CN1250761A - 含有热解共混氧化物的模塑物及其用途 - Google Patents
含有热解共混氧化物的模塑物及其用途 Download PDFInfo
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- CN1250761A CN1250761A CN99120378A CN99120378A CN1250761A CN 1250761 A CN1250761 A CN 1250761A CN 99120378 A CN99120378 A CN 99120378A CN 99120378 A CN99120378 A CN 99120378A CN 1250761 A CN1250761 A CN 1250761A
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
基于热成法共混氧化物的模塑物,其具有如下的物化指标:外径0.8—25mm,BET表面积5—400m2/g,孔体积0.2—1.8ml/g,断裂强度5—350N;组成SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能的组合,只是SiO2/Al2O3共混氧化物例外,其中含有> 75wt.%的SiO2。其它成份< 1wt.%,堆积密度250—1500g/l的制备是,将热成法共混氧化物,借助选自甲基纤维素、甲基羟乙基纤维素、蜡、硬脂酸镁、硬脂酸铝或聚乙二醇的一种或多种化合物以及水的添加而按要求匀质化,产品在70—150℃的温度下干燥,可选粉碎以得到粉体,可选压缩模塑粉体以得到模塑物,并且在400—1200℃的温度下进行热处理0.5—10小时。这些模塑物可以作为水合乙烯或丙烯用的催化剂或催化剂载体。
Description
本发明涉及基于热成法共混氧化物的模塑物、其制备工艺以及其作为催化剂载体或催化剂的用途。
热成法氧化物的特征在于超细度和相当高的比表面积、非常高的纯度、球形粒子状态以及无孔隙性。鉴于这些性能,对热成法氧化物作为催化剂载体(D.Koth,H.Ferch,Chem.Ing.Techn.52,628(1980))的兴趣一直都有增无减。在某些情况下,热解氧化物也用作催化剂。
因为热成法氧化物粉化得特别细,所以在把它们成型为催化剂载体或催化剂时碰到了一些困难。
DE-A31 32 674给出了从热成法氧化物制备压模模塑物的工艺,其中以硅溶胶作粘合剂。
DE-A 34 06 185给出了制备压模模塑物的工艺,其中以釉质玻璃粉作粘合剂以及甘油作润滑剂。
DE-A 39 12 504给出了制备压模模塑物的工艺,其中以硬脂酸铝、硬脂酸镁和/或石墨作润滑剂,脲以及甲基纤维素作成孔剂。
这些压模模塑物以Aerosil片no.350,Degussa有售。它们含有大约0.4wt.%的Mg。
基于热解氧化物的模塑物是已知的。EP-B0 393 356就描述了基于热成法二氧化硅的高纯模塑物。这些模塑物含有>99wt.%的热成法SiO2并具有低的粘合用物质含量。实施例描述了硬脂酸Mg和Al的使用。
DE-A 196 19 961描述了基于热成法二氧化硅的模塑物。这些模塑物的纯度已提高到>99.8wt.%的SiO2。
文献EP-B 0452 619、EP-B 0 394 677和EP-B 0 327 723描述了基于热成法二氧化钛的模塑物。这些模塑物的差异尤其体现在其锐钛矿含量、金红石含量、纯度、尺寸等。二氧化钛含量据说可达>99wt.%、>99.5wt.%和>94wt.%。在后一种情况中,锐钛矿的含量至少是50wt.%,余下的0-6wt.%则由非热成法SiO2和/或非热成法Al2O3构成。
EP-B 0 327 721描述了基于热成法Al2O3的模塑物。纯度据说达到94-99wt.%的Al2O3含量。余下的1-6wt.%为SiO2。SiO2成份来自于在氧化铝粉末成型过程中所采用的高岭土。
