CN102821842B - 粗载体二氧化硅颗粒 - Google Patents
粗载体二氧化硅颗粒 Download PDFInfo
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- CN102821842B CN102821842B CN201180015532.7A CN201180015532A CN102821842B CN 102821842 B CN102821842 B CN 102821842B CN 201180015532 A CN201180015532 A CN 201180015532A CN 102821842 B CN102821842 B CN 102821842B
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- silica
- absorbate
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Abstract
本发明涉及一种新的粒状二氧化硅,其用作载体材料,特别是用作固定床反应器催化剂的载体,本发明还涉及其生产和用途。
Description
背景技术
本发明涉及一种新的粒状二氧化硅,其用作载体材料,特别是作为不同的反应器系统中的催化剂的载体,和涉及其生产和用途。
技术领域
在许多的应用领域中,例如在用于农作物保护的产品领域中,在活性药物成分的情况中,在生产动物饲料和动物饲料添加剂或者在食品工业中,使用载体材料来例如将液体或者树脂质活性成分转化成自由流动的和存储稳定的形式。为了生产固体配料,将液体或者可熔的物质或者物质混合物施用到载体材料上,在一些情况中与辅助剂(例如表面活性剂和分解剂)一起施用。在固体物质的情况中,载体材料主要用作填料,而它们在液体或者低熔融物质的情况中吸收了液体。这应当提供了易于处理的,表面干燥的被吸收物质,其然后投入市场,例如用于农用化学品领域,直接处于粉末的形式(称作WP,可润湿粉末)或者处于进一步加工的形式,用作颗粒/挤出物(WG,水可分散颗粒)。如果具体的应用需要,则可以干燥该吸收液,或者可以固化该吸收熔融物。通常,可以提及的是负载的载体材料。
对于载体材料的一个主要的需求是足够高的吸收性,以使得需要使用尽可能少的载体材料。一系列的专利申请例如DE102006002765因此涉及到提高被吸收的材料在载体材料上的含量的方法。但是,进行这些方法是非常复杂的,并且它们迄今在工业规模上还没有确立。
对于载体材料的另一需求是被吸收物质具有良好的自由流动和因此良好的加工性。另外,二氧化硅在被吸收物质的运输、分配和生产过程中应当具有最小生尘水平。为了改进自由流动,EP0984772B1和EP0966207B1例如因此提出了使用微粒状二氧化硅作为载体材料,该二氧化硅是近似球形的,平均粒度大于150μm。虽然以此方式被吸收物质具有改进的自由流动性,但是二氧化硅的加工性不是最佳的,因为在用这些二氧化硅生产被 吸收物质中经常观察到在混合器中发生团块,并且有时候必须以昂贵的和不方便的方式除去。
在固定床催化领域中,对于载体或者载体材料存在着另外的要求。例如,必需确保固定床反应器(其中反应物流过填充有负载的载体材料的反应室,催化剂已经施用到该载体材料上)中的反应在反应室中产生了最小的压降。在其中催化剂负载的载体材料悬浮于反应介质中的反应的情况中,该载体材料在反应结束时必须可以再次容易的除去。最后,在流化床反应器中的反应要求负载的载体材料能够在其中有效的流态化。因此很显然不同的反应器类型对于负载的载体和因此同样对于载体材料提出了相当不同的需求。迄今,如上所示,研究工作主要集中于载体材料的吸收性或者其加工性。对于催化方法中特定的需求来说,这里仍然没有令人满意的载体材料。
因此仍然非常需要廉价的载体或者载体材料,其具有良好的加工性,允许生产具有良好自由流动性的高负载被吸收物质,此外具有对于催化方法而言良好的适应性。
被吸收物质理解为表示负载有活性物质或者活性物质混合物的载体或者载体二氧化硅,直接的或者处于分散体、溶液中或者处于熔体中。除了活性物质或者活性物质混合物之外,它还可以负载辅助剂或者赋形剂。负载到载体或者载体二氧化硅上的物质在此也称作被吸收的物质。
发明内容
因此本发明的一个目标是提供一种新的粒状二氧化硅,其仅仅具有很低程度的(如果不是一点没有)现有技术的载体或者载体材料的至少一些缺点,并且其允许生产新的负载的载体或者具有改进性能的载体。另外,还提供了生产这些粒状二氧化硅的方法和生产负载的载体的方法。
本发明的一个具体目标是提供粒状二氧化硅,其允许生产这样的载体,该载体已经负载有催化剂,并且其能够非常容易地从悬浮液中除去。
本发明的另外一个具体目标是提供粒状二氧化硅,其允许生产这样的载体,该载体已经负载有催化剂,并且其在固定床反应器中,在它流过时,引起了反应混合物最小程度的压降。
这些目标和另外的没有明确提及的目标是通过权利要求书、说明书和实 施例中详细说明的粒状二氧化硅、负载的载体和生产方法来实现的。
已经令人惊讶地发现使用EP0984772B1和EP0966207B1中所述的球形和平均粒度大于150μm的载体材料来生产被吸收物质是不足的,因为这样的载体材料在固定床反应中没有实现令人满意的结果。
本发明人通过深入研究已经发现载体材料必须满足的基本标准是其对于机械应力的稳定性。当载体材料过软时,在混合器中作用于载体材料上的应力会导致结块。另外,在负载的载体材料进一步加工过程中和在反应器填充过程中,一部分的载体材料会粉化,并且所形成的粉末会堵塞反应器,导致反应器中的压降增加。
还已知的是如果载体材料不够硬,则在流体流过反应器中的负载的载体时,会发生磨损现象;这能够明显地解释在固定床反应器运行操作中的压降或者悬浮的催化剂区域中的过滤问题。
最后,已经发现载体材料的颗粒必须具有特定的粒度分布,以便在固定床反应器或者流化床反应器中产生最小的流动阻力。
可以通过特定的生产方法来提高本发明的粒状二氧化硅的硬度,以使得它们能够明显更好地经受住被吸收物质生产中、被吸收物质加工和反应器运行中的机械应力,并因此具有明显改进的性能。另外,改进了粒度分布,并且确保了硬化的粒状二氧化硅具有足够高的孔隙率。本发明的粒状二氧化硅因此在下面的方面中是显著的:足够高的孔隙率(用Hg孔体积表示),更好稳定的孔壁(用未超声波曝露的平均粒度(d50)与超声波曝露3min后的平均粒度(d50U)之比表示)和最佳的粒度(用dQ3=10%来描述细颗粒部分,和用dQ3=90%来描述粗颗粒部分)。换句话说,实现了机械稳定性的提高,和与此同时,获得了具有最佳粒度分布的高吸收性。
在一种优选的实施方案中,本发明的二氧化硅具有大约中性的pH,以使得它们能够非常普遍地用作载体,并且对于被吸收的材料的存储稳定性不具有任何不利的作用。
另外,本发明的二氧化硅,与市售使用的载体或者载体二氧化硅例如来自Rhodia Chimie的Zeosil165GR或者来自Huber Corp的Zeodent DP-9175相比,具有最佳比例的硬度(即,机械稳定性)、细颗粒部分和粗颗粒部分的粒度分布、和吸收性。
本发明因此提供一种粒状二氧化硅,具有
-Hg孔体积(<4μm)大于0.90ml/g,
-dQ3=10%大于400μm,同时dQ3=90%小于3000μm,和
-未超声波曝露的d50与超声波曝露3min后的d50之比<4.00。该测量是在400-500μm的颗粒部分上进行的。
本发明另外提供一种粒状二氧化硅,其除了上述参数之外,具有至少一种下面的性能:
-pH为5-8.5
-未超声波曝露的d50与超声波曝露3min后的d50之比是1.00-3.00,优选1.00-2.60,更优选1.00-2.10,特别优选1.00-1.60。该测量是在400-500μm的颗粒部分上进行的。
本发明另外提供了生产本发明的粒状二氧化硅的第一方法,其包含步骤:
a)提供沉淀的或者气相法二氧化硅,其处于干燥的和/或研磨的形式,并且具有
