CN1167786A - 用于生产压块和压制的粒状材料的方法及其应用 - Google Patents
用于生产压块和压制的粒状材料的方法及其应用 Download PDFInfo
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- CN1167786A CN1167786A CN97111205A CN97111205A CN1167786A CN 1167786 A CN1167786 A CN 1167786A CN 97111205 A CN97111205 A CN 97111205A CN 97111205 A CN97111205 A CN 97111205A CN 1167786 A CN1167786 A CN 1167786A
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Classifications
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
- C04B18/028—Agglomerated materials, e.g. artificial aggregates temporarily agglomerated, e.g. agglomerates which fall apart during mixing with the other mortar or concrete ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
- C04B18/022—Agglomerated materials, e.g. artificial aggregates agglomerated by an organic binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/22—Compounds of iron
- C09C1/24—Oxides of iron
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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
- C09C1/34—Compounds of chromium
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C09C1/346—Chromium oxides
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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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- C09C1/3638—Agglomeration, granulation, pelleting
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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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- C—CHEMISTRY; METALLURGY
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
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- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/046—Densifying, degassing, packaging
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Abstract
本发明涉及用于生产压块和压制的粒状材料的方法及其用于染色建筑材料例如混凝土和沥青，和有机介质例如涂料、塑料和色浆的用途。
Description