基于热成法ZrO2的模塑物更是已知的。这些在文献EP-B 0 327 814中有描述。这些物质的纯度据说达>92wt.%的二氧化锆含量。在这里也是,余下的部分由非热成法SiO2和Al2O3级份构成。也存在有少部分的HfO2,这是ZrO2中的天然杂质。
基于热成法氧化物的现有模塑物可以用作催化剂或催化剂载体。高的纯度和好的机械和化学性能在许多应用领域中起到了重要的作用。
更为已知的是,为了特定的用途,通过有目的地加入某种外来元素而对模塑物组合物改性。此例在文献EP-A 0 723 810中有描述。提到了含有SiO2的载体,其组成通过浸渍Al、Zr和/或Ti而改变。模塑物浸渍后,进行干燥并煅烧。
此类已知的制备方法是昂贵的,因通过浸渍、干燥及煅烧的方法对基体物质进行改性对设备和能量有很高的要求。而且,改性模塑物的制备时间显著加长。
已知制备热解共混氧化物是,至少两种不同的金属以挥发金属化合物的形式,比如氯化物,在H2/O2焰中同时发生反应。此类氧化物的一个例子是SiO2/Al2O3共混氧化物,由Degussa提供,以商品名AerosilMOX 170有售。在制备AerosilMOX 170时,SiCl4和AlCl3的混合物在火焰中直接水解。相应的硅烷,比如甲基三氯硅烷、三氯硅烷等也可以作为氯化物替代用原料或额外组分。(DegussaTechnical Bulletin Pigments,No.11:Basic Characteristics ofAerosil,pp.37,11-12;AT-A 195 893;DE-A 952 891;DE-A 33 925;DE-A 27 02 896)。
更为已知的是基于热成法二氧化硅/氧化铝共混氧化物模塑物(EP-B 0 327 815)的制备。这些共混氧化物含有至少75wt.%的二氧化硅和至多25wt.%的氧化铝。
本发明提供了基于热成法共混氧化物的模塑物,它具有如下的物化指标:
外径 0.8-25mm
BET表面积 5-400m2/g
孔体积 0.2-1.8ml/g
断裂强度 5-350N
组成 SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能
的组合,只是SiO2/Al2O3共混氧化物例外,其中含
有>75wt.%的SiO2。
其它成份 <1wt.%
堆积密度 250-1500g/l
本发明的模塑物可以加工成挤出模塑物、挤出物或片体。其形态可以呈现为圆柱、具圆端面的圆柱、球形、环状、车轮状、小碎块或其它固定床催化剂常见的形状。
本发明也提供了制备基于热成法氧化物模塑物的工艺,其具有如下的物化指标:
外径 0.8-25mm
BET表面积 5-400m2/g
孔体积 0.2-1.8ml/g
断裂强度 5-350N
组成 SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能
的组合,只是SiO2/Al2O3共混氧化物例外,其中含
有>75wt.%的SiO2。
其它成份 <1wt.%
堆积密度 250-1500g/l其工艺特征在于热成法共混氧化物,借助选自甲基纤维素、甲基羟乙基纤维素、蜡、硬脂酸镁、硬脂酸铝或聚乙二醇的一种或多种化合物以及水的添加而按要求匀质化,在70-150℃的温度下干燥,可选粉碎以得到粉体,粉体经压缩模塑得到模塑物,并且在400-1200℃的温度下热处理0.5-10小时。
本发明的模塑物可以在印模压机、偏心式压机、等静态压机、挤出压机、旋转压机或捣碎机中制备。
在压制前,在本发明的一个特定的实施方案中,混合物具有如下的组成:
50-90wt.% 共混氧化物
0.1-20wt.% 甲基羟乙基纤维素,优选5-15wt.%
0.1-15wt.% 蜡,优选5-12wt.%
0.1-15wt.% 聚乙二醇,优选5-10wt.%
通过改变起始物质的用量以及压制压力,可以对断裂强度、总比表面积和孔体积在一定范围调整。
本发明也提供了制备基于热成法氧化物模塑物的工艺,其具有如下的物化指标:
外径 0.8-25mm
