镍、铌、硅、锡、钛、钒或锌形成的金属氧化物。应当理解,颜料组分还可以包含各种有机颜料的混合物或各种无机颜料的混合物或有机和无机颜料的混合物。
颜料组分可以包含一种或多种颜料。应当理解,也可以使用两种或更多种颜料的混合物。
颜料以细分散的形式存在。因此,它们的中值颗粒尺寸通常在0.01至5μm的范围内。
所使用的无机颜料可以是彩色、黑色和白色颜料(颜色颜料)以及光泽颜料。典型的有机颜料是彩色和黑色颜料。合适的有机颜料的实例是:单偶氮颜料:C.I.颜料棕25;C.I.颜料橙5,13,36,38,64和67;C.I.颜料红1,2,3,4,5,8,9,12,17,22,23,31,48:1,48:2,48:3,48:4,49,49:1,51:1,52:1,52:2,53,53:1,53:3,57:1,58:2,58:4,63,112,146,148,170,175,184,185,187,191:1,208,210,245,247和251;C.I.颜料黄1,3,62,65,73,74,97,120,151,154,168,181,183和191;C.I.颜料紫32;双偶氮颜料:C.I.颜料橙16,34,44和72;C.I.颜料黄12,13,14,16,17,81,83,106,113,126,127,155,174,176,180和188;双偶氮缩合颜料:C.I.颜料黄93,95和128;C.I.颜料红144,166,214,220,221,242和262;C.I.颜料棕23和41;二苯并芘二酮颜料:C.I.颜料红168;蒽醌颜料:C.I.颜料黄147,177和199;C.I.颜料紫31;蒽嘧啶(anthrapyrimidine)颜料:C.I.颜料黄108;喹吖啶酮(quinacridone)颜料:C.I.颜料橙48和49;C.I.颜料红122,202,206和209;C.I.颜料紫19;喹酞酮(quinophthalone)颜料:C.I.颜料黄138;二酮吡咯并吡咯(diketopyrrolopyrrole)颜料:C.I.颜料橙71,73和81;C.I.颜料红254,255,264,270和272;二恶嗪颜料:C.I.颜料紫23和37;C.I.颜料蓝80;黄烷士酮(flavanthrone)颜料:C.I.颜料黄24;阴丹酮(indanthrone)颜料:C.I.颜料蓝60和64;异吲哚啉颜料:C.I.颜料橙61和69;C.I.颜料红260;C.I.颜料黄139和185;异吲哚啉酮颜料:C.I.颜料黄109,110和173;异紫蒽酮(isoviolanthrone)颜料:C.I.颜料紫31;金属络合物颜料:C.I.颜料红257;C.I.颜料黄117,129,150,153和177;C.I.颜料绿8;芘酮(perinone)颜料:C.I.颜料橙43;C.I.颜料红194;苝(perylene)颜料:C.I.颜料黑31和32;C.I.颜料红123,149,178,179,190和224;C.I.颜料紫29;酞菁颜料:C.I.颜料蓝15,15:1,15:2,15:3,15:4,15:6和16;C.I.颜料绿7和36;皮蒽酮(pyranthrone)颜料:C.I.颜料橙51;C.I.颜料红216;吡唑并喹啉酮(pyrazoloquinazolone)颜料:C.I.颜料橙67;C.I.颜料红251;硫靛(thioindigo)颜料:C.I.颜料红88和181;C.I.颜料紫38;三芳基碳鎓颜料:C.I.颜料蓝1,61和62;C.I.颜料绿1;C.I.颜料红81,81:1和169;C.I.颜料紫1,2,3和27;C.I.颜料黑1(苯胺黑);C.I.颜料黄101(醛连氮黄(aldazine yellow));C.I.颜料棕22。合适的无机颜料的实例是:白色颜料:二氧化钛(C.I.颜料白6),锌白,颜料级氧化锌;硫化锌,锌钡白;黑色颜料:氧化铁黑(C.I.颜料黑11),铁锰黑,尖晶石黑(C.I.颜料黑27);炭黑(C.I.颜料黑7);彩色颜料:氧化铬,氧化铬水合物绿;铬绿(C.I.颜料绿48);钴绿(C.I.颜料绿50);群青绿;钴蓝(C.I.颜料蓝28和36;al.颜料蓝72);群青蓝;锰蓝;群青紫;钴紫和锰紫;红色氧化铁(C.I.颜料红101);硫硒化镉(C.I.颜料红108);硫化铈(C.I.颜料红265);钼酸红(C.I.颜料红104);群青红;棕色氧化铁(C.I.颜料棕6和7),混合棕,尖晶石相和刚玉相(C.I.颜料棕29,31,33,34,35,37,39和40),铬钛黄(C.I.颜料棕24),铬橙;硫化铈(C.I.颜料橙75);黄色氧化铁(C.I.颜料黄42);镍钛黄(C.I.颜料黄53;C.I.颜料黄157,158,159,160,161,162,163,164和189);铬钛黄;尖晶石相(C.I.颜料黄119);硫化镉和硫化镉锌(C.I.颜料黄37和35);铬黄(C.I.颜料黄34);钒酸铋(C.I.颜料黄184)。光泽颜料是具有单相或多相结构的片状颜料,其颜色范围通过干涉、反射和吸收现象的相互作用来标记。实例是铝片,具有一种或多种涂层(特别是金属氧化物)的铝、氧化铁和云母片。颜料优选选自氧化物/氢氧化物颜料、混合金属氧化物颜料、炭黑颜料、单偶氮、萘酚AS、苯并咪唑酮、异吲哚啉(酮)和多环颜料。
溶剂组分可以由一种或多种溶剂组成,所述溶剂优选是至少部分可混溶的。优选的溶剂是水、醇和二醇,例如乙二醇、丙二醇、二乙二醇,三乙二醇、更高级的二醇及其混合物。优选地,溶剂包含水。优选地,固体着色剂中的溶剂的量低,例如相对于固体着色剂的总重量小于5重量%,优选小于3重量%,更优选小于2.5重量%。