本发明涉及用于生产压块和压制的粒状材料的方法及其用于染色建筑材料例如混凝土和沥青，和有机介质例如涂料、塑料和色浆的用途。
为了实现最佳的颜色效应，颜料颗粒的生产要求将颜料研磨成基本颗粒。由此所形成的粉末产生大量的粉尘，由于其处于细分散状态，而易于粘附和粘在配料设备上。因此对于毒性有害物质，在生产过程中必须采取保护措施，以避免由于所形成的粉尘对人和环境产生损害。然而即使对于安全惰性物质例如氧化铁颜料，市场上也越来越需要避免由于粉尘而产生的刺激。
因此，处理颜料的目的是避免粉尘和改进作为良好的流动性结果的剂量性，从而实现用于建筑材料和有机介质中时一致质量的颜色效应。该目的大体上可以通过使颜料粒化的方法来实现。这里通常使用造粒和喷雾粒化作用。压制成型方法迄今仍不太适合，这是由于借此得到的颗粒物的分散性有限所致。
原则上，对于颜料颗粒的应用，市场上要求颜料有两个完全相反的性质：粒状物质的机械稳定性和良好的分散性。机械稳定性是造成在制造者与用户之间的运输过程中良好运输性质以及使用过程中颜料的良好剂量性和流动性的主要原因。它是由高附着力产生的，并取决于例如粘合剂的量乃至成型过程中的成型压力。另一方面，分散性受粒化之前的充分研磨(湿研磨和干研磨)、混合过程中的机械能(剪切力)和分散剂(它直接降低混入介质的过程中干粒状物质间的粘附力)影响。但是，由于添加剂与颜料的费用比，在颜料中大量使用分散剂将受到限制。另外，添加剂的高比例将相应地降低着色强度或散射能力。由于着色强度的变化通常小于±5％，因此即使是同时作为增粘剂和分散剂的添加剂也限制使用。而且添加剂必须使最终产品例如建筑材料、塑料和涂料的使用性不发生不利的改变：例如，混凝土的强度或凝结性，沥青的抗压强度或抗磨性和塑料的强度或抗缺口冲击性以及弹性体(聚合物)的弹性。
根据现有技术，适用于颜料颗粒的生产方法是：例如喷雾粒化(盘或喷管喷雾干燥)和造粒(混合器，流动床粒化器，盘或滚筒)。
喷雾干燥粒化通过使用粘合剂从颜料悬浮液开始。在许多被保护的权利要求中描述了相关的方法；其中使用了水溶性粘合剂。DE-A 3 619 363，EP-A 0 268 645和EP-A 0 365 046中的方法从有机物开始，例如木素磺酸盐、甲醛缩合物，葡糖酸、聚乙二醇醚硫酸酯，而DE-A 3 918694和US-A 5 215 583中的方法从无机盐开始，例如硅酸盐和磷酸盐。EP-A 0 507 046中描述了喷雾粒化和造粒的组合。DE-A 3 619 363(第3栏，44-47行)和EP-A 0 268 645(第7栏，18，19行)中采用了压制成型的方法。在该方法中，用压力实现颗粒的强粘附，以致可以得到良好的运输稳定性，但同时又降低了分散性。
EP-A 0257 423和DE-A 3 841 848中描述了用聚硅氧烷作为疏水、亲油添加剂的喷雾粒化作用。对于喷雾干燥的产品来说，为使物质变成疏水的，所进行的后处理将产生流动性非常好的粒状物质，但粉尘特别严重，而且几乎是不能用水湿润的。
EP-A 0424 896描述了低粉尘细粒状物质的生产，在已知的强度混合器中进行生产操作。用低含量蜡与乳化剂和湿润剂混合，从而产生水分散体。在该过程中通常得到的水含量为20％至高达50％以上。首先必须将这些粒状物质干燥，并且将其从粒度过大和过小的物质中分离出来。
DE-A 31 32 303描述了流散性良好的和低粉尘的无机颜料颗粒，将其与在热作用下变成液体的粘合剂混合，用筛分设备(压力)通过筛分使其粒化。流量的约10-20％累积作为＜0.1mm的细物质。
EP-A 0 144 940描述了低粉尘的颜料颗粒，从含水约50％的过滤沉积物开始，经过向其中加入0.5-10％的表而活性剂，以及在50-200℃下液化的蜡或矿物油，将其混合直至达到润滑点为止。该生产过程在强度混合器中进行，如果必要的话，将混合物粒化并干燥。在最终的产物中含10-15％的水，这对于加入到塑料中是不利的。
其他方法也在其应用上受限制。由于形成小液滴，喷雾粒化需要使用流散性良好的和充分液化的悬浮液。因此，对于该干燥过程，有更大量的水必须被蒸发掉，比通常可用的流动床干燥过程中从高压过滤颜料浆中蒸发掉的水还多，这导致高能耗。对于预先通过煅烧而产生的颜料，喷雾粒化包括附加的高能耗处理步骤。另外，在喷雾粒化过程中，累积了更大或更小比例的精细物质，它们必须返回到生产设备中。