-未超声波处理的平均粒度d50是0.1-350μm,
-BET表面积是30-800m2/g,和
-DBP值是140-400g/100g;
b)根据用于30-80重量%的干燥失重所用的成形方法,来增湿来自步骤a)的二氧化硅;
c)通过挤出、粒化、压实或者其他常规成形方法来成形来自步骤b)的二氧化硅;
d)在适于此的干燥单元中,干燥该成形的二氧化硅体;和
e)以3000μm的筛孔尺寸来过筛粒化或者过筛所述颗粒,并且用400μm筛孔尺寸筛掉细颗粒。
作为上述本发明第一方法的一种选项,还可以使用干燥失重为30-80重量%的含水滤饼,作为用于步骤c)的起始材料。
本发明进一步提供用于生产本发明的粒状二氧化硅的第二方法,其包含步骤
i)提供沉淀的或者气相法二氧化硅,其处于干燥的和/或研磨的形式,并 且干燥失重<30重量%,和具有
-未超声波处理的平均粒度d50是0.1-350μm,
-BET表面积是30-800m2/g,和
-DBP值是140-400g/100g;
ii)通过干压实,优选在两个旋转辊之间,以0.5kN/cm辊宽-12kN/cm辊宽的特定接触压力使来自步骤i)的二氧化硅成形,来产生小块(slug),和
iii)以3000μm的筛孔尺寸来过筛粒化或者过筛所述小块,并且用400μm筛孔尺寸筛掉细颗粒。
在上述本发明全部的方法中,可以通过将颗粒在高温例如70°C-400°C用水蒸气进行处理,来进一步提高颗粒硬度。其后,另外的干燥步骤会是必需的。
另外,可以通过将颗粒与碱性物质接触一定的时间来提高颗粒的pH,来提高颗粒的硬度。该方法详细描述在DE 102008035867A1中。
提高颗粒硬度另外的手段包括将颗粒在高温,典型的在700°C-1200°C,煅烧一定时间(通常<1h)。
上述用于硬化颗粒的方法步骤可以在筛分颗粒和过筛的方法步骤之前或者之后进行。
本发明第一方法的增湿和/或粒化方法步骤可以在高速强力混合器、捏合机、压实机、盘式造粒机和/或穿孔压模机等中进行。可选择的,该增湿之后可以是挤出,或者含水滤饼可以直接挤出。挤出的成形体随后可以通过另外合适的方法(例如来自Caleva的球化机(spheronizer))来改变几何形状。
本发明第一方法的干燥方法步骤可以例如在干燥箱、流化床干燥器,带式干燥器等中进行。如果需要,该干燥的成形体随后可以通过另外的方法例如以3000μm的筛孔尺寸过筛或者过筛粒化,和用400μm筛孔尺寸筛掉细颗粒,来调整到适当的粒度级。
本发明第二方法的成形步骤优选是在压实机,例如在来自Hosokawa Bepex GmbH的设备中,例如在Bepex L200/50,或者Alexanderwerk AG中进行的。
本发明两种方法的过筛粒化优选是在设备例如来自Frewitt或者 Hosokawa Bepex GmbH的筛磨机中进行的。该过筛可以通过全部已知的技术来进行,优选通过来自公司例如Vibra、Engelsmann或者Allgeier的振动筛来进行。可以进行若干个过筛或者若干个筛选步骤。
本发明另外提供本发明的二氧化硅的用途,其用作载体材料,优选用作催化剂的载体材料。
本发明最后提供包含至少一种本发明的二氧化硅的被吸收物质。
本发明的主题在下文中详细描述。在本发明的上下文中,术语“二氧化硅”、“沉淀的二氧化硅”和“气相法二氧化硅”是同义使用的。
足够高的孔隙率确保了本发明的粒状二氧化硅在中孔和/或大孔范围内具有足够的孔体积,并因此该催化剂具有对于反应物良好的可接近性,和同时需要最小量的载体材料用于生产本发明的被吸收物质。本发明的粒状二氧化硅因此具有大于0.90ml/g,优选大于1.35ml/g,更优选大于1.60,甚至更优选大于1.80,特别优选大于1.90的Hg孔体积(<4μm)。
另外优选本发明的粒状二氧化硅的Hg孔体积(<4μm)是0.9-1.34ml/g,更优选0.9ml/g-1.30ml/g,最优选0.9ml/g-1.20ml/g。
本发明的粒状二氧化硅另外一个重要的性能是其硬度。当孔隙率较高时,会是这样的情况,即,不再能够保证机械稳定性,这会导致在作用于二氧化硅和由其所生产的被吸收物质的机械应力下,细颗粒形成的增加。在二氧化硅包装和运输过程中,在被吸收物质生产过程中和在负载的载体材料使用过程中,机械应力是通过对悬浮于水中的二氧化硅施加3min的超声波作用来模拟的。未超声波曝露的d50与超声波曝露3min之后的d50之比给出了关于d50被机械应力降低了多少的信息。二氧化硅越硬,超声波曝露之后的d50U和未超声波曝露的d50之间的差异越小,即,在理想的情况中,未超声波曝露的d50与超声波曝露3min后的d50U之比是1.00。本发明的粒状二氧化硅具有非常良好的硬度(不管它们高的平均粒度),这样未超声波曝露的d50U与超声波曝露3min后的d50之比小于3.00,优选小于2.60,更优选小于2.10和特别优选小于1.60。这个测量是在400μm-500μm的颗粒部分上进行的。
粒度分布(用dQ3=10%和dQ3=90%表征)对于确保在固定床反应器中良好的流动性或者确保在流化床反应器中良好的流化性来说是重要的。过大的颗 粒不具有用于反应、溶解和扩散所需的足够的比表面积。过小的颗粒反过来增加了流动阻力。本发明的粒状二氧化硅因此具有dQ3=10%>400μm和dQ3=90%<3000μm。
本发明的粒状二氧化硅优选的pH是5-8.5。这种基本中性pH的二氧化硅确保了对于待吸收液体宽的应用范围,因为过酸性或者过碱性的载体材料会触发或者加速待吸收液体的分解或者其他化学转化。
对于载体或者载体应用来说,市售的许多二氧化硅可以用于本发明的方法中。其例子是来自Evonik Degussa GmbH的二氧化硅 50、 50S、500LS、22、 22S、 22LS和 33。如本发明人已经发现的,这些二氧化硅(即使专门开发用于载体或者载体应用)它们本身不适于或者仅仅不充分的适于作为载体材料用于催化方法领域中。造成此的原因(特别是在喷雾干燥、喷嘴塔干燥和/或研磨颗粒的情况中)是其过低的粒度,其如上所述,会导致反应器中不期望的压力升高。通过本发明的方法,进行了二氧化硅的压实,由此获得的颗粒的粒度和强度是通过本发明的方法来控制的,来获得具有最佳粒度分布和硬度的颗粒,其在反应器中具有低的流动阻力或者能够容易地从悬浮液中滤出。
除了已经提及的二氧化硅之外,在本发明第一方法的步骤a)中,可以使用例如来自Evonik Degussa GmbH的二氧化硅 2200、 200,来自Rhodia Chimie的 38A到X,来自PPG的 SC60和 SC72,来自Huber的 5170,和欧洲专利EP0984772B1、EP0966207B1和EP0937755A1中所公开的二氧化硅。
本发明方法中所用的二氧化硅具有:
-未超声波处理的平均粒度d50是0.1-350μm,优选0.1-200μm,更优选0.1-150μm和最优选1-50μm;
-BET表面积是30-800m2/g,优选40-700m2/g,更优选50-600m2/g,最优选150-550m2/g;和
-DBP值是140-400g/(100g),优选140-350g/(100g),更优选190-350g/(100g),最优选290-350g/(100g)。
本发明的第一方法优选是在混合器、捏合机或者压实机(任选的具有下 游挤出机)和下游干燥机、筛网造粒机和筛网中进行。例如,可以首先例如在来自Eirich GmbH的设备中用液体润湿初始加入的二氧化硅(除非滤饼是直接使用的),然后将它压缩或者压实,然后挤出它和干燥它。同样可以干燥该液体润湿的和压缩的或者压实的二氧化硅,然后进行过筛粒化,然后将它过筛到期望的颗粒部分。
最终的载体或者载体颗粒的硬度可以通过压缩或者压实起始二氧化硅的手段来控制。压实通常是通过加水,同时引入剪切能来进行的。另外,还可以加入水溶液例如纤维素溶液或者油,其适于充当颗粒之间的粘合剂。基于1.00g/ml的密度,液体优选的加入比例是50-90重量%,更优选的比例是60-90重量%和最优选的比例是65-90重量%。另外,在压实过程中,可以加入固体,其适于充当颗粒之间的粘合剂,例如纤维素、蜡或者聚合物,或者随后聚合的单体。该固体的加入比例是0.1-50重量%,优选的比例是0.5-15重量%,更优选的比例是0.5-8重量%。