固体着色剂中的表面活性剂组分可以包含一种或多种表面活性剂。表面活性剂类型的选择尤其取决于颜料的选择和所需的颜色。表面活性剂是降低液体的表面张力、两种液体之间的界面张力或液体和固体之间的界面张力的化合物。在溶液中,这种行为被称为润湿,并且其结果是表面活性剂吸附到空气/水界面。表面活性剂可以充当洗涤剂、润湿剂、乳化剂、发泡剂和分散剂。表面活性剂被用于在漆料和其它应用的乳液聚合期间稳定聚合物颗粒的分散体。漆料的机械稳定性、冻融稳定性和保质期都通过添加表面活性剂来改善。特别地,有用的表面活性剂是非离子和/或阴离子的水溶性表面活性添加剂。特别合适的非离子表面活性剂是基于聚醚。除了未混合的聚氧化烯烃,优选C2-C4氧化烯烃和苯基取代的C2-C4氧化烯烃,具体是聚氧化乙烯、聚氧化丙烯和聚(苯基氧化乙烯)之外,特别地,嵌段共聚物,尤其具有聚氧化丙烯和聚氧化乙烯嵌段或聚(苯基氧化乙烯)和聚氧化乙烯嵌段的聚合物,以及这些氧化烯烃的无规共聚物是合适的。这些聚氧化烯烃可通过将氧化烯烃加成到起始分子(例如饱和或不饱和的脂族和芳族醇、饱和或不饱和的脂族和芳族胺、饱和或不饱和的脂族羧酸和羧酰胺、以及芳族羧酰胺和磺酰胺)上而获得。芳族起始分子可以被C1-C20烷基或C7-C30芳烷基取代。通常相对于每摩尔起始分子使用1至300摩尔、优选3至150摩尔的氧化烯烃,然而在芳族起始分子的情况下,氧化烯烃的量特别地在2至100摩尔的范围内,优选在5至50摩尔范围内,尤其在10至30摩尔范围内。加聚产物可以具有末端OH基团或封端的端基,例如为C1-C6烷基醚的形式。
合适的脂族醇通常包含6-26个碳原子,优选8-18个碳原子,并且可以具有无支链的、支链或环状结构。实例是辛醇、壬醇、癸醇、异癸醇、十一烷醇、十二烷醇、2-丁基辛醇、十三烷醇、异十三烷醇、十四烷醇、十五烷醇、十六烷醇(鲸蜡醇)、2-己基癸醇、十七烷醇、十八烷醇(硬脂醇)、2-庚基-十一烷醇、2-辛基癸醇、2-壬基十三烷醇、2-癸基十四烷醇、油醇和9-十八烯醇、以及这些醇的混合物,例如C8/C10、C13/C15和C16/C18醇,以及环戊醇和环己醇。特别感兴趣的是通过脂解和还原由天然原料获得的饱和和不饱和脂肪醇以及来自羰基合成法(oxo process)的合成脂肪醇。与这些醇的氧化烯烃加合物通常具有200至5000的平均分子量Mn。
上述芳族醇的实例不仅包括未取代的苯酚和α-萘酚和β-萘酚,而且还包括特别被C1-C12烷基、优选C4-C12烷基或C1-C4烷基取代的烷基取代产物,以及芳烷基取代产物,特别是C7-C30芳烷基取代的苯酚,例如己基苯酚、庚基苯酚、辛基苯酚、壬基苯酚、异壬基苯酚、十一烷基苯酚、十二烷基苯酚、二丁基苯酚、三丁基苯酚和二壬基苯酚,以及双酚A及其与苯乙烯的反应产物,特别是在两个OH基的邻位上被总共4个苯基-1-乙基取代的双酚A。
合适的脂族胺对应于上述脂族醇。此处特别重要的是饱和和不饱和的脂肪胺,其优选具有14至20个碳原子。芳族胺的实例是苯胺及其衍生物。有用的脂族羧酸尤其包括优选包含14至20个碳原子的饱和和不饱和脂肪酸以及完全氢化、部分氢化和未氢化的树脂酸以及多官能羧酸,例如二羧酸,例如马来酸。合适的羧酰胺衍生自这些羧酸。除了与单官能胺和醇的氧化烯烃加合物外,与至少双官能胺和醇的氧化烯烃加合物是非常特别感兴趣的。
至少双官能的胺优选具有2至5个胺基并且特别符合式H2N--(R1--NR2)n--H(R1:C2-C6亚烷基;R2:氢或C1-C6-烷基;n:1-5)。具体实例是:乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、1,3-丙二胺、二亚丙基三胺、3-氨基-1-亚乙基氨基丙烷、六亚甲基二胺、二亚己基三胺、1,6-双(3-氨基丙基氨基)己烷和N-甲基二亚丙基三胺,其中更优选六亚甲基二胺和二亚乙基三胺,最优选乙二胺。
这些胺优选首先与氧化丙烯反应,然后与氧化乙烯反应。嵌段共聚物的氧化乙烯含量通常为约10重量%至90重量%。基于多官能胺的嵌段共聚物的平均分子量Mn通常在1000至40000的范围内,优选在1500至30000的范围内。
所述至少双官能醇优选具有2-5个羟基。实例是C2-C6亚烷基二醇和相应的二亚烷基二醇和聚亚烷基二醇,例如乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,4-丁二醇、1,6-己二醇、二丙二醇和聚乙二醇、甘油和季戊四醇,其中更优选乙二醇和聚乙二醇,最优选丙二醇和二丙二醇。特别优选的与至少双官能醇的氧化烯烃加合物具有中心聚氧化丙烯嵌段,即其基于丙二醇或聚丙二醇,首先与另外的氧化丙烯反应,然后与氧化乙烯反应。嵌段共聚物的氧化乙烯含量通常在10重量%至90重量%的范围内。基于多元醇的嵌段共聚物的平均分子量Mn通常在1000至20000的范围内,优选在1000至15000的范围内。
这种非离子表面活性添加剂是已知的并且可以例如以下列商品名购得:和(BASF),Symperonic(Uniquema),EmulgatorWN和386(Lanxess)以及Rhodasurf、(Rhodia),Genopol(Clariant),Dowfax(Dow),Berol、Duomeen、Ethomeen(Akzo),Ethylan(Akcros)。
特别有用的水溶性阴离子表面活性剂的实例是基于烯属不饱和羧酸的聚合物的添加剂,基于聚氨酯的添加剂,基于上述聚醚的酸性磷酸酯、膦酸酯、硫酸酯和/或磺酸酯的添加剂,和基于芳族磺酸和甲醛的缩聚产物的添加剂。
应当理解,也可以使用多种添加剂的混合物,即,不仅是各种非离子添加剂的混合物,而且还可以是各种阴离子添加剂的混合物,以及非离子和阴离子添加剂的混合物。
特别地,基于不饱和羧酸的聚合物的有用的水溶性阴离子表面活性添加剂是选自烯属不饱和单羧酸和/或烯属不饱和二羧酸的均聚物和共聚物的添加剂,其各自可进一步包含不含酸官能团的互聚的乙烯基单体、这些均聚物和共聚物的烷氧基化物以及这些均聚物和共聚物及其烷氧基化物的盐。