造粒也经常显示出缺点。从颜料粉末开始，该方法可以在高涡流条件下的混合器中以流化床方法进行，要么通过盘式粒化和滚筒式粒化而进行。所有这些方法的共同之处是，对于粘合剂(大多数情况为水)的需要量如此之高，以致随后必须有干燥这样的附加处理步骤。这里，也得到不同尺寸的粒状物质，尤其是如果对于一定量的粉末来说粘合剂不足或实际分布不是最佳时。对于用作粒状物质来说，某一部分可能过大，而另一方面有些部分过小，因此粉尘的形成仍然存在。因此必须将所形成的粒状物质选分，把过大和过小的物质返回。
盘式粒化产生具有宽粒度范围的粒状颗粒。而这是不理想的，因为过大的颗粒分散性差，该粒化方法必须通过人力的强力操纵来控制，并且粒状物质的生产必须通过人工控制大量颗粒使其最佳化。通常在其之后也将进行选分，并把过大和过小的物质返回。
在干燥过程中，从浆液开始的挤压方法导致形成相对固化的粒状物质；由于它们的粒度，它们不能保证最佳分散性。
DE-A 42 14 195描述了用油作为粘合剂，用无机颜料颗粒染色沥青的方法。该方法是一种简单的粒化方法。
ED-A 4 336 613和DE-A 4 336 612中，通过将颜料与粘合剂混合、压制成型、粗研磨和粒化而生产出无机颜料颗粒。这样得到的粒状物质是不能令人满意地通过风力设备输送；在输送过程中，形成大量的粉尘，这是不理想的。
因此，本发明的目的是提供一种可以避免迄今所述的喷雾粒化、挤压粒化或造粒在其应用到无机颜料中的缺点的方法，该方法可以提供具有足够稳定的可以剂量的粒状物质，该粒状物质的粉尘低，而且与迄今使用的粉末有同样良好的分散性。
目前已发现，该目的可以通过混合、压制和分离的多步组合来实现，也可以再加上磨圆步骤。
本发明提供了一种由碳黑和助剂生产压块和压制的粒状物质的方法，该方法的特征是：a)把一种或多种炭黑与一种或多种可以提高加工性能的助剂混合，b)使该混合物经压制或压块步骤，c)把该压制或压块所得到的产物粉碎，d)把粉碎的产物分成两份或多份，e)把至少85％的颗粒大于80μm，优选大于100μm，或在80与2000μm之间，优选在100与1000μm之间的那部分除去，也可以在附加步骤中将其磨圆，而将其他部分转移出该过程或返回。
在c)步之前，优选可以把压制或压块的产物分成两份(中间步骤x)，为的是然后在c)步中，粉碎粗的部分，在该部分中至少85％的颗粒大于500μm，优选600μm，也为了分出其他部分，在d)步把细的部分再次分成两或多部分，将其与c)步的产物分开或放在一起。
优选在d)步中，只将由中间步x)所得到的细的部分分成两或多部分，而将由中间步x)所得到的粗的部分在c)步中粉碎，然后转移出该过程作为产品。
中间步x)优选可以通过风力选分或筛分(机械分离)而进行。优选使用筛分设备。
尤其优选在d)步中把粉碎的产物分成两份，把小于80μm的精细部分转移出或返回该过程，而大于80μm的粗的部分可以在附加步骤中磨圆。
优选也可以在d)步中把粉碎的产物分成三份，把细的部分和粗的部分转移出该过程或返回该过程，而在80与2000μm之间，尤其优选在100与1000μm之间，最优选在100与500μm之间的中间部分可以在附加步骤中磨圆。
粒状物质优选含有残余水的量低于4％重量，尤其优选低于2％重量。如果必要这可以通过后干燥来实现。
e)中的磨圆步骤优选在除去粉尘部分的情况下进行。
此外，优选可以用助剂涂敷e)中通过磨圆所形成的产物。
如果进行e)中的磨圆步骤，那么以后优选可以把粒度＞1500μm的粗的部分分离出来，也可以返回到该过程中。
粒状炭黑的体积密度优选在0.1与2.5g/cm3之间。
无机和有机物质都可以用作助剂。
所用的助剂优选为水、选自磷酸盐、碳酸盐、硝酸盐、硫酸盐、氯化物、硅酸盐、铝酸盐和硼酸盐的盐、甲酸盐、草酸盐、柠檬酸盐和酒石酸盐；多糖、纤维素衍生物例如纤维素醚、纤维素酯、膦酰基羧酸、改性硅烷、硅油、由生物学培育出的油(例如，菜子油、大豆油、玉米油、橄榄油、椰子油、葵花油)、基于链烷烃和/或环烷烃的精制石油、合成油、烷基酚、乙二醇、聚醚、聚乙二醇、聚乙二醇衍生物、蛋白质脂肪酸缩合物、烷基苯磺酸盐、烷基萘磺酸盐、木素磺酸盐、聚乙二醇醚硫酸酯、三聚氰胺甲醛缩合物、萘甲醛缩合物、葡糖酸、多羟基化合物或它们的水溶液。
此外，在混合过程中，优选可以加入所用颜料重量的0.01-5％重量，优选0.01-3％重量的乳化剂、湿润剂和分散剂。