在一种优选的实施方案中,将载体或者载体材料压缩或者压实,而不加入粘合剂。
压实优选在10°C-90°C,更优选10°C-70°C的温度进行。
在本发明第一方法中的成形优选是如下来进行的:在混合单元中,将起始二氧化硅借助于所加入的液体来深度压实,直到液体部分排出,并且颗粒开始粒化为止。因此获得的颗粒(原料颗粒)的粒度可以通过挤出步骤来均化,然后可以将它们干燥。另外,在省略了挤出步骤时,潮湿的原料颗粒也可以直接干燥和例如经过特征尺寸为3000μm的筛子,其粉碎了大于所述特征筛子尺寸的颗粒。该通过优选是在设备例如来自Frewitt或者HosokawaBepex GmbH的筛磨机中进行的。大于通过筛特征尺寸的颗粒在本发明的载体材料用于悬浮液催化领域的情况中,会导致被吸收物质不期望的沉降和导致长的扩散或者反应时间。当除去全部小于400μm的筛分时,它是另外有利的。如上所述,这些小颗粒对于颗粒的流动阻力具有不利的作用,并且导致了固定床反应器中的压降。
过筛可以通过全部已知的技术来进行,优选通过来自公司例如Vibra、Engelsmann或者Allgeier的振动筛来进行。可以进行若干个过筛或者若干个筛分步骤。
在本发明方法的第二种情况中,在其中二氧化硅的压实优选是在具有下游筛网造粒机和筛子的干燥压实机中进行的,换句话说,初始加入的二氧化硅首先例如在来自Hosokawa Bepex GmbH的设备例如Bepex L200/50中压实,或者在来自Alexanderwerk AG的设备中压实,然后将该压实的材料筛分成期望的颗粒部分。
在本发明第二方法的步骤ii)中,将干燥的起始二氧化硅压实,即,压成小块,其具有对于本发明的应用来说最佳的粒度和硬度。硬度可以通过起始二氧化硅的压实所用的压力来控制。压实优选是在0.5-15kN/cm辊宽,更优选3-12kN/cm辊宽和最优选6-10kN/cm辊宽的特定接触压力,和10°C-90°C,更优选10°C-70°C的温度进行的。另外,在压实过程中,可以加入液体,优选水、水溶液例如纤维素溶液、或者油,其适于充当颗粒之间的粘合剂。液体优选的加入比例是1-30重量%,更优选的比例是1-20重量%和最优选的比例是3-15重量%。另外,在压实过程中,可以加入这样的固体,其适于充当颗粒之间的粘合剂,例如纤维素、蜡或者聚合物或者单体,其随后聚合。该固体的加入比例是0.1-50重量%,优选的比例是0.5-15重量%,更优选的比例是0.5-8重量%。
这种干燥压实优选是以这样的方式进行的,即,将干燥的起始二氧化硅在两个旋转辊之间的压实单元中压缩,至少一个辊子更优选具有凹进部例如凹槽、凹陷或者衬垫,其特征尺寸大于待获得的颗粒的这些尺寸。所述辊子是直的或者凹陷构造的。另外一种特别优选的实施方案包括使用至少一个有孔锯齿的轮辊。另外,当至少一个辊子配置成使得在辊子表面可以产生减压,通过其将待压实的二氧化硅吸入到辊子上,则它会是有利的。二氧化硅可以通过本领域技术人员已知的所有传输装置例如螺旋传输机、双螺杆等供给到压实单元。
在压实后,使所获得的小块经过特征尺寸为3000μm的筛子,在此过程中,粉碎了大于特征筛子尺寸的颗粒。该通过优选是在设备例如来自Frewitt或者Hosokawa Bepex GmbH的筛磨机中进行的。大于通过筛特征尺寸的颗粒在本发明的载体材料用于悬浮液催化领域的情况中,会导致被吸收物质不期望的沉降和导致长的扩散或者反应时间。另外,除去了小于400μm的筛分。如上所述,这些小颗粒对于颗粒床的流动阻力具有不利的作用, 并且导致了固定床反应器中的压降。
对于完成的干燥颗粒可能的水蒸气处理可以在所有的适于此目的设备中完成,例子是带式干燥机、旋转管式干燥机、干燥箱、流化床干燥机等。将颗粒曝露于70°C-400°C,优选80°C-300°C,更优选90°C-200°C和最优选106°C-180°C的温度。在此温度的驻留时间最高到16h,优选最高到12h,更优选最高到8h,最优选最高到4h。
颗粒可能的煅烧可以在不同的设备中进行,例如在煅烧炉、带式或者旋转管式煅烧机,或者在闪或者流化床煅烧机中进行。这包括将颗粒曝露于700°C-1200°C,优选800°C-1200°C,更优选800°C-1100°C的温度。驻留时间取决于煅烧温度和期望的颗粒硬度。在所述方法中驻留时间是1h,优选20min,更优选小于10min。
本发明的粒状二氧化硅可以用于生产被吸收物质,该被吸收的物质优选是硬化剂或者引发剂、交联剂、催化剂、活性药物成分和赋形剂、活性化妆品成分和赋形剂、清洁和/或护理组合物、调味剂、芳香剂和香味剂、动物饲料或者动物饲料添加剂、例如氨基酸、维生素、矿物质、食品或者食品添加剂、染料和/或颜料、氨基酸、氧化或者漂白剂,具有微生物,特别是真菌或者杀菌作用的添加剂,用于农业和林业的化学品,和/或混凝土混合物。吸收到载体上的材料可以是含水或者非含水液体,例如油、树脂、溶液、分散体、悬浮液、乳液、蜡、聚合物或者熔体。被吸收的物质随后可以热处理、加热处理或者诱导结晶来凝固、分离或者反应。另外,被吸收的物质可以事先或者之后进行干燥。
在动物饲料和动物饲料添加剂领域中的被吸收物质包括例如维生素、矿物质、羧酸、无机酸、氨基酸、脂肪、油和芳香剂。它们更优选是甲酸、乙酸、丙酸、乳酸、磷酸、氯化胆碱溶液、维生素E乙酸酯和植物提取物,例如万寿菊提取物。
在农业和林业领域中的被吸收物质包括例如被吸收的肥料,例如含有硝酸盐和/或磷酸盐的肥料、农作物保护组合物、杀虫剂,例如除草剂,杀真菌剂、杀虫剂。
在化妆品产品领域中的被吸收物质包括例如油类例如香精油、香油、护理油、香味油和硅油、活性抗菌剂、抗病毒或者抗真菌成分;消毒剂和抗 菌物质;除臭剂;抗氧化剂;生物活性物质和源于生物的活性成分;维生素和维生素络合物;酶和酶体系例如淀粉酶、纤维素酶、脂肪酶和蛋白酶;化妆活性物质例如化妆品和个人卫生产品的成分;清洗-和清洁-活性物质例如全部种类的表面活性剂、清洗-和/或清洁-活性无机和有机酸、除污剂和污物-释放活性成分、氧化剂和漂白剂、漂白活化剂、增洁剂和助增洁剂、抗再沉积添加剂、灰化和变色抑制剂、用于护色的活性物质、用于洗衣护理的物质和添加剂、荧光增白剂、泡沫抑制剂、pH调节剂和pH缓冲物质。
在食品和食品添加剂领域中的被吸收物质包括例如被吸收的芳香剂、食品增补剂、维生素、矿物质、氨基酸。
来自活性药物成分的被吸收物质包括全部种类的活性药物成分,例如α-蛋白酶抑制剂、阿巴卡韦、阿昔单抗、阿卡波糖、乙酰基水杨酸、阿昔洛韦、腺苷、舒喘灵、阿地白介素、阿仑唑奈、阿夫唑嗪、阿洛司琼、阿普唑仑、阿替普酶、氨溴索、氨磷汀、乙胺碘呋酮(amiodarone)、氨磺必利、氨氯地平、羟氨苄青霉素(amoxycillin)、安非他明、两性霉素、氨比西林、安瑞那韦、阿那格雷、阿那曲唑(anastrozole)、安克洛酶、抗血友病因子、抑肽酶、阿替洛尔、阿托伐他汀、阿托品、azelastine、阿奇霉素、甘菊环、巴尼地平、氯地米松、贝那普利、苄丝肼(benserazide)、贝前列素、倍他米松、倍他索洛尔、苯扎贝特、比卡胺(bicalutamide)、甜没药醇(bisabolol)、比索洛尔、肉毒杆菌毒素、溴莫尼定、溴西泮、溴麦角环肽、布地缩松(budesonide)、布比卡因、安非他酮、丁螺环酮、布托啡诺(butorphanol)、卡麦角林、calcipotriene、降血钙素、钙三醇、樟脑、坎地沙坦、candesartancilexetil、卡托普利、卡巴咪嗪、卡比多巴、卡铂、卡维地洛、头孢克洛、头孢羟氨苄、头孢西丁(cefaxitin)、头孢唑林、头孢地尼、头孢吡肟、头孢克肟、头孢美唑(cefmetazole)、头孢哌酮、头孢替安、头孢唑兰(cefoxopran)、头孢泊肟(cefpodoxime)、头孢丙烯、头孢他啶、头孢布烯、头孢三嗪(ceftriaxone)、头孢呋新(cefuroxime)、celecoxib、塞利洛尔、头孢氨苄、西立伐他汀、西替利嗪、氯霉素、西司他丁、西拉普利、甲氰咪胍、环丙贝特、环丙沙星、西沙必利、顺氯氨铂(cisplatin)、西酞普兰、克拉霉素、克拉维酸、氯洁霉素、氯米帕明、氯硝西泮、氯压定、氯吡格雷、克霉唑、氯氮平(clozapine)、色甘酸、环磷酰胺、环孢菌素、去乙酰环丙氯地孕酮、 