作为含羧基单体和乙烯基单体的实例,可以提及:丙烯酸、甲基丙烯酸和巴豆酸;马来酸、马来酸酐、马来酸单酯、马来酸单酰胺、马来酸与二胺的反应产物,其可被氧化形成包含氧化胺基团的衍生物,和富马酸,其中马来酸、马来酸酐和马来酸单酰胺是优选的;乙烯基芳族化合物,例如苯乙烯、甲基苯乙烯和乙烯基甲苯;乙烯、丙烯、异丁烯、二异丁烯和丁二烯;乙烯基醚,例如聚乙二醇单乙烯基醚;直链或支链单羧酸的乙烯基酯,例如乙酸乙烯酯和丙酸乙烯酯;烯属不饱和单羧酸的烷基酯和芳基酯,特别是丙烯酸酯和甲基丙烯酸酯,例如丙烯酸甲酯、丙烯酸乙酯、丙烯酸丙酯、丙烯酸异丙酯、丙烯酸丁酯、丙烯酸戊酯、丙烯酸己酯、丙烯酸2-乙基己酯、丙烯酸壬酯、丙烯酸十二烷基酯、丙烯酸羟基乙酯、甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丙酯、甲基丙烯酸异丙酯、甲基丙烯酸丁酯、甲基丙烯酸戊酯、甲基丙烯酸己酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸壬酯、甲基丙烯酸十二烷基酯、甲基丙烯酸羟基乙酯以及丙烯酸苯酯、甲基丙烯酸苯酯、丙烯酸萘酯、甲基丙烯酸萘酯、丙烯酸苄酯、甲基丙烯酸苄酯;烯属不饱和二羧酸的二烷基酯,如马来酸二甲酯、马来酸二乙酯、马来酸二丙酯、马来酸二异丙酯、马来酸二丁酯、马来酸二戊酯、马来酸二己酯、马来酸二(2-乙基己酯)、马来酸二壬酯、马来酸二(十二烷基酯)、马来酸二(2-羟基乙酯)、富马酸二甲酯、富马酸二乙酯、富马酸二丙酯、富马酸二异丙酯、富马酸二丁酯、富马酸二戊酯、富马酸二己酯、富马酸二(2-乙基己酯)、富马酸二壬酯、富马酸二(十二烷基酯)、富马酸二(2-羟基乙酯);乙烯基吡咯烷酮;丙烯腈和甲基丙烯腈;其中苯乙烯、异丁烯、二异丁烯、丙烯酸酯和聚乙二醇单乙烯基醚是优选的。
特别地,聚丙烯酸被提及作为这些单体的优选均聚物的实例。
所提到的单体的共聚物可以由两种或更多种(特别是三种)不同的单体构成。共聚物可以是无规、交替、嵌段或接枝的。优选的共聚物是苯乙烯-丙烯酸、丙烯酸-马来酸、丙烯酸-甲基丙烯酸、丁二烯-丙烯酸、异丁烯-马来酸、二异丁烯-马来酸和苯乙烯-马来酸共聚物,它们可各自包含丙烯酸酯和/或马来酸酯作为额外的单体组分。
优选地,非烷氧基化的均聚物和共聚物的羧基全部或部分以盐的形式存在,以便可以确保在水中的溶解性。碱金属盐,例如钠盐和钾盐,以及铵盐是合适的。
非烷氧基化的聚合物添加剂通常具有在900-250000范围内的平均分子量Mw。当然,特别适合于单个聚合物的分子量范围取决于它们的组成。各种聚合物的分子量数据通过实例给出:聚丙烯酸:Mw为900至250000;苯乙烯-丙烯酸共聚物:Mw为1000至50000;丙烯酸-甲基丙烯酸共聚物:Mw为1000至250000;丙烯酸-马来酸共聚物:Mw为2000至70000。除了这些均聚物和共聚物本身之外,它们的烷氧基化物也特别感兴趣用作添加剂。特别地,这些烷氧基化物是通过与聚醚醇的部分(如果可能)到完全酯化而形成的聚合物。这些聚合物的酯化度通常在30至80摩尔%的范围内。
特别地,用于酯化的有用的聚醚醇是醇,例如乙醇、丙醇、异丙醇、丁醇;脂肪醇;聚醚醇本身,优选聚乙二醇和聚丙二醇,以及它们的单侧封端的衍生物,特别是相应的单醚,例如单芳基醚,诸如单苯基醚,特别是单-C1-C26烷基醚,例如用脂肪醇醚化的乙二醇和丙二醇;以及聚醚胺,所述聚醚胺可通过例如将相应的聚醚醇的端羟基转化或通过将氧化烯烃优选加聚在伯脂族胺上而制备。在此优选聚乙二醇、聚乙二醇单醚和聚醚胺。所使用的聚醚醇及其衍生物的平均分子量Mn通常在200至10000的范围内。
通过改变极性基团与非极性基团的比例,可以实现特定的表面活性性能。
这些阴离子表面活性添加剂同样是已知的并且可商购获得,例如以名称(BASF)、(Johnson Polymer)、(Alco)、(Rhodia)、(Goodrich)、(Avecia)、和(Rohm&Haas)、(Byk)以及(Degussa)。
包含在这些颜料制剂中的有用的阴离子表面活性添加剂还包括基于聚氨酯的添加剂。
为了本发明的目的,术语“聚氨酯”不仅仅包括多官能异氰酸酯与含异氰酸酯反应性羟基的有机化合物的纯反应产物,而且还包括在通过加入另外的异氰酸酯反应性化合物(实例是带有伯氨基或仲氨基的羧酸)额外官能化之后的这些反应产物。这些添加剂由于其低离子电导率和与其它表面活性添加剂相比的中性pH值而著称。特别地,用于制备添加剂的有用的多官能异氰酸酯是二异氰酸酯,但是也可以使用具有三个或四个异氰酸酯基团的化合物。可以使用芳族和脂族异氰酸酯。
优选的二异氰酸酯和三异氰酸酯的实例是:2,4-甲苯二异氰酸酯(2,4-TDI)、4,4′-二苯基甲烷二异氰酸酯(4,4′-MDI)、对二甲苯二异氰酸酯、1,4-二异氰酸根合苯、四甲基二甲苯二异氰酸酯(TMXDI)、2,4′-二苯基-甲烷二异氰酸酯(2,4′-MDI)和三异氰酸根合甲苯以及异佛尔酮二异氰酸酯(IPDI)、2-丁基-2-乙基五亚甲基二异氰酸酯、四亚甲基二异氰酸酯、六亚甲基二异氰酸酯、十二亚甲基二异氰酸酯、2,2-双(4-异氰酸根合环己基)丙烷、三甲基己烷二异氰酸酯、2-异氰酸根合丙基环己基异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯、2,2,4-三甲基六亚甲基二异氰酸酯、2,4’-亚甲基双(环己基)二异氰酸酯、顺式-环己烷-1,4-二异氰酸酯、反式-环己烷-1,4-二异氰酸酯和4-甲基环己烷-1,3-二异氰酸酯(H-TDI)。