对于用于含水的建筑材料体系例如混凝土，合适的乳化剂具体地说是HLB值为7-40，尤其是8-18的乳化剂，它们由烷基或丙烯酰基和亲水的中间部分以及端基例如酰胺、胺、醚、羟基、羧酸酯、硫酸盐、磺酸盐、磷酸盐、胺盐、聚醚、聚酰胺、多磷酸盐组成。根据它们的HLB值，可以分别使用这些物质，或将它们组合使用。
合适的湿润剂具体地说是烷基苯磺酸盐、脂肪醇硫酸酯、脂肪醇醚硫酸酯、脂肪醇乙氧基化物、烷基酚乙氧基化物、烷基磺酸酯、烯属磺酸酯。
优选使用三聚氰胺磺酸酯、萘磺酸酯、金属皂、聚乙烯醇、聚硫酸乙烯酯、聚丙烯酰胺、脂肪酸硫酸酯作为分散剂。
为了增加粒状物质的稳定性或促进粒状物质的生产，最后用附加层涂敷该粒状物质是有利的。该层可以通过涂敷无机盐溶液、多羟基化合物、油或蜡或聚醚、多羧酸酯或纤维素衍生物优选羧甲基纤维素而制备。
在混合过程中，也可以向粒状物质中加入防腐剂，其浓度为颜料重量的0.01-1％重量。可以提到的例子是可以释放甲醛的化合物、酚化合物或异噻唑啉酮制剂。
令人吃惊的是，用于压制和压块粒状物质(尤其是如果它们准备用作加入到含水建筑材料体系例如水泥砂浆或混凝土中)的助剂不仅可以是水溶性物质，而且也可以是水不溶的物质例如油。
助剂的加入量优选为所用颜料的0.001-10％重量，特别优选为0.01-5％重量，最优选为0.1-3％重量。
可以加入的助剂优选为与其他添加剂例如湿润剂、金属皂等化合的物质。
压制或压块步骤b)优选用辊式压制机或铸型压制机进行，优选在线压力为0.1-50kN/cm，优选0.1-20kN/cm下进行。
在压制或压块(压制成型，步骤b))中，重要的数值是每cm辊宽上的压力(kN)(线压力)。在辊间压制的过程中，认为压力是线性传递的，因为施加压力的表面不能确定，因此无法计算出压力(kN/cm2)。
压制成型优选在低线压力下进行。所施加的线压力通常优选在市售设备的较低范围内；优选在0.1与50kN/cm之间。线压力最优选为0.1-20kN/cm。市售设备的例子是由Bepex GmbH(Leingarten/Germany)公司制造的Pharmapaktor 200/50。
附加分离步骤x)优选用筛分机械例如转筒筛、振动筛和摆动筛进行。
粉碎可以用所有的工业粉碎设备例如破碎机、齿辊式破碎机、装有摩擦设备的碾压机和筛式轧碎机进行。
粉碎步骤c)优选用筛式轧碎机或筛式研磨机进行，其中物质通过筛孔为0.5-4mm，特别优选为0.5-2.5mm，最优选为1-2mm的筛(所谓的破碎机)而被压制。如通常所知道的那样，叶轮的运动是循环或振动的，其圆周速度为0.05米/秒-10米/秒，优选为0.3-5m/sec。叶轮与筛或破碎机肘板间的距离为0.1-15mm，优选为0.1-5mm，最优选为1-2mm。
可以使用的粉碎设备的例子是由Frewitt(Fribourg/Switzerland)公司制造的Flake破碎机。
粉碎后，把小于80μm的细物质分离出来。该细物质的量优选为10-50％重量，特别优选为10-30％重量。优选将该细物质返回到步骤b)。余下的部分流散性良好，可以定剂量，粉尘低，并且易分散。另外可以通过附加的磨圆步骤达到最佳效果。
磨圆步骤e)优选在旋转盘上、滚筒或拉绳滚筒中、转筒筛中或类似设备中或流化床上和筛分设备中进行。这里粉尘部分优选可以通过抽吸除去，或在流化床上通过空气运送出去。
根据DE-A 4 336 613或DE-A 4 336 612中的方法，通过在旋转盘上造粒，可以磨圆不均匀的颗粒。它们由致密的心和外层或在其上所形成的层(它们可以被磨掉)组成。因此这些产品将形成粉尘，尤其是当靠压缩空气输送时，并且流动性特别不好。按照本发明的方法得到的产品无这些缺点，这是由于它们是由具有均匀密度和强度的均匀的致密颗粒组成的。
按照本发明的方法生产的粒状物质可以用于染色建筑材料例如混凝土、水泥砂浆和灰泥，还可以用于染色有机介质例如涂料、塑料和颜料浆，并且还可以用于生产分散染料和淤浆。
根据本发明所生产的粒状物质特别适合用于掺入到干水泥砂浆中，和掺入到灰泥中。
在本发明的多步方法中，重要的是在第一步中通过在混合器中加入助剂而制备出有足够粘性的均相物质。然后在第二步中进行压块或压制。
本发明也提供了用炭黑染色建筑材料例如混凝土的方法，其特征是，压块或压制的无机粒状物质是由炭黑和助剂制成的，并且是通过本发明的方法生产的，把该粒状物质以水泥的0.1-10％重量，优选1-5％重量与建筑材料混合。