达替肝素(dalteparin)、去铁胺、去氧孕烯、右旋安非他明、安定、双氯芬酸、去羟肌苷、洋地黄毒苷、异羟洋地黄毒苷、双氢麦角胺、地尔硫卓、白喉蛋白、白喉类毒素(diphtheriatoxoid)、divalproex、多巴酚丁胺、多西紫杉醇(docetaxel)、多拉司琼(dolasetron)、多奈哌齐、阿法链道酶(dornase-α)、多佐胺(dorzolamide)、多沙唑嗪(doxazosin)、去氧氟尿苷、多柔比星、地屈孕酮、依卡倍特、依非韦伦、依那普利(enalapril)、enoxaparin、乙哌立松、依匹斯汀、表柔比星、埃替非巴肽(eptifibatide)、红细胞生成素-α、红细胞生成素-β、etanercept、乙炔基雌二醇、依托度酸、依托泊苷、VIII因子、泛昔洛韦(famciclovir)、法莫替丁(famotidine)、法罗培南(faropenem)、非洛地平(felodipine)、非诺贝特(fenofibrate)、非诺多泮(fenoldopam)、芬太奴(fentanyl)、非索非那定(fexofenadine)、非格司亭(filgrastim)、非那雄胺(finasteride)、氟氧头孢(flomoxef)、氟康唑(fluconazole)、氟达拉滨(fludarabine)、氟尼缩松(flunisolide)、氟硝西泮(flunitrazepam)、氟西汀(fluoxetine)、氟他米特(flutamide)、氟替卡松(fluticasone)、氟伐他汀(fluvastatin)、氟伏沙明(fluvoxamine)、促滤泡素-α、促滤泡素-β、福莫特罗(formoterol)、福辛普利(fosinopril)、利尿磺胺(furosemide)、加巴喷丁(gabapentin)、钆双胺(gadodiamide)、更昔洛韦(ganciclovir)、加替沙星(gatifloxacin)、吉西他滨(gemcitabine)、乙羟基二降孕二烯炔酮(gestodene)、格拉替雷(glatiramer)、格列本脲(glibenclamide)、格列美脲(glimepiride)、格列吡嗪(glipizide)、格力本(glyburide)、戈舍瑞林(goserelin)、格拉司琼(granisetron)、灰黄霉素(griseofulvin)、B型肝炎抗原、透明质酸、hycosin、二氢氯噻(hydrochlorothiazide)、氢可酮(hydrocodone)、氢化可的松、氢吗啡酮(hydromorphone)、羟化氯喹(hydroxychloroquine)、hylan G-F20、布洛芬、异环磷酰胺(ifosfamide)、咪达普利(imidapril)、伊米苷酶(imiglucerase)、亚胺培南(imipenem)、免疫球蛋白、茚地那韦(indinavir)、消炎痛(indomethacin)、因福利美(infliximab)、胰岛素、人胰岛素、胰岛素lispro、胰岛素aspart、干扰素-β、干扰素-α、碘-125、碘克沙醇(iodixanol)、碘苯六醇(iohexol)、碘美普尔(iomeprol)、碘普罗胺(iopromide)、碘佛醇(ioversol)、ioxoprolene、抗乙酰胆碱(ipratropium)、依普黄酮(ipriflavone)、 厄贝沙坦(irbesartan)、伊立替康(irinotecan)、异山梨醇(isosorbide)、异维甲酸(isotretinoin)、伊拉地平(isradipine)、伊曲康唑(itraconazole)、二钾氯氮卓(potassium chlorazepate)、氯化钾、酮咯酸(ketorolac)、酮替芬(ketotifen)、百日咳疫苗、凝血因子IX、拉米夫定(lamivudine)、拉莫三嗪(lamotrigine)、兰索拉唑(lansoprazole)、拉坦前列素(latanoprost)、来氟米特(leflunomide)、来格司亭(lenograstim)、来曲唑(letrozole)、亮丙瑞林(leuprolide)、左旋多巴(levodopa)、左氧氟沙星(levofloxacin)、右旋甲基炔诺酮(levonorgestrel)、右旋甲状腺素(levothyroxine)、利多卡因(lidocaine)、利奈唑胺(linezolide)、赖诺普利(lisinopril)、碘帕醇(lopamidol)、氯碳头孢(loracarbef)、氯雷他定(loratadine)、劳拉西泮(lorazepam)、氯沙坦(losartan)、洛伐他汀(lovastatin)、赖氨酸乙酰基水杨酸、马尼地平(manidipine)、甲钴胺(mecobalamin)、甲孕酮(medroxyprogesterone)、甲地孕酮(megestrol)、美洛昔康(meloxicam)、四烯甲萘醌(menatetrenone)、脑膜炎球菌疫苗(meningococcus vaccine)、促生育素(menotropin)、美罗培南(meropenem)、美沙拉嗪(mesalamine)、美他沙酮(metaxalone)、甲福明二甲双胍(metformin)、吕太灵(methylphenidate)、甲基脱氢皮质醇(methylprednisolone)、美托洛尔(metoprolol)、咪达唑仑(midazolam)、米力农(milrinone)、二甲胺四环素(minocycline)、米氮平(mirtazapine)、米索前列醇(misoprostol)、米托蒽醌(mitoxantrone)、吗氯贝胺(moclobemide)、莫达非尼(modafinil)、莫米松(mometasone)、孟鲁司特(montelukast)、莫尼氟酯(morniflumate)、吗啡(morphium)、莫西沙星(moxifloxacin)、麦考酚酯(mycophenolate)、萘丁美酮(nabumetone)、nadroparin、萘普生(naproxen)、那拉曲坦(naratriptan)、奈法唑酮(nefazodone)、尼非那韦(nelfinavir)、奈韦拉平(nevirapine)、烟酸、尼卡地平(nicardipine)、尼麦角林(nicergoline)、硝苯地平(nifedipine)、尼鲁米特(nilutamide)、尼伐地平(nilvadipine)、尼莫地平(nimodipine)、硝化甘油、尼扎替丁(nizatidine)、炔诺酮(norethindrone)、诺氟沙星(norfloxacin)、奥曲肽(octreotide)、奥氮平(olanzapine)、奥美拉唑(omeprazole)、昂丹司琼(ondansetron)、奥利司他(orlistat)、奥司他韦(oseltamivir)、雌二醇(oestradiol)、雌激素(oestrogens)、奥沙利铂(oxaliplatin)、奥沙普秦(oxaprozin)、恶喹酸(oxolinic acid)、奥昔 