应当理解,也可以使用异氰酸酯的混合物。例如可以通过实例的方式提及:2,4-甲苯二异氰酸酯和三异氰酸根合甲苯的结构异构体的混合物,实例是80mol%的2,4-甲苯二异氰酸酯和20mol%的2,6-甲苯二异氰酸酯的混合物;顺式-和反式-环己烷-1,4-二异氰酸酯的混合物;2,4-或2,6-甲苯二异氰酸酯与脂族二异氰酸酯的混合物,例如六亚甲基二异氰酸酯和异佛尔酮二异氰酸酯。
有用的异氰酸酯反应性有机化合物优选包括每分子具有至少两个异氰酸酯反应性羟基的化合物。然而,可用的化合物进一步包括每分子仅具有一个异氰酸酯反应性羟基的化合物。在与多异氰酸酯的反应中,这些单官能化的化合物可以部分或全部替代每分子包含至少两个异氰酸酯反应性羟基的化合物。
现在将列举特别优选的每分子具有至少两个异氰酸酯反应性羟基的异氰酸酯反应性化合物的实例。它们是每分子具有平均至少两个羟基的聚醚二醇、聚酯二醇、基于内酯的聚酯二醇、至多12个碳原子的二醇和三醇、二羟基羧酸、二羟基磺酸、二羟基膦酸、聚碳酸酯二醇、聚羟基烯烃和聚硅氧烷。
有用的聚醚二醇包括例如C2-C4氧化烯烃(例如氧化乙烯、氧化丙烯和氧化丁烯)、四氢呋喃、氧化苯乙烯和/或表氯醇的均聚物和共聚物,其在合适的催化剂(实例为三氟化硼)存在下可获得。其它有用的聚醚二醇可通过在具有至少两个酸性氢原子的起始物的存在下使这些化合物(共)聚合而获得,起始物的实例是水、乙二醇、硫代乙二醇(thioglycol)、巯基乙醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、1,12-十二烷二醇、乙二胺、苯胺或1,2-二-(4-羟基苯基)丙烷。
特别合适的聚醚二醇的实例是聚乙二醇、聚丙二醇、聚丁二醇和聚四氢呋喃及其共聚物。聚醚二醇的分子量Mn优选在250-5000的范围内,更优选在500-2500的范围内。可用的异氰酸酯反应性化合物还包括常见的聚酯二醇(羟基聚酯)。
优选的聚酯二醇是二醇与二羧酸或其反应性衍生物(实例是酸酐或二甲酯)的反应产物。有用的二羧酸包括饱和的和不饱和的脂族和芳族二羧酸,其可带有另外的取代基,例如卤素。优选的脂族二羧酸是包含3至22个、特别地4至12个碳原子的饱和的无支链的α,ω-二羧酸。
特别合适的二羧酸的实例是琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、1,12-十二烷二羧酸、马来酸、马来酸酐、富马酸、衣康酸、邻苯二甲酸、间苯二甲酸、邻苯二甲酸酐、四氢邻苯二甲酸酐、六氢邻苯二甲酸酐、四氯邻苯二甲酸酐、内亚甲基四氢邻苯二甲酸酐、对苯二甲酸,对苯二甲酸二甲酯和间苯二甲酸二甲酯。
有用的二醇特别包括饱和的和不饱和的脂族和脂环族二醇。特别优选的脂族α,ω-二醇是无支链的并且具有2至12个、特别地2至8个、具体地2至4个碳原子。优选的脂环族二醇衍生自环己烷。
特别合适的二醇的实例是:乙二醇、丙二醇、1,3-丙二醇、1,4-丁二醇、2-甲基丙烷-1,3-二醇、1,5-戊二醇,新戊二醇,1,6-己二醇、1,8-辛二醇、1,10-癸二醇、1,12-十二烷二醇、顺式-丁-2-烯-1,4-二醇、反式-丁-2-烯-1,4-二醇、2-丁炔-1,4-二醇、顺式-1,4-二(羟甲基)-环己烷和反式-1,4-二(羟甲基)环己烷。聚酯二醇的分子量Mn优选在300至5000的范围内。特别地,可用作异氰酸酯反应性化合物的基于内酯的聚酯二醇是基于具有4至22个、优选4至8个碳原子的脂族饱和无支链的ω-羟基羧酸。还可以使用支化的ω-羟基羧酸,其中亚烷基链中的一个或多个-CH2-基团被-CH(C1-C4-烷基)-代替。
优选的ω-羟基羧酸的实例是γ-羟基丁酸和δ-羟基戊酸。应当理解,上述二醇可以同样用作异氰酸酯反应性化合物,在这种情况下,可以采用与上述相同的优选方案。
三醇,特别是具有3-12个碳原子的三醇,并且具体是具有3-8个碳原子的三醇同样可用作异氰酸酯反应性化合物。三羟甲基丙烷是特别合适的三醇的实例。特别地,用作异氰酸酯反应性化合物的二羟基羧酸是优选包含4至14个碳原子的脂族饱和二羟基羧酸。二羟甲基丙酸(DMPA)是这些二羟基羧酸的特别优选的实例。
有用的异氰酸酯反应性化合物还包括相应的二羟基磺酸和二羟基膦酸,例如2,3-二羟基丙烷膦酸。如本文所用的二羟基羧酸还应包含含有多于一个羧基官能团(或视情况而定可为酸酐或酯官能团)的化合物。这样的化合物可以通过二羟基化合物与四羧酸二酐(例如均苯四甲酸二酐或环戊烷四羧酸二酐)在聚加成反应中以2∶1至1.05∶1的摩尔比反应而获得,并且优选具有在500至10000范围内的平均分子量Mn。
有用的聚碳酸酯二醇的实例是光气与过量二醇(特别地具有2至12、特别地2至8个、具体地2至4个碳原子的无支链饱和脂族α,ω-二醇)的反应产物。
特别地,可用作异氰酸酯反应性化合物的聚羟基烯烃是α,ω-二羟基烯烃,并且优选α,ω-二羟基丁二烯。
此外,可用作异氰酸酯反应性化合物的聚硅氧烷每分子包含平均至少两个羟基。特别合适的聚硅氧烷包含平均5-200个硅原子(数均),特别地被C1-C12烷基,特别是被甲基取代。
特别地,仅包含一个异氰酸酯反应性羟基的异氰酸酯反应性化合物的实例是脂族、脂环族、芳脂族或芳族单羟基羧酸和单羟基磺酸。
在这方面,除了上述异氰酸酯反应性化合物之外,可以加入具有异氰酸酯反应性基团的其它化合物,例如二硫醇、硫醇(例如硫代乙醇)、氨基醇(例如乙醇胺和N-甲基乙醇胺)或二胺(例如乙二胺),从而制备除氨基甲酸酯基团外还额外带有异氰脲酸酯基团、脲基甲酸酯基团、脲基团、缩二脲基团、脲二酮基团或碳二亚胺基团的聚氨酯。这种异氰酸酯反应性化合物的其它实例是具有至少两个伯氨基和/或仲氨基的脂族、脂环族、芳脂族或芳族羧酸和磺酸。
应当理解,也可以加入仅具有一个异氰酸酯反应性基团的相应化合物,实例是一元醇、伯单胺和仲单胺、单氨基羧酸和磺酸以及硫醇。通常用量高达10mol%,基于。