BET表面积 5-400m2/g
孔体积 0.2-1.8ml/g
断裂强度 5-350N
组成 SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能
的组合,只是SiO2/Al2O3共混氧化物例外,其中含
有>75wt.%的SiO2。
其它成份 <1wt.%
堆积密度 250-1500g/l其工艺特征在于热成法共混氧化物,借助选自甲基纤维素、甲基羟乙基纤维素、蜡、硬脂酸镁、硬脂酸铝或聚乙二醇的一种或多种化合物以及水的添加而按要求匀质化,经过捏合及成型加工后挤出,挤出物可选以切割设备切成所要求的长度,在70-150℃的温度下干燥,并且在400-1200℃的温度下热处理0.5-10小时。
任何能提供良好匀质化的混合器或磨,比如桨式混合器、流化床混合器、离心式混合器或空气活塞式混合器,都适宜进行本发明的工艺。那些物料在混合时能额外被密实的混合器是特别适宜的,比如犁条式混合器、碾式磨或球磨机。但是,混合和捏合也可以直接在挤出机中实现。也可以以单或双螺杆挤出机、挤出压机或捣碎机制备挤出物。
匀质化后,产品在70-150℃充分干燥,以便在一个可选的粉碎操作之后,得到易流动的粉体。
本发明的模塑物可以直接作为催化剂或用作催化剂载体。在后一种情况中,模塑物一经制备,就与催化活性物质接触,并可选经适当的后处理活化。
本发明自热成法共混氧化物制备的模塑物在烯烃水合工艺中特别用作催化剂载体。
本发明的模塑物具有如下的优点:
同文献EP 0 723 810 A1和EP 0 792 859 A2的模塑物相比,本发明模塑物的制备非常简单,并对能量、时间和设备的需求较低。
本发明的模塑物在水合工艺中表现出改进的水热稳定性。
催化剂在使用过程中会经历老化,导致活性和/或选择性的降低。失活经常是因为高温所致的载体比表面积的降低。
载体的比表面积与其孔结构密切相关。而且,大比表面积固体一般具有完全无定形或大体无定形的结构,具有转变成热力学稳定态的倾向,伴随晶体的生长和比表面积的降低。
已发现含二氧化硅的已知催化剂载体也经历这种老化行为。水合条件加速老化。更为已知的是杂质,尤其是碱金属,会加速水合条件下含二氧化硅载体的老化(参考文献比如R.K.Iler的“The Chemistryof Silica”,pp.544,John Wiley&Sons(1979))。
EP 0 393 356所述的基于热成法二氧化硅的催化剂载体在水合条件下也经历老化,其中小的孔隙融汇成大的孔洞以至比表面积的损失。但是,孔体积几乎不变。
如EP 0 792 859 A2所述,通过添加Ti和/或Zr可改进老化稳定性。在此专利中,这些元素通过浸渍而附到SiO2模塑物上,继以干燥和煅烧。一如前文所解释,这些附加步骤需要时间、能量和设备。
因此,本发明的目的是给出催化剂载体,其在水热条件下使用时表现出改进的老化稳定性。
利用催化剂,其含有一种载在本发明基于热成法共混氧化物模塑物上的活性成份,更好地实现了本文稳定性的目的。
本发明更提供一种对烯烃水合以制备相应醇的工艺,在磷酸或其它活性成份如杂多酸作为催化剂装载于本发明基于热成法共混氧化物的模塑物上的存在下进行。
一种可以采用本发明基于热成法共混氧化物模塑物的工艺,其描述比如见文献EP-A 0 578 441。在此工艺中,水和乙烯在温度225-280℃、压力20-240巴下发生反应形成乙醇。此工艺中采用的水∶乙烯的摩尔比为0.15-0.5。催化剂的荷载,按每分钟及每毫升催化剂的水/乙烯混合物的克数计量,可在0.01-0.1g/(min×ml)范围内选择。此反应中乙醚作为副产物生成。
在相似的条件下水合丙烯以制备异丙醇,但温度稍低,在180-225℃范围。此反应中正丙醇作为副产物生成。
EP 0 578 441 A2的合成二氧化硅小球,其具有高的断裂强度、高的孔隙度和低的金属杂质含量,是用于磷酸活性成份的已知催化剂载体。
本发明的用途对于烯烃水合特别有利。载体的稳定性对其它在水热条件下进行的催化反应也有益。