布宁(oxybutynin)、紫杉醇(paclitaxel)、帕利珠单抗(palivizumab)、帕米德诺内(pamidronate)、胰脂肪酶(pancrelipase)、帕尼培南(panipenem)、泮托拉唑(pantoprazole)、扑热息痛(paracetamol)、帕罗西汀(paroxetine)、己酮可可碱(pentoxifylline)、培高利特(pergolide)、苯妥英(phenytoin)、吡格列酮(pioglitazone)、哌拉西林(piperacillin)、吡罗昔康(piroxicam)、普拉克索(pramipexole)、普伐他汀(pravastatin)、哌唑嗪(prazosin)、普罗布可(probucol)、黄体酮、普罗帕酮(propafenone)、普鲁泊福(propofol)、丙氧芬(propoxyphene)、前列腺素(prostaglandin)、quetiapin、喹那普利(quinapril)、雷贝拉唑(rabeprazole)、雷洛昔芬(raloxifene)、雷米普利(ramipril)、雷尼替丁(ranitidine)、瑞格列奈(repaglinide)、利血平(reserpine)、病毒唑(ribavirin)、利鲁唑(riluzole)、利培酮(risperidone)、利托那韦(ritonavir)、利妥昔(rituximab)、依西隆(rivastigmin)、利扎曲普坦(rizatriptan)、罗非昔布(rofecoxib)、罗匹尼罗(ropinirole)、罗格列酮(rosiglitazone)、沙美特罗(salmeterol)、沙奎那韦(saquinavir)、沙格司亭(sargramostim)、舍雷肽酶(serrapeptase)、舍曲林(sertraline)、司维拉姆(sevelamer)、西布曲明(sibutramine)、西地那非(sildenafil)、辛伐他汀(simvastatin)、生长激素(somatropin)、甲磺胺心定(sotalol)、安体舒通(spironolactone)、司他夫定(stavudine)、舒巴坦(sulbactam)、磺胺乙二唑(sulfaethidole)、新诺明(sulfamethoxazole)、水杨酸偶氮磺胺吡啶(sulfasalazine)、舒必利(sulpiride)、舒马普坦(sumatriptan)、他克莫司(tacrolimus)、它莫西芬(tamoxifen)、坦洛新(tamsulosin)、三唑巴坦(tazobactam)、替考拉宁(teicoplanin)、替莫普利(temocapril)、替莫唑胺(temozolomide)、tenecteplase、替诺昔康(tenoxicam)、替普瑞酮(teprenone)、特拉唑嗪(terazosin)、特比萘芬(terbinafine)、特布他林(terbutaline)、破伤风菌疫苗(tetanus toxoid)、四苯喹嗪(tetrabenazine)、tetrazapam、麝香草酚(thymol)、噻加宾(tiagabine)、甲基异炔酮(tibolone)、替卡西林(ticarcillin)、噻氯匹定(ticlopidine)、噻吗洛尔(timolol)、替罗非班(tirofiban)、替扎尼定(tizanidine)、托普霉素(tobramycin)、维生素E烟酸酯(tocopheryl nicotinate)、托特罗定(tolterodin)、托吡酯(topiramate)、拓扑替康(topotecan)、托拉塞米(torasemide)、曲马多(tramadol)、群多普利 (trandolapril)、曲妥珠(trastuzumab)、去炎松(triamcinolone)、三唑仑(triazolam)、曲美布汀(trimebutine)、甲氧苄氨嘧啶(trimethoprim)、曲格列酮(troglitazone)、托烷司琼(tropisetron)、妥洛特罗(tulobuterol)、乌诺前列酮(unoprostone)、尿促卵泡素(urofollitropin)、发昔洛韦(valacyclovir)、丙戊酸、缬沙坦(valsartan)、万古霉素(vancomycin)、文拉法辛(venlafaxine)、戊脉安(verapamil)、维替泊芬(verteporfin)、氨己烯酸(vigabatrin)、长春瑞滨(vinorelbine)、长春西丁(vinpocetine)、伏格列波糖(voglibose)、杀鼠灵(warfarin)、扎鲁司特(zafirlukast)、扎来普隆(zaleplon)、扎那米韦(zanamivir)、齐多夫定(zidovudine)、佐米格(zolmitriptan)、唑吡坦(zolpidem)、佐匹克隆(zopiclone)及其衍生物。但是,活性药物成分也被理解为表示其他物质例如维生素、维生素原、必需脂肪酸、植物和动物来源的提取物、植物和动物来源的油类、植物药物制剂和顺势疗法制剂(homeopathic preparation)。
本发明的粒状二氧化硅可以特别作为载体用于动物添加剂,例如甲酸、丙酸、乳酸、磷酸、氯化胆碱溶液、维生素E乙酸酯或者植物提取物,例如万寿菊提取物。
另外,本发明的粒状二氧化硅可以作为载体材料,用于化学产品例如蜜胺树脂、橡胶添加剂、塑料添加剂,用于建筑化学品的添加剂或者涂料添加剂。
本发明的粒状二氧化硅最优选作为载体材料,用于所有种类的催化剂。该催化剂可以特别优选是酶或者不同酶的组合,例如选自下面种类的酶:氧化还原酶、转移酶、水解酶、脂肪酶、裂解酶、异构酶和连接酶(根据国际生物化学和分子生物学联合会命名委员会的EC(Enzyme Commission)值)。术语“酶”同样还包括例如通过重组技术所生产的酶变体。
为了生产负载的载体或者载体,将本发明的粒状二氧化硅与至少一种待吸收的物质接触,以使得该物质能够渗透到二氧化硅的孔中。为此目的,可以使用本领域技术人员已知的全部技术,例如喷涂、逐滴施涂、浸透、浸渍、喷嘴涂覆等。二氧化硅优选初始加入到固体混合单元例如捏合机、桨式干燥机、转动混合器、垂直混合器、桨式混合器、Schugi混合器、水泥混合器、Gericke连续混合器、Eirich混合器和/或仓筒混合器。根据待吸 收物质的性能和组成,混合单元中的温度优选是5-90°C,更优选10-70°C。混合器中的压力优选是0.1bar-2bar,更优选0.5bar-1.2bar。
被吸收的物质在负载的载体或者载体中的含量是5-70%,优选5-65%,更优选5-60%。术语“被吸收的物质”描述了施用到载体上的全部物质的总和。
本发明的被吸收物质特别优选作为催化剂用于非均相催化领域固定床反应器中、流化床反应器中和用于在悬浮液中进行反应。
具体实施方式
所用原料和本发明的粒状二氧化硅的物理化学数据是通过下面的方法来确定的:
BET表面积的测量
二氧化硅的比氮气表面积(下文称作BET表面积)是根据ISO9277,作为多点表面积来测量的。所用的测量仪器是来自Micromeritics的TriStar 3000表面积测量仪。BET表面积典型地是在液氮的饱和蒸气压的0.05-0.20的分压范围内测量的。样品是如下来制备的:在来自Micromeritics的VacPrep061加热站中,将样品在160°C和真空下加热1小时。
DBP吸收值的测量
DBP吸收值(DBP数),其是二氧化硅吸收性的度量,是基于标准DIN53601如下来测量的。
将12.50g的含水量为3-10%(如果需要,含水量是通过在干燥箱中在105°C干燥来调整的)的二氧化硅引入到来自Brabender的C吸收仪的捏合室中。在C吸收仪上的测量是用使用软件BRABEN DER Automatic OilAbsorption System版本1.1.2用PC载体,以所测量的转矩曲线的固定阻尼来进行的。
在滤饼的情况中,将其在使用前在105°C的干燥箱中干燥到含水量≤10%,并且通过3mm筛子,然后通过300μm筛子。
在125rpm的圆周速度的左手捏合机桨叶处,使用Titronic Universal burette(来自Schott,其形成了C吸收仪的一部分)来将邻苯二甲酸二丁酯以4ml/min的速度逐滴加入到室温捏合室中。断开点(在该点时,C吸收仪的控制软件停止了捏合机和DBP计量)定义为在0.6Nm扭矩的点。
使用下式来计算DBP吸收值[g/100g]:
这里
DBP:DBP吸收值[g/100g]