优选地,反应产物的一些或所有羧基为盐形式,以便确保在水中的溶解度。可用的盐包括例如碱金属盐(例如钠盐和钾盐)和铵盐。通常,添加剂的平均分子量Mw在500-250000的范围内。
通过改变极性基团与非极性基团的比例,可以实现添加剂的特定表面活性性能。这种阴离子表面活性添加剂是已知的且可商购获得,例如以名称Borchi GEN SN95(Borchers)。
特别地,基于聚醚的酸性磷酸、膦酸、硫酸和/或磺酸酯的水溶性阴离子表面活性添加剂一方面是基于上述聚醚与磷酸、五氧化二磷和膦酸的反应产物,另一方面是基于上述聚醚与硫酸和磺酸的反应产物。在反应中,聚醚一方面转化为相应的磷酸单酯或二酯和膦酸酯,另一方面转化为硫酸单酯和磺酸酯。这些酸性酯优选以水溶性盐的形式存在,特别地作为碱金属盐(具体是钠盐)和铵盐,但也可以以游离酸的形式使用。
优选的磷酸盐和膦酸盐尤其衍生自烷氧基化的,特别是乙氧基化的脂肪和羰基合成醇、烷基酚、脂肪胺、脂肪酸和树脂酸,并且优选的硫酸盐和磺酸盐特别是基于烷氧基化的,特别是乙氧基化的脂肪醇、烷基酚和胺(包括多官能胺,例如六亚甲基二胺)。这种阴离子表面活性添加剂是已知的并且可以例如以名称(BASF)、(BASF)、(Croda)、(Rhodia)、(BASF)、(Cognis)、(Albright&Wilson)、(ICI)、(Rhodia)和(BASF)商购。
基于芳族磺酸和甲醛的水溶性阴离子添加剂特别地基于萘磺酸,并且同样优选以盐形式,特别是作为钠盐使用。它们的平均分子量Mw通常在4000至15000的范围内。添加剂同样是已知的,并且例如可以以名称(BASF)商购。
相对于固体着色剂的总重量,表面活性剂的量为3至40重量%,优选5至30重量%,更优选10至25重量%。
固体着色剂可以包含一种或多种添加剂。添加剂类型的选择可以取决于颜料的选择以及期望的颜色。用于本发明的固体着色剂中的添加剂可以是例如消泡剂、粘合剂、杀生物剂、UV稳定剂、湿润剂、pH稳定剂、流变改性剂、干燥剂,粘附促进剂、抗氧化剂、缓冲剂、聚结剂、增量剂、流平剂、中和剂、荧光增白剂、珠光剂、增塑剂、聚合物添加剂、防腐剂、反应性稀释剂、增稠剂、增粘剂和蜡。添加剂可以以至多10重量%,优选0.1-5重量%的量存在。
可存在于固体着色剂中的添加剂之一是抗氧化剂。合适的抗氧化剂的实例包括众所周知的空间位阻酚类、芳族胺类、硫代增效剂类、亚磷酸酯和亚膦酸酯类以及空间位阻胺类。基于空间位阻酚的抗氧化剂包含作为必要结构单元的被至少一个叔丁基邻位取代(特别是在相对于OH基团的两个邻位被叔丁基取代)的苯酚。大多数已知的产品包含多个这些结构单元,其通过各种桥接成员彼此结合。基于芳族胺的抗氧化剂主要是二芳基胺、胺-酮缩合产物(例如苯胺-丙酮缩合物)和取代的对苯二胺。硫代增效剂的实例是二烷基二硫代氨基甲酸的金属盐、二烷基二硫代磷酸锌和硫代二丙酸的酯(特别是二月桂基、二肉豆蔻基和二硬脂基酯)。基于亚磷酸酯和亚膦酸酯的抗氧化剂通常是磷的相应的酸与烷基取代的(特别是叔丁基取代的)酚的酯。基于空间位阻胺(HALS)的抗氧化剂包含2,6-二烷基取代的(特别是2,6-二甲基取代的)哌啶作为必要结构单元,其在4位通过大范围的桥连成员与另外的哌啶结构单元连接。抗氧化剂是通常已知的并且可以例如以名称和(Ciba)、(ICI)、(Clariant)和(Goodyear)获得。当液体颜料分散体包含抗氧化剂时,基于液体颜料分散体的总重量,抗氧化剂含量通常为0.1重量%至5重量%,优选0.1重量%至2重量%。
优选地,液体颜料分散体还可以包含消泡剂。消泡剂是在着色剂加工过程中减少和阻碍泡沫形成的化学添加剂。消泡剂的实例是不溶性油、聚二甲基硅氧烷、聚醚硅氧烷共聚物和其它硅酮、某些醇、硬脂酸酯和二醇。可商购的消泡剂例如来自Tego、Byk或Borchers。相对于液体颜料分散体的总重量,消泡剂的量在0.1和2重量%之间,优选在0.1和1重量%之间,更优选在0.1和0.5重量%之间。
液体颜料分散体可以包含少量的杀生物剂(相对于液体颜料分散体的总重量,在0.01和0.5重量%之间)。杀生物剂可以加入到液体颜料分散体中以保护它们免受生物侵染和生长。
根据本发明的固体着色剂可以包含无色填料。填料通常不溶于溶剂,并且特别地选自以下化学类别(作为实例列举,不仅是天然来源的产物,而且还包括合成来源的产物):氧化物和氢氧化物:天然的:氧化铝和氧化镁;合成的:氢氧化铝和氢氧化镁;二氧化硅和硅酸盐:天然的:石英、方英石、硅藻土(kieselguhr)、滑石、高岭土、硅藻土(diatomaceousearth)、云母、硅灰石和长石;合成的:热解法二氧化硅、沉淀二氧化硅、铝硅酸盐和煅烧硅铝酸盐;碳酸盐:天然的:钙和镁的碳酸盐,例如方解石、白垩、白云石和菱镁矿;合成的:沉淀碳酸钙;硫酸盐:天然的:钡和钙的硫酸盐,如重晶石和石膏;合成的:沉淀硫酸钡。无色填料的量为0至60重量%。在一个实施方式中,相对于固体着色剂的总重量,无色填料的量为5至40重量%。
根据本发明的固体着色剂可以包含粘合剂。粘合剂可以是聚合物粘合剂,包括胶乳聚合物和溶液聚合物。示例性的粘合剂包括但不限于:丙烯酸类共聚物、苯乙烯/丙烯酸类共聚物、乙酸乙烯酯共聚物、乙酸乙烯酯/丙烯酸类共聚物、叔碳酸乙烯酯/丙烯酸类共聚物、乙烯/乙酸乙烯酯共聚物、苯乙烯/丁二烯共聚物、聚酯、干性油改性的聚合物(如聚酯和聚氨酯)、聚酰胺、环氧酯、聚脲、聚氨酯、聚硅氧烷、硅酮、氟化共聚物(如偏二氟乙烯)以及任何上述聚合物粘合剂的共混物。基础漆料、染色剂或着色剂可包含用于粘合剂的多组分(例如,双组分)反应性体系的一种或多种组分,例如异氰酸酯-多胺、异氰酸酯-多元醇、环氧-多胺、碳二亚胺-多元酸、氮丙啶-多元酸、三聚氰胺-多元醇或脲甲醛-多元醇体系的组分。粘合剂的量相对于固体着色剂的总重量为0至15重量%,或例如1至10重量%,或3至7重量%。聚合物粘合剂的玻璃化转变温度可以例如为约-20至约+60℃。