根据本发明所生产的粒状物质的另一个优选的用途是在分散染料和淤浆中的应用。
本发明还提供了用炭黑染色有机介质例如涂料体系、塑料和颜料浆的方法，其特征是，压块或压制的无机粒状物质是由炭黑和助剂制成的，并且是通过本发明的方法生产的，把该粒状物质以有机介质的0.1-10％重量与有机介质混合。
按照下列方法，根据白色水泥所产生的光谱，通过测定着色强度，在水泥砂浆中试验在建筑材料中的分散性：
水泥-石英砂比1∶4；水灰比0.35；颜料沉积程度为水泥的1.2％；所用的混合器，从RK Toni Technik，Berlin得到的，结构类型1551，转动速度140转/分；一次操作所需原料，500g水泥。100秒后，用混合物(300g)的3个样品，在压力(300巴)下制备出试验块(5×10×2.5cm)。试验块的固化：在30℃和95％的大气湿度下进行24小时，然后在60℃下干燥4小时。按照Dataflash 2000，Datacolor Internat ional，Cologne测定色彩数据，每石测定4个点，每个颜料混合物测定12个点。把所得到的平均值与标准样品的值比较。评价色差Eab和着色强度(标准样品＝100％)(DIN5033，DIN6174)。与标准样品的着色强度的差值最高达5％，称该分散性为良好，差值高达10％为令人满意的。
按照ASTM Test D 1200-88，通过评价从具有6mm开门的100ml漏斗中流出的情况，试验流动性。如果物质自由流动，那么认为流动性良好。如果物质不流动，或只有去掉塞子后才流动，那么认为流动性差。
根据DIN 4188的筛孔为80μm的VA筛，用Alpine 200 LS型空气喷射式筛分机确定细物质(由于筛孔过大)。用20g样品进行试验。抽吸5分钟除去细物质，重新称量筛上粗的部分的量。
按照DIN 53 775的第7部分“Testing of coloring material inplasticized polyvinyl chloride(PVC-P)materials；determination ofdispersing hardness by two roll milling”中的试验确定塑料的分散性。
在160±5℃下，用混合辊把试验的颜料分散在PVC中。把所得到的滚动层分开，然后一半露出来，以便在室温下通过滚动增加剪切力。对于彩色颜料，分散性的度量标准是热滚动与冷滚动的PVC层之间CIELAB(DIN 5033，6174)的色差ΔE，而对于白色颜料是热滚动与冷滚动的PVC层之间的标准三色激励值Y(DIN 5033)的差。易分散的颜料即使在低剪切力下电可以被分散，而为了分散相对不易分散的颜料，在低温滚动过程中需要增加剪切力。因此该规律是：色差ΔE或标准三色激励值Y的差越小，颜料的分散性越好。分散性是非常重要的，尤其是对于粒状物质，因为分散在塑料材料中的粒状物质的颗粒首先必须被分开。对于粒状物质，人们寻找与相应的颜料粉末一样良好的分散性，以便使粉末和粒状物质的特征值ΔE或Y没有太大的差别。
按照DIN 55992测定用于确定颗粒稳定性的细粉尘颗粒。用Heubach“粉尘测定仪”可以确定颗粒形成粉尘性。从滚筒中冒出的细粉尘颗粒的量可以用玻璃纤维过滤器，通过所流过的特定密度的空气流，用重量分析法测定。改变暴露的周期后，通过进行测定，可以确定粉尘形成的改进，这是由于机械应力的作用。
下面通过实施例更详细地说明本发明，但不应认为是对本发明的限定。实施例1
把500g Corasol C 30炭黑(a Degussa trade product)和500g Monarch800炭黑(a Cabot Corp.trade product)各自在混合器中与不同量的木素磺酸铵和V100机油混合18分钟。在WP50N型压实器(Remscheid的Alexanderwerk制造)用不同的线压力压制该混合物，然后，在RFG细轧碎机(Remscheid的Alexanderwerk制造)中用筛孔为1.5mm的筛将其粉碎。用筛孔为250μm的筛把粉碎的产物分成两份。对大于250μm的部分进行试验，其表现出良好的流动性(相应的粉末具有较差的流动性)。关于该部分与原来粉末的其余数据都列在表1中。确定混凝土的相对色强度，并与相应的原来粉末相比较。也可以把混凝土的相对色强度转换成相关的颗粒中的颜料含量(理论值)。实施例2