V:所消耗的DBP[ml]
D:DBP密度[g/ml](在20°C为1.047g/ml)
E:二氧化硅的起始重量[g]
K:根据水分校正表的校正值[g/100g]
DBP吸收值是针对无水的干燥二氧化硅而定义的。在使用未干燥的二氧化硅的情况中,在计算DBP吸收值时应当考虑校正值K。这个值可以使用下表的校正来确定。
表1:用于邻苯二甲酸二丁酯(无水)吸收的水分校正表
实施例:
如果二氧化硅的含水量是5.8%,则将33g/100g的校正值K加到上述的用于DBP吸收值的分析值上。二氧化硅的含水量是通过正文中下面所述的“含水量测量”方法来确定。
通过激光衍射测量粒度
使用激光衍射来测量粉末固体的粒度分布是基于在全部方向上颗粒散射或者衍射来自单色激光束的光的现象,并且具有根据它们尺寸的不同的强度图案。照射的颗粒的直径越小,单色激光束的散射或者衍射角越大。
用于通过激光衍射的粒度测量的样品制备
因为样品颗粒的尺寸部分地超过了所用仪器的测量范围和未超声波曝露的d50与超声波曝露3min后的d50U之比取决于起始粒度(材料的较小颗粒具有较高的所述的尺寸比),因此该测量是在筛出样品的400μm-500μm的颗粒部分后进行的。这种操作允许将不同材料的稳定性可靠地进行比较,来获得关于物质-比稳定性的情况。筛分是用来自Haver&Boecker,59302Oelde的HAVER EML 200Digital Plus筛选机来进行的,其装备有400μm和500μm筛。将5g的起始材料施用到上部的500μm筛子上,并且用1.0的设定振幅过筛2分钟。使用400μm-500μm的颗粒部分来进一步分析。
如果400μm-500μm部分(其对于比较而言是重要的)不是本发明的载体或者载体材料的粒度分布的一部分,相应的筛分是如下来生产:将足够量的起始材料以100次振动/min的速度借助于来自Eweka GmbH,Heusenstamm的TG2S筛子造粒机,通过500μm的筛子,然后通过400μm的筛子筛掉。该过筛是如上所述来完成的。
未超声波曝露的d
50
测量
在亲水二氧化硅的情况中,制备样品,其用于通过LS230激光衍射系统(来自Beckman Coulter;测量范围0.04-2000μm)和液体模块(Small Volume Module Plus,120ml,来自Beckman Coulter,具有整合的超声波 指针),借助于0.05%m/m的在软化水作为分散液体的二磷酸四钠,和在乙醇/水混合物(体积比1:1)作为分散液体的水不能充分润湿的二氧化硅的情况中,进行分析(模块冲洗等)。
在开始分析之前,激光衍射系统必须升温2小时。其后,将SVM模块用分散液体冲洗3次。
应当设定下面的与颗粒分析有关的参数:
分析时间: 60s
测量数: 1
泵速: 75%
光学模型: Fraunhofer
PIDS功能: 失活
偏移分析: 激活
调整: 自动
背景测量: 激活
设定样品浓度: 激活
使用抹刀来加入二氧化硅筛分(400-500μm),直到达到所需的测量浓度,在该浓度时,LS230激光衍射仪给出“OK”的信息。在未超声波曝露情况下泵循环60s来分配二氧化硅悬浮液之后,在室温进行分析。所述软件由原始数据曲线,基于Fraunhofer模型(Fraunhofer.rfd file)来计算粒度分布和未超声波曝露的d50(中值)。
在100%振幅超声波处理3分钟后d
50U
的测量
将存在于LS230激光衍射仪中的二氧化硅悬浮液通过整合在SVM模块(来自Sonics的Vibra Cell VCX130超声波处理器,具有CV181超声波转换器和6mm超声波尖端)的超声波指针,在100%振幅超声波处理180s,同时在液体模块中泵送循环来重新分散,并且如上所述来分析。
所述软件由原始数据曲线基于Fraunhofer模型(Fraunhofer.rfd file)来计算粒度分布和超声波曝露3分钟之后的d50U(中值)。
通过动态图像评价测量粒度
在动态图像评价中,散装材料流向下落到光源和照相机之间。将颗粒作为发射区域进行检测,用计算机程序数字化和转化成粒度。
dQ3=10%和dQ3=90%的确定
为了测量粒度,使用了来自RETSCH Technology GmbH,Haan的CAMSIZER。借助于具有存储通道的DR100-40计量通道,将颗粒供给到测量仪器。对于图像评价来说,应当使用版本3.12d的软件。
在开始分析之前,将仪器升温2h。它确保了照明单元和照相机之前的玻璃护罩没有灰尘。将通道和计量通道之间的距离调整到最大粒度的大约3倍。将计量通道直接置于测量仪器上。将大约150ml的样品引入到通道中。在分析任务文件(*.afg)中记录了下面的分析参数:
为了调节计量通道,在软件中记录了下面的设定值:
在数字化图像的评价中,x值是由min(xc)值来计算的。没有使用波形因子:
dQ3=10%和dQ3=90%的输出是在基础参数中测量的:
没有借助于拟合文件对分析数据进行拟合。
含水量的测量
二氧化硅的含水量是根据ISO787-2来测量的。为此目的,将1-4g的样品量在(105±2)℃的干燥箱中干燥2小时,并且根据ISO规范进行评价。这个干燥失重主要由物理结合的水组成。
二氧化硅pH的测量
二氧化硅的pH是作为在室温的含水悬浮液来测量的。将粒化的样品事先捣碎或者研磨。将95g去离子水加入到5g二氧化硅中。通过磁搅拌器将悬浮液搅拌5分钟。其后立即借助于在预期测量范围内校正的pH计(Metrohm780pH计),将悬浮液的pH精确测量到一位小数点位置。
<4μm的水银孔体积的测量
该方法基于根据DIN66133的水银浸入,使用来自Micromeritics的AutoPore IV9520系统。
该方法原理是基于随所施加的压力而变的注射到多孔固体中的水银体 积的测量。这仅仅覆盖了在所施加的压力(最大414MPa)下水银能够渗透到其中的孔(Ritter和Drake方法)。
非润湿性液体仅仅在压力下渗透到多孔体系中。所消耗的压力是与孔口的内径成反比例的。对于圆柱形孔,孔半径rp和压力p之间的关系是通过Washburn等式来给出的:
rp:孔半径
p:压力
σ:表面张力(480mN/m*)
θ:水银的接触角(140°*)
*根据DIN66133
<4μm的水银孔体积是由直径<4μm到AutoPore IV9520水银孔隙率计检测极限(最大压力414MPa)的全部孔的累积孔体积来计算的。
下面的实施例目的是详细说明本发明,而非限制其范围。
实施例1
将来自Evonik Degussa GmbH的在混合器(来自Somakon,MP-L1)中与添加的200ml水/100g二氧化硅混合并压实。这是使用0.5L混合容器在23℃的温度进行的,该混合容器装备有标准的混合十字架。在2200rpm的混合速率,在20s内将30g水计量到称重为15g的二氧化硅中,然后将该混合物混合直到粒化。一旦形成了表面上稍微潮湿的5mm聚集体,则停止操作。将所获得的颗粒在160℃的干燥箱中干燥到恒重,然后通过500μm的筛子,并且在进一步的步骤中通过400μm的筛子过筛。将因此获得的400–500μm的筛分用于随后测试硬度和孔隙率。
实施例2
将来自Evonik Degussa GmbH的在混合器(来自Somakon,MP-L1)中与添加的270ml水/100g二氧化硅混合并压实。这是使用0.5L混合容器在23℃的温度进行的,该混合容器装备有标准的混合十字架。在2200rpm的混合速率,在20s内将40.5g水计量到称重为15g的二氧化 硅中,然后将该混合物混合直到粒化。一旦形成了表面上稍微潮湿的5mm聚集体,则停止操作。将所获得的颗粒在160°C的干燥箱中干燥到恒重,然后通过500μm的筛子,并且在进一步的步骤中通过400μm的筛子过筛。将因此获得的400-500μm的筛分用于随后测试硬度和孔隙率。
实施例3
将实施例2所生产的载体或者载体二氧化硅样品在110°C的水蒸汽气氛中存储16h,然后在120°C干燥到恒重,并用于随后测试硬度和孔隙率。
实施例4