本发明还涉及可用于制备根据本发明的固体着色剂的液体颜料分散体。所述液体颜料分散体包含:
a)15-75重量%的颜料;
b)20-70重量%的溶剂;
c)5-30wt%的表面活性剂;
其中所述wt%是相对于所述液体颜料分散体的总重量。
在优选的实施方式中,液体颜料分散体包含:
a)50-75重量%的颜料;
b)25-60wt%的溶剂;
c)5-20wt%的表面活性剂;
d)0-30wt%的无色填料;
e)0.1-5wt%的添加剂;
其中所述wt%是相对于所述液体颜料分散体的总重量。
颜料、溶剂、表面活性剂、无色填料和添加剂如上文对固体着色剂所定义。
本发明还涉及制备固体着色剂的方法。制备根据本发明的固体着色剂的方法包括以下步骤:
a)提供含有至少颜料、溶剂和表面活性剂的液体颜料分散体;
b)喷射液体颜料分散体以获得液体颜料分散体的液滴;
c)冷冻液体颜料分散体的液滴以获得经冷冻的着色剂;
d)冷冻干燥经冷冻的着色剂以获得固体着色剂。
优选地,在步骤b)中制备的液滴尺寸一致。优选地,在步骤c)中,在单个液滴之间可以发生接触之前冷冻液滴,以便防止液滴凝聚。优选地,溶剂是水。
液体颜料分散体的喷射可以通过任何方式进行。喷涂通常通过使用喷嘴进行。在喷嘴中,液体颜料分散体被雾化,将液体颜料分散体分散成液滴。喷嘴可以具有一个或多个出口。喷嘴的实例是单流体喷嘴、双流体喷嘴、振动喷嘴、旋转雾化器和超声波雾化器。喷射优选通过使用振动喷嘴进行。振动喷嘴具有在0.1-0.4mm之间、优选在0.15和0.35mm之间、更优选在0.18和0.32mm之间的喷嘴直径。振动通常以介于100和5000Hz之间的频率、优选地介于200和2000Hz之间的频率、更优选地介于500和1200Hz之间的频率发生。
优选地,喷射提供均匀的液滴。液滴尺寸例如在100和5000μm之间,优选在400和1400μm之间,更优选在500和1300μm之间或在600和1000μm之间。
液体分散体的液滴优选在它们可以彼此接触并再次开始凝聚之前被冷冻。为了此目的,优选快速冷却步骤,其允许单个液滴固化并防止单个液滴的凝聚。快速冷却优选用低温气体进行。空气可以用冷却器、液体二氧化碳或其它方式冷却。低温气体优选具有在-10和-200℃之间、更优选地在-60至-150℃之间、或在-50至-100℃之间的温度。优选使用温度在-10和-200℃之间、更优选在-50和-100℃之间的冷却氮气流作为冷却介质,以快速冷冻各个液滴。
经冷冻的液体分散液滴被冷冻干燥以从液滴中除去大部分溶剂。通过冷冻干燥,溶剂从液滴中升华,导致颗粒的开孔结构。在冷冻步骤中,使液体分散液滴达到-10℃和-200℃之间,优选-50℃和-100℃之间的温度。当液体分散体的液滴在喷射后通过直接优选与冷冻气体接触而冷冻时,该冷冻步骤等同于冷冻干燥中的预冷冻步骤。当液滴以另一种方式冷冻时,可能需要预冷冻阶段以使经冷冻的着色剂达到合适的温度以开始初级干燥阶段。
冷冻干燥在低于大气压(真空)下进行。该压力通常低于6毫巴,优选低于1毫巴,更优选低于0.1毫巴。冷冻干燥过程中的温度通常为<30℃。
本发明涉及固体着色剂用于给漆料组合物调色的用途。
本发明还涉及一种用于给基础漆料组合物着色的系统,其包含:
a)至少一种基础漆料组合物,其被包装在体积为约0.2至20L且配备有用于开口的可开启和可再封闭的盖子、盖或其它封闭物的容器中,通过所述开口着色剂可从自动或手动着色剂分配器分配到入基础漆料组合物中;和
b)被包装在体积为0.5至5升且具有着色剂分配器的的容器中的着色剂系列,着色剂可从所述着色剂分配器被分配到基础涂料组合物中,
其中所述着色剂是固体着色剂,并且以体积方式进行固体着色剂的分配。
优选地,固体着色剂的比例S/A[颗粒尺寸分布的标准偏差/平均颗粒尺寸]<25%,优选<22%,且更优选<20%。优选地,固体着色剂的平均颗粒尺寸在400μm和1400μm之间,优选在500μm和1300μm之间,更优选在600μm和1000μm之间。体积计量是预定体积的固体着色剂的计量。预定体积可以通过测量着色剂分配器中固体着色剂的初始体积,然后计量固体着色剂直到达到终止体积来计量,其中预定体积是初始体积和终止体积之间的差。或者,当着色剂分配器每次计量恒定或已知体积时,可以确定分配某个预定体积所需的时间。
附图:
图1涉及通过喷雾干燥方法制备的颗粒的颗粒尺寸分布的实例。
图2涉及通过根据本发明的方法制备的颗粒。
图3示出了用于固体颜料颗粒的体积计量的测试设备。测试设备包括容器1(其具有用于排出固体颗粒的开口2)、柱塞3(其能够上下移动以打开或关闭容器1的开口2以便释放固体颗粒4)。
实施例
已经准备了许多实施例来说明本发明。用于制备固体着色剂(SC)的液体颜料分散体(LPD)的组成概括在表1中
表1:所用材料的列表和配方
LPD=液体颜料分散体
SC=固体着色剂
实验1:液体颜料分散体的制备
在配方(表1)中给出了制备液体颜料分散体所需的原料量。首先,使用天平将液体称重到10升容器中。将容器置于高剪切溶解器下。使用药匙缓慢加入固体材料(预先在罐中称重的量)。应当调节溶解器的剪切,使得在添加固体期间在所有时间可见涡流。在加入所有固体之后,在Stormer流变仪上测量粘度,并且在研磨阶段(通常在70和120Krebs单位(KU)之间)之前通过加入水调节粘度。将分散体在珠磨机上研磨直至粒度通常<15μm。颗粒尺寸的测量使用Hegman量规(根据SFS-ISO 1524)进行。测量粘度、颜色强度和色调(根据CIE lab),并将液体颜料分散体稀释至所需的粘度和颜色标准。