把500g Corasol C 30炭黑(a Degussa trade product)在混合器中与8％的木素磺酸铵和1％的V100机油混合18分钟。在WP50N型压实器(Remscheid的Alexanderwerk制造)以7KN/cm的线压力压制该混合物，然后，在RFG细轧碎机(Remscheid的Alexanderwerk制造)中用筛孔为1.5mm的筛将其粉碎。
用筛孔为250μm的筛把一部分粉碎的产物分成两份。对大于250μm的部分(该量的60％)进行试验，其表现出良好的流动性(相应的粉末具行较差的流动性)。
把另一部分粉碎的产物(约150g，包括一定量的细颗粒)在直径为15cm的辊筒中以60转/分的速度粒化5分钟。细颗粒全部粒化成更大的颗粒，该产物也表现出粒化的流动性和令人满意的分散性。但这两个产物在Heubach粉尘测定仪中的粉尘情况有很大的差别。试验后，压制、粉碎并后粒化的物质含1328mg粉尘，而压制粉碎并筛分没进行后粒化的物质含548mg粉尘。根据粉尘测定仪，原来的粉末Corasol C 30产生2669mg的粉尘。
表1
LS＝木素磺酸铵油＝V100机油
| 添加剂 | 线性压力〔kN/cm〕 | 体积密度〔g/ml〕 | 产率〔％〕 | 流出时间〔秒〕 | 在混凝土中的相对色强度〔％〕 | 在混凝土中的相对色强度〔％〕的理论值 | |
| Corasol C 30炭黑粉末〔1〕 | -- | -- | 0.40 | -- | 不能流动 | 100 | 100 |
| 由粉末〔1〕制备的炭黑颗粒1 | 8％ LS+1％油 | 7 | 0.48 | 60 | 33 | 81 | 89 |
| 由粉末〔1〕制备的炭黑颗粒2 | 8％ LS+1％油 | 5 | 0.46 | 52 | 32 | 85 | 93 |
| Monarch 800炭黑粉末〔2〕 | -- | -- | 0.20 | -- | 不能流动 | 100 | 100 |
| 由粉末〔2〕制备的炭黑颗粒3 | 1％ LS+1％油 | 7 | 0.27 | 47 | -- | 90 | 92 |
Claims (19)
1、一种由炭黑和助剂生产压块和压制的粒状物质的方法，该方法包括下列步骤：
a)把一种或多种无机炭黑与一种或多种可以提高加工性能的助剂混合，
b)使该混合物经压制或压块步骤，产生压制或压块产物，
c)把该压制或压块到的产物粉碎，产生粉碎产物，
d)把粉碎产物分成两份或多份，
e)分离出至少85％的颗粒至少为80μm的第一部分作为产物，而将其他部分转移出该过程。
2、根据权利要求1的方法，其中在c)步之前，把由b)步得到的压制或压块产物分成两份，这两份包括至少85％的颗粒大于500μm的粗的部分和细的部分，使粗的部分经过步骤c)，使细的部分经过步骤d)，在d)中被分开，将其与c)步的粉碎产物分开或放在一起。
3、根据权利要求1的方法，其中，在d)步中把粉碎的产物分成两部分，这两部分包括含有大于80μm的颗粒的粗的部分和含有小于80μm的颗粒的细的部分，把细的部分转移出该过程，其中粗的部分在磨圆步骤中磨圆。
4、根据权利要求1的方法，其中在d)步中把粉碎的产物分成三份，这三份包括粗的部分、细的部分和含有80-2000μm的颗粒的中间部分，把细的部分和粗的部分转移出该过程，其中中间的部分在磨圆步骤中磨圆。
5、根据权利要求4的方法，包括除去磨圆步骤中的任何粉尘的步骤。
6、根据权利要求1的方法，包括用助剂涂敷d)步中所得到的产物。
7、根据权利要求1的方法，其中助剂选自水、选自磷酸盐、硅酸盐、铝酸盐和硼酸盐的盐、甲酸盐、草酸盐、柠檬酸盐和酒石酸盐；多糖和纤维素衍生物、由生物学培育出的油、基于链烷烃和/或环烷烃的精制石油、合成油、烷基酚、乙二醇、聚醚、聚乙二醇、聚乙二醇衍生物、蛋白质脂肪酸缩合物、烷基苯磺酸盐、烷基萘磺酸盐、木素磺酸盐、聚乙二醇醚的硫酸酯、三聚氰胺甲醛缩合物、萘甲醛缩合物、葡糖酸、多羟基化合物或它们的水溶液。
8、根据权利要求1的方法，其中所加入的助剂量为所用炭黑的0.001-10％重量。
9、根据权利要求1的方法，其中，以0.1-50kN/cm的线压力，用辊式压制机或铸型压制机进行b)步中的压制或压块。
10、根据权利要求1的方法，其中步骤c)的粉碎是使物质通过筛孔为0.5-4mm的筛而筛分来进行的。