将固含量大约25%的滤饼 22(来自Evonik Degussa GmbH)悬浮液以预先粉碎的形式引入到鼓式造粒机(来自RWK)中。在20%的填充水平时,速度8rpm,批次时间(batch time)90分钟和加热温度120°C形成了干燥颗粒。该颗粒随后在筛子造粒机中(来自Frewitt,MG633)用1250μm的筛子嵌入物压碎到规定的最大粒度。为了获得无尘产品,通过400μm的筛子过筛(来自Gough,Vibrecon GV2/1, )来除去细颗粒。这些细颗粒可以与滤饼一起用于接下来的粒化批次中。将所获得的颗粒在160°C的干燥箱中干燥到恒重,然后通过500μm的筛子,并且在进一步的步骤中通过400μm筛子过筛。将因此获得的400-500μm筛分用于随后测试硬度和孔隙率。
实施例5
将固含量大约25%的滤饼 22(来自Evonik Degussa GmbH)悬浮液以预先粉碎的形式引入到鼓式造粒机(来自RWK)中。在20%的填充水平时,速度8rpm,批次时间90分钟和加热温度120°C形成了干燥颗粒。
将因此获得的5.0g颗粒称重到瓷盘(质量:154g;直径:120mm)中,并且置于预热到1000°C的实验室炉子(Nabertherm)中。5分钟后,除去样品,并且将其立即转移到冷的玻璃容器中。将冷却的颗粒随后通过500μm筛子,和在进一步的步骤中用400μm筛子过筛。将因此获得的400-500μm筛分用于随后测试硬度和孔隙率。
实施例6
将来自Evonik Degussa GmbH的 22在压实机(来自Bepex,L200/50)中以40kN的辊子接触压力进行压实。将压实物随后在筛子造粒机(来自Frewitt,MG633)中用2800μm筛子嵌入物压碎到规定的最大粒度。为了获得无尘产品,通过400μm的筛子过筛(来自Gough,Vibrecon GV2/1, )来除去粒化形成的细颗粒,并且再循环到压实机的初始加料中。为了测试,将颗粒通过500μm的筛子过筛,并且在进一步的步骤中通过400μm筛子过筛。将因此获得的400-500μm筛分用于随后测试硬度和孔隙率。
实施例7
将来自Evonik Degussa GmbH的 50S在混合器(来自Somakon,MP-L1)中与添加的233ml水/100g二氧化硅混合和压实。这是使用0.5L混合容器在23°C的温度进行的,该混合容器装备有标准的混合十字架。在2200rpm的混合速率,在20s内将35g水计量到称重为15g的二氧化硅中,然后将该混合物混合直到粒化。一旦形成了表面上稍微潮湿的5mm聚集体,则停止操作。将所获得的颗粒在160°C的干燥箱中干燥到恒重,然后通过500μm的筛子,并且在进一步的步骤中通过400μm的筛子过筛。将因此获得的400-500μm的筛分用于随后测试硬度和孔隙率。
本发明实施例1-7的二氧化硅的理化性能列于下表2中。
对比例
表2包含了现有技术的对比二氧化硅理化性能的数据。对比例A和B相应于来自Evonik Degussa GmbH的 7000GR和 VN3GR。对比例C包括来自于Rhodia Chimie的 165 对比例D包括来自于Huber的Zeodent DP-9175。对比例A-C的二氧化硅商业上用于增强汽车轮胎橡胶。
表2:
A | 1.83 | 21.34 | 439 | 6292 |
B | 1.63 | 5.40 | 955 | 5538 |
C | 1.60 | 16.67 | 316 | 5311 |
D | 1.31 | 1.74 | 299 | 603 |
在表2中,实施例1和2清楚的表明,通过起始二氧化硅的压实所引起的颗粒的稳定性(通过未超声波曝露的d50U与超声波曝露3min后的d50之比来度量)在增湿过程中随着含水量的降低而升高。但是,与此同时,用Hg孔体积所表示的吸收性降低。
所述的生产方法确保了实施例1-7的产品具有仅仅非常小的细颗粒部分,这是用大于400μm的dQ3=10%来表示的。
另外,实施例3表明本发明的二氧化硅的后处理产生了颗粒稳定性令人惊讶的明显增加,并且具有基本上不改变的孔隙率。
实施例5表明煅烧能够实现具有极高硬度的颗粒。
在对比例A-C中所测试的载体或者载体二氧化硅具有相当高的吸收率,但是不适于在催化方法中使用,因为它们具有过低的硬度(用d50与d50U之比来表征)。另外,dQ3=90%值明显大于3000μm,作为其结果,反应物和产物在二氧化硅孔体系中的扩散路径作为催化剂载体应用而言是过长的。
在对比例D中所测试的载体或者载体二氧化硅显著的特点在于足够的吸收率和硬度,但是具有过低的dQ3=10%,其导致了反应器中压降的增加和被吸收物质流动阻力的增加。
这证实了本发明的粒状二氧化硅具有足够低的细颗粒含量,和因此同时产生了足够的稳定性和孔隙率,这明显不同于目前通常市售使用的载体或者载体二氧化硅。
Claims (33)
1.一种粒状二氧化硅,其具有
-<4μm直径的Hg孔体积大于0.90ml/g,
-dQ3=10%大于400μm,同时dQ3=90%小于3000μm,和
-未超声波曝露的d50与超声波曝露3min后的d50之比<4.00,该测量是在400-500μm的颗粒部分上进行的,
其中粒度分布用dQ3=10%和dQ3=90%表征,并且使用来自Haan的RETSCHTechnology GmbH的CAMSIZER确定dQ3=10%和dQ3=90%,孔隙率用Hg孔体积表示,并且<4μm直径的Hg孔体积是由从直径<4μm到最大压力为414MPa的AutoPore IV9520水银孔隙率计的检测极限的全部孔的累积孔体积来计算的。
2.根据权利要求1的粒状二氧化硅,特征在于其pH是5-8.5。
3.根据权利要求1或2的粒状二氧化硅,特征在于其具有的未超声波曝露的d50与超声波曝露3min后的d50之比是1.00-3.00,这个测量是在400-500μm的颗粒部分上进行的。
4.根据权利要求3的粒状二氧化硅,其中所述d50之比为1.00-2.60。
5.根据权利要求4的粒状二氧化硅,其中所述d50之比为1.00-2.10。
6.根据权利要求5的粒状二氧化硅,其中所述d50之比为1.00-1.60。
7.根据权利要求1或2的粒状二氧化硅,特征在于其<4μm直径的Hg孔体积大于1.35ml/g。
8.根据权利要求7的粒状二氧化硅,其<4μm直径的Hg孔体积大于1.60ml/g。
9.根据权利要求8的粒状二氧化硅,其<4μm直径的Hg孔体积大于1.80ml/g。
10.根据权利要求9的粒状二氧化硅,其<4μm直径的Hg孔体积大于1.90ml/g。
11.根据权利要求1或2的粒状二氧化硅,特征在于其<4μm直径的Hg孔体积是0.9-1.34ml/g。
12.根据权利要求11的粒状二氧化硅,其中其<4μm直径的Hg孔体积是是0.9ml/g-1.30ml/g。
13.根据权利要求12的粒状二氧化硅,其中其<4μm直径的Hg孔体积是是0.9ml/g-1.20ml/g。
14.一种生产根据权利要求1的粒状二氧化硅的方法,其包含步骤:
a)提供沉淀的或者气相法二氧化硅,其是干燥的和/或研磨的形式,并且具有
-未超声波曝露的平均粒度d50是0.1-350μm,
-BET表面积是30-800m2/g,和
-DBP值是140-400g/100g;
b)根据30-80重量%的干燥失重所用的成形方法,增湿来自步骤a)的二氧化硅;
c)通过挤出、粒化、压实或者其他常规成形方法使来自步骤b)的二氧化硅成形;
d)在适于此的干燥单元中,干燥该成形的二氧化硅体;和
e)以3000μm的筛孔尺寸过筛粒化或者过筛所述颗粒,并且用400μm筛孔尺寸筛掉细颗粒。
15.根据权利要求14的方法,特征在于步骤b)的二氧化硅是干燥失重为30-80重量%的含水滤饼的形式。
16.根据权利要求14的方法,特征在于来自步骤b)的二氧化硅在步骤c)中在高速强力混合器中被压实和粒化。
17.一种生产根据权利要求1的粒状二氧化硅的方法,其包含步骤:
i)提供沉淀的或者气相法二氧化硅,其是干燥的和/或研磨的形式,并且具有的干燥失重<30重量%,和具有
-未超声波曝露的平均粒度d50是0.1-350μm,