表2:液体颜料分散体的测量
实验2:通过对比方法A制备固体着色剂
通过喷雾干燥制备固体着色剂:
(a)借助于单料喷嘴来雾化悬浮液,这在喷雾塔中进行;
(b)使步骤(a)中产生的液滴与空气接触以将其干燥,得到具有给定残留水分含量的颗粒。喷雾塔中的气体入口温度为165℃。气体出口温度为70℃。
(c)从气流中分离颗粒。
形成具有大颗粒尺寸分布和低孔隙率(BET值通常≤15m2/g,具体地≤10m2/g)的不规则颗粒。S/A通常在40和60之间的范围(参见表4)。
实验3:通过方法B制备固体着色剂
使用振动喷嘴形成液体颜料分散体的液滴,其在含有冷冻氮气流(与颗粒逆流)的管中被立即冷却,所述冷冻氮气流的温度在约-78℃至-70℃之间。将经冷冻的液滴收集在容器中并在冷冻干燥器(压力为0.1mbar且温度为25℃)中冷冻干燥。
振动喷嘴的直径优选为0.3mm。典型使用的频率为500Hz,振幅为400mV,压力为110毫巴。获得了界限清楚的固体着色剂颗粒,其具有窄的颗粒尺寸分布,S/A在5和20之间(参见表4)。
实验4:由于球体的颗粒尺寸导致溶解度的差异
为了在实践中使用固体着色剂,在漆料中形成全色强度的最大摇晃时间(使用漆料摇动器)为2分钟。球的尺寸可能对固体着色剂的溶解度有影响。
根据实验1,使用表1(第3列)中给出的配方,制备氧化物黄色颜料的液体颜料分散体。使用如实验3中所述的方法B从该液体颜料分散体制备了固体着色剂,得到具有表1(第4栏)中给出的配方的固体着色剂。根据振动喷嘴的尺寸,已经获得了不同的级分。
固体着色剂已经使用具有不同网目的筛子分成具有不同颗粒尺寸(0-250、250-500、500-710、710-1000、1000-1400、1400-2000μm)的级分。
对于每个级分中,在120ml塑料罐(高度70mm,直径50mm)中将1.3克加入到100克丙烯酸类白漆中。将这些混合物在振动的漆料摇动器(例如来自Corob的Vibro ST)中摇晃不同时间(t=1、2、3、4、5和6分钟)。在每次摇晃时间后,打开样品,取出一部分漆料,使用150μm的块涂布器在黑白卡上进行涂刮。
使用分光光度计测量所有样品的颜色强度(根据LAB颜色空间在Z轴上测量)。将具有最小颗粒尺寸(0-250μm)并且摇动6分钟的样品用作标准。所有其它样品已经根据该标准测量。测量标准品和样品之间的颜色强度,并且差异以%表示在表2中。当标准品和样品之间的颜色强度差异<2%时,认为颗粒溶解。
表3:不同颗粒尺寸下的颜色强度发展
球体的颗粒尺寸对球体在涂料中的溶解度有影响。最大球体的粒度应小于1400μm以防止颗粒尺寸影响在2分钟的所需最大摇晃时间内球体在涂料中的溶解度。
实验5:由于所用的生产固体着色剂的方法导致的PSD差异
分配器或具体地定量给料单元的精确体积计量的重要因素是粉末颗粒尺寸的变化。
为了测定颗粒尺寸和颗粒分布,使用了OCCHIO ZEPHYR ESR分析仪。分析仪给出颗粒尺寸从20μm到30mm的自由流动粉末的精确尺寸和形状分析。OCCHIO ZEPHYR ESR分析仪根据ISO 13322-1静态图像分析第一版2004-12-01标准来工作。
将每个样品送到振动进料器,在那里将样品被输送到倾卸轴,以获得样品在OCCHIO ZEPHYR ESR分析仪中的重力分散。此后,相机对焦点中的所有颗粒拍摄图片。对于每个样品,分析50000个颗粒的颗粒尺寸。使用CALLISTO软件进行统计学评价。
根据实验1,使用表1中给出的配方(第3、5、7和9列)制备氧化物黄、蓝、绿和红颜料的液体颜料分散体。使用如实验2和3中所述的方法A和方法B,由该液体颜料分散体来制备固体着色剂,得到具有如表1(第4、6、8和10栏)中给出的配方的固体着色剂。
在表4中给出了PSD测量结果的总结。最小-最大值和因子S/A[颗粒尺寸分布的标准偏差/平均粒度](%)是固体着色剂的尺寸和分布均匀性的量度,其是流动性的重要指标。为了球体的最佳体积分配,需要完美的流动性。图1和图2是使用不同的方法产生球体的PSD的差异的实例。
结果表明,与方法B的固体着色剂球体相比,方法A的固体着色剂球体的尺寸相对非常小。此外,方法B的球体显示出比方法A的球体小得多的尺寸变化。在方法B的球体中看到的尺寸均匀性(S/A<25%,优选<20%)是这些球体的优异流动能力的重要指标。
表4:用于不同类型的球体和固体着色剂的球形着色剂(ISO直径)数据
实验6:固体着色剂的体积计量的测试
构建用于测试固体颗粒的体积计量的测试装置。该装置示意性地示于图3中。测试单元包含容器或容纳器1,其具有用于计量固体颗粒的开口2。开口可以通过可上下移动的柱塞3打开或关闭。在柱塞打开的时间内,一定体积的固体着色剂将通过重力计量。
已经使用如图3所示的装置测试了两个样品的体积计量。
已使用了以下的测试方法:
柱塞向下移动,这意味着计量单元关闭。容器1部分地填充有固体球体。柱塞向上移动,这开始在一个确定的时间内对通过开口2的固体着色剂计量。柱塞再次向下移动以关闭计量单元。球体的量通过重量测量,使用振实密度来确定体积。
在第一测试中,漏斗填充有用生产方法B(参见实验5,表4)生产的氧化物黄PY42。颗粒尺寸范围在593-1375μm之间,具有窄的颗粒尺寸分布(S/A为14%)。柱塞关闭时,没有颗粒泄漏。当填充漏斗时,样品看起来是均匀的;在样品的顶部和底部之间没有观察到颗粒尺寸的差异。
在第二(比较)测试中,漏斗填充有用生产方法A(参见实验5,表4)生产的氧化物黄PY42固体球。颗粒尺寸范围在22.5-645μm之间,S/A为40%,这意味着颗粒尺寸分布非常宽。甚至当柱塞3关闭时,小颗粒的部分开始通过柱塞3和开口2之间的(小)开口下落。