11、根据权利要求1的方法，包括用于磨圆第一部分的颗粒的磨圆步骤，其中磨圆步骤在旋转盘上、滚筒中、筛分设备中或流动床上进行。
12、用按照权利要求1的方法生产的粒状物质染色包括混凝土、水泥砂浆和灰泥的建筑材料和染色包括涂料、塑料和颜料浆的有机介质以及生产分散染料和淤浆的方法。
13、染色建筑材料的方法，该方法包括把根据权利要求1生产的压块和压制的粒状物质以水泥的0.1-10％重量与建筑材料混合。
14、染色有机介质的方法，该方法包括把根据权利要求1生产的压块和压制的粒状物质以有机介质的0.1-10％重量与有机介质混合。
15、根据权利要求1的方法，其中第一部分有85％大于100μm的颗粒。
16、根据权利要求1的方法，其中第一部分有85％在80-2000μm之间的颗粒。
17、根据权利要求16的方法，其中第一部分有85％在100-1000μm之间的颗粒。
18、根据权利要求1的方法，包括用于磨圆第一部分颗粒的磨圆步骤。
19、根据权利要求18的方法，包括除去磨圆步骤中的任可粉尘的步骤。
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| DE19649756B4 (de) * | 1996-04-18 | 2005-05-25 | Bayer Chemicals Ag | Verfahren zur Herstellung von Brikettier- und Preßgranulaten aus Rußpigmenten und deren Verwendung |
| DE19704943A1 (de) * | 1997-02-10 | 1998-08-13 | Bayer Ag | Anorganische Pigmentgranulate zum Einfärben von Kunststoffen, Lacken und Baustoffen und ein Verfahren zu deren Herstellung |
| DE19706899C1 (de) * | 1997-02-21 | 1998-11-05 | Bayer Ag | Anorganische, kompaktierte Pigmentgranulate, Verfahren zu ihrer Herstellung und ihre Verwendung |
| DE19731698A1 (de) * | 1997-07-23 | 1999-01-28 | Brockhues Chem Werke Ag | Verfahren zur Einfärbung von Baustoffen und Asphalt |
| US5853476A (en) * | 1997-08-11 | 1998-12-29 | Elementis Pigments, Inc. | Process for coloring concrete using compacted inorganic granules |
| DE19811553A1 (de) | 1998-03-18 | 1999-09-23 | Bayer Ag | Rußgranulate |
| DE19846774A1 (de) * | 1998-10-10 | 2000-04-20 | Cognis Deutschland Gmbh | Additive für die Verarbeitung von Kunststoffen |
| DE10046152A1 (de) * | 2000-09-15 | 2002-03-28 | Merck Patent Gmbh | Pigmentpräparation in Granulatform |
| DE19950712A1 (de) | 1999-10-21 | 2001-04-26 | Vti Thueringer Verfahrenstechn | Farbpigmentgranulat |
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- 1997-04-07 ES ES97105720T patent/ES2179233T3/es not_active Expired - Lifetime
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