-BET表面积是30-800m2/g,和
-DBP值是140-400g/100g;
ii)通过干压实,以0.5kN/cm辊宽-12kN/cm辊宽的特定接触压力使来自步骤i)的二氧化硅成形,产生小块,和
iii)以3000μm的筛孔尺寸过筛粒化或者过筛所述颗粒,并且用400μm筛孔尺寸筛掉细颗粒。
18.根据权利要求17的方法,其中通过在两个旋转辊之间干压实使来自步骤i)的二氧化硅成形。
19.根据权利要求14-18任一项的方法,特征在于除去全部的小于400μm的筛分。
20.根据权利要求14或18的方法,特征在于成形步骤c)和ii)是在不加入粘合剂的情况下进行的。
21.根据权利要求1-13任一项的粒状二氧化硅的用途,其用于生产被吸收物质。
22.一种被吸收物质,其包含至少一种根据权利要求1-13任一项的粒状二氧化硅。
23.根据权利要求22的被吸收物质,特征在于其包含至少一种催化活性物质。
24.根据权利要求22或23的被吸收物质,特征在于该被吸收的物质的使用比例是1-70重量%。
25.根据权利要求24的被吸收物质,其中,该被吸收的物质的使用比例是3-60重量%。
26.根据权利要求25的被吸收物质,其中,该被吸收的物质的使用比例是5-50重量%。
27.根据权利要求22或23的被吸收物质,特征在于活性物质或者活性物质混合物的使用比例是1-20重量%。
28.根据权利要求27的被吸收物质,其中所述活性物质或者活性物质混合物的使用比例是3-20重量%。
29.根据权利要求28的被吸收物质,其中所述活性物质或者活性物质混合物的使用比例是5-15重量%。
30.根据权利要求22-29任一项的被吸收物质的生产方法,特征在于将根据权利要求1-13任一项的粒状二氧化硅与选自下面的至少一种液体接触:硬化剂或者引发剂、交联剂、催化剂、活性药物成分和赋形剂、活性化妆品成分和赋形剂、清洁和/或护理组合物、调味剂、芳香剂和香味剂、动物饲料或者动物饲料添加剂、食品或者食品添加剂、染料和/或颜料、氨基酸、氧化或者漂白剂、具有杀微生物作用、特别是杀真菌或者杀菌作用的添加剂、用于农业和林业的化学品、和/或混凝土混合物。
31.根据权利要求22-29任一项的被吸收物质的用途,其用于催化方法中。
32.根据权利要求31的用途,特征在于该催化方法是在固定床反应器、流化床反应器中进行的,或者通过将被吸收物质悬浮于反应混合物中来进行的。
33.根据权利要求31或32的用途,特征在于被吸收物质包含在根据权利要求1-13任一项的粒状二氧化硅上作为催化剂的酶。
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ES2908958T3 (es) * | 2013-02-01 | 2022-05-04 | Grace W R & Co | Gel de sílice porosa como portador para tecnologías líquidas |
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WO2016171753A1 (en) * | 2015-04-22 | 2016-10-27 | The United States Of America As Represented By The Secretary Of The Navy | Insect control formulation with improved autodissemination characteristics |
RU2613917C2 (ru) * | 2015-07-06 | 2017-03-22 | Общество с ограниченной ответственностью "Эмпилс - Цинк" | Способ гранулирования порошков и оборудование для его осуществления |
DE102015216505A1 (de) * | 2015-08-28 | 2017-03-02 | Wacker Chemie Ag | Silica Formkörper mit geringer thermischer Leitfähigkeit |
CN106115720B (zh) * | 2016-08-14 | 2017-07-14 | 皖西学院 | 一种利用稻壳灰制备纳米二氧化硅的方法 |
JP6855583B2 (ja) | 2017-02-27 | 2021-04-07 | ワッカー ケミー アクチエンゲゼルシャフトWacker Chemie AG | 疎水性シリカ顆粒の製造法 |
RU2708003C1 (ru) * | 2019-03-21 | 2019-12-03 | Акционерное общество "Обнинское научно-производственное предприятие "Технология" им. А.Г. Ромашина" | Способ получения гранулята кремния для аддитивного производства изделий из реакционносвязанных нитридов и карбидов кремния |
CN111303993A (zh) * | 2020-03-20 | 2020-06-19 | 佳格食品(中国)有限公司 | 一种新型环保吸附剂在高效吸附植物油风险物质中的应用 |
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Publication number | Publication date |
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CN102821842A (zh) | 2012-12-12 |
KR20130018700A (ko) | 2013-02-25 |
WO2011117100A1 (de) | 2011-09-29 |
ES2651742T3 (es) | 2018-01-29 |
DE102010003204A1 (de) | 2011-12-15 |
ZA201207135B (en) | 2013-05-29 |
AR080715A1 (es) | 2012-05-02 |
RU2012145006A (ru) | 2014-04-27 |
JP5777697B2 (ja) | 2015-09-09 |
PT2550095T (pt) | 2017-12-18 |
EP2550095A1 (de) | 2013-01-30 |
HUE035792T2 (en) | 2018-05-28 |
MX2012010878A (es) | 2012-10-15 |
EP2550095B1 (de) | 2017-10-18 |
BR112012024021A2 (pt) | 2016-08-30 |
JP2013525239A (ja) | 2013-06-20 |
RU2551858C2 (ru) | 2015-05-27 |
TWI534083B (zh) | 2016-05-21 |
US20120322893A1 (en) | 2012-12-20 |
TW201206827A (en) | 2012-02-16 |
US10752510B2 (en) | 2020-08-25 |
PL2550095T3 (pl) | 2018-03-30 |
BR112012024021B1 (pt) | 2018-07-24 |
CA2794028A1 (en) | 2011-09-29 |
KR101770855B1 (ko) | 2017-08-23 |
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