由于小颗粒的泄漏和容器1中颗粒的不均匀性,颗粒的计量不准确且不可靠。此外,注意到在填充漏斗期间,较大的颗粒到达表面,而较小的颗粒移动到底部。预期这将导致体积计量的不准确。
从上述测试可以得出结论,需要小的颗粒尺寸分布用于精确的体积计量。当固体着色剂的颗粒尺寸太小时,体积计量变得不可能。
Claims (14)
1.一种固体着色剂,其包含:
a.30-97重量%的颜料;
b.小于5重量%的溶剂;
c.3-40重量%的表面活性剂;
并且其中所述固体着色剂的比例S/A[颗粒尺寸分布的标准偏差/平均颗粒尺寸]<25%,优选<22%,且更优选<20%,其中重量%是相对于所述固体着色剂的总重量,并且其中所述颗粒尺寸分布是通过使用OCCHIOZEPHYR ESR分析仪根据ISO 13322-1静态图像分析第一版2004-12-01采用全自动图像分析的光散射测定的。
2.根据权利要求1的固体着色剂,其中所述平均颗粒尺寸在400μm和1400μm之间,优选在500μm和1300μm之间,更优选在600μm和1000μm之间。
3.根据权利要求1的固体着色剂,其中所述着色剂包含:
a.50-95重量%的颜料;
b.小于3重量%的溶剂;
c.5-30重量%的表面活性剂;
d.0.1-5重量%的添加剂;
e.0-20重量%的无色填料;
f.0-10重量%的粘合剂;
其中所述固体着色剂的比例S/A[颗粒尺寸分布的标准偏差/平均颗粒尺寸]<25%,优选<22%,且更优选<20%,其中所述固体着色剂的平均颗粒尺寸在400μm和1400μm之间,优选在500μm和1300μm之间,更优选在600μm和1000μm之间,并且其中重量%是相对于所述固体着色剂的总重量。
4.根据权利要求1-3中任意一项的固体着色剂,其中基于固体着色剂的总重量,所述着色剂包含0.1重量%至5重量%、优选0.1重量%至2重量%的抗氧化剂。
5.根据权利要求1-4中任意一项的固体着色剂,其中所述着色剂包含0.1重量%至2重量%、优选0.1重量%至1重量%、更优选0.1重量%至0.5重量%的量的消泡剂。
6.一种用于制备根据权利要求1-5中任意一项的固体着色剂的方法,其中所述方法包括以下步骤:
a)提供含有至少颜料、溶剂和表面活性剂的液体颜料分散体;
b)喷射所述液体颜料分散体以获得液体颜料分散体的液滴;
c)通过温度在-10℃和-200℃之间、更优选在-50℃和-100℃之间的冷却气流来冷冻所述液体颜料分散体的液滴,以获得经冷冻的着色剂;
d)冷冻干燥经冷冻的着色剂以获得固体着色剂。
7.根据权利要求6的方法,其中,基于所述液体分散体的总重量,所述液体分散体包含50到95重量%的固体。
8.根据权利要求6或7的方法,其中所述喷射是通过振动喷嘴进行的。
9.根据权利要求6-8中任意一项的方法,其中喷射是使用喷嘴直径在0.1mm和0.4mm之间的振动喷嘴来进行的。
10.根据权利要求7-9中任意一项的方法,其中所述振动喷嘴以200到2000Hz的振动来运行。
11.根据权利要求1-5中任意一项的固体着色剂用于给漆料组合物调色的用途。
12.根据权利要求11的用途,其中固体着色剂的计量是以体积方式进行的。
13.漆料组合物,其包含根据权利要求1-5中任意一项的固体着色剂或根据权利要求6-10中任意一项的方法来制备的固体着色剂。
14.一种用于给基础漆料组合物着色的系统,其包含:
a)至少一种浅色的基础漆料组合物,其被包装在体积为约0.2L至20L且配备有用于开口的可开启和可再封闭的盖子、盖或其它封闭物的容器中,通过所述开口着色剂可从自动或手动着色剂分配器分配到基础漆料组合物中;和
b)着色剂系列,其被包装在体积为0.5升至5升且具有着色剂分配器的容器中,着色剂可从所述着色剂分配器被分配到基础涂料组合物中,
其中所述着色剂是如权利要求1-5中任意一项所定义的固体着色剂,并且以体积方式进行固体着色剂的分配。
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CN109306213A (zh) * | 2017-07-28 | 2019-02-05 | Swimc有限公司 | 使用粉末状着色剂对水性和溶剂型漆料和色料进行调色 |
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CN113597541B (zh) * | 2019-03-08 | 2024-01-16 | 克罗玛夫洛技术公司 | 固体着色剂分配装置和包括该装置的着色机 |
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AU2015254616B2 (en) | 2018-12-06 |
AU2015254616A1 (en) | 2016-12-08 |
WO2015165994A3 (en) | 2016-02-04 |
US20170051151A1 (en) | 2017-02-23 |
ES2821815T3 (es) | 2021-04-27 |
CN106661341B (zh) | 2020-08-04 |
US10308811B2 (en) | 2019-06-04 |
EP3137559B1 (en) | 2020-07-22 |
CA2947449C (en) | 2021-06-15 |
PL3137559T3 (pl) | 2021-02-08 |
EP3137559A2 (en) | 2017-03-08 |
WO2015165994A2 (en) | 2015-11-05 |
CA2947449A1 (en) | 2015-11-05 |
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