烯烃水合时,磷酸作为活性成份装载在催化剂载体上。为此,载体浸入磷酸水溶液中并随后浸渍。为此而采用的磷酸溶液含有15-85wt.%的磷酸,相对于溶液的总量。
烯烃水合的一个主要用途是将乙烯水合以制备乙醇和乙醚,以及丙烯水合以制备异丙醇。现有技术已知的反应条件在这里也适用。
本发明进一步的目的是给出催化剂,其在水热条件下应用时表现出改进的老化稳定性。
此目的的实现是通过一种磷酸催化剂,其含有1-50wt.%的磷酸,相对于催化剂的总量,装载在本发明的模塑物上。此催化剂的特征在于基于热成法共混氧化物的模塑物具有如下的物化指标:
外径 0.8-25mm
BET表面积 5-400m2/g
孔体积 0.2-1.8ml/g
断裂强度 5-350N
组成 SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能
的组合,只是SiO2/Al2O3共混氧化物例外,其中含
有>75wt.%的SiO2。
其它成份 <1wt.%
堆积密度 250-1500g/l
以磷酸作为活性成份表面改性模塑物以制备本发明的催化剂。为此,载体粒子或模塑物浸入磷酸水溶液中并随后浸渍,从而以磷酸溶液填充载体粒子的孔体积。为此采用的磷酸溶液含有15-85wt.%的磷酸,相对于溶液的总量。有赖于载体粒子的特定孔体积,所述的粒子可以以1-50wt.%的H3PO4表面改性,相对于成品催化剂的总量。
将挥发性金属化合物注射到氢气和空气的爆鸣气火焰中,以制备共混氧化物。这些金属化合物在爆鸣气生成水的作用下水解,产生金属氧化物和盐酸。离开火焰后,金属氧化物进入所谓的凝聚区,共混氧化物的初级粒子和初级聚集体在此中凝聚。而产品,在此阶段是一种气溶胶态,在旋风分离器中同气态伴生物分离后,以潮湿的热空气后处理。经由此工艺,残余盐酸的含量可能降低到低于0.025wt.%。因为经过此工艺得到的共混氧化物的堆积密度只有约15g/l,因此真空密实可以随后进行,借此可能达到约50g/l或更高的填充密度。
改变反应条件,如火焰温度、氢或氧含量、金属氯化物的品质和用量、火焰中的停留时间或凝结区域的长度,可以改变此法制备的产品粒径。
按照DIN 66 131以氮气测定BET比表面积。孔体积根据微、中和大孔体积的总和计算。采用Erweka公司的断裂强度测定仪TBH 28型测定断裂强度。
通过记录N2等温线测定微孔和中孔,并根据BET,de Boer和Barret,Joyner,Halenda对其进行评价。
以本领域技术熟练人员所知的常用方法测定堆积密度。
采用Hg渗透法测定大孔。
实施例1
71.4wt.% 热解SiO2/TiO2共混氧化物(70wt.%SiO2,30wt.%TiO2)
12.9wt.% 甲基羟乙基纤维素
7.1wt.% 蜡
8.6wt.% 聚乙二醇在添加水的条件下密实,于90℃干燥,粉碎以得到可流动的粉体,并采用偏心式压机成型为模塑物。粗片体在750℃煅烧6小时。实施例2
71.4wt.% 热解SiO2/TiO2共混氧化物(82wt.%SiO2,18wt.%TiO2)
12.9wt.% 甲基羟乙基纤维素
7.1wt.% 蜡
8.6wt.% 聚乙二醇在添加水的条件下密实,于100℃干燥,粉碎以得到可流动的粉体,并采用偏心式压机成型为模塑物。粗片体在700℃煅烧6小时。实施例3
71.4wt.% 热解SiO2/TiO2共混氧化物(91wt.%SiO2,9wt.%TiO2)
12.9wt.% 甲基羟乙基纤维素
7.1wt.% 蜡
8.6wt.% 聚乙二醇在添加水的条件下密实,于100℃干燥,粉碎以得到可流动的粉体,并采用偏心式压机成型为模塑物。粗片体在600℃煅烧10小时。实施例4
71.4wt.% 热解SiO2/TiO2共混氧化物(91wt.%SiO2,9wt.%TiO2)
12.9wt.% 甲基羟乙基纤维素
7.1wt.% 蜡
8.6wt.% 聚乙二醇在添加水的条件下密实,于100℃干燥,粉碎以得到可流动的粉体,并采用偏心式压机成型为模塑物。粗片体在750℃煅烧6小时。实施例5
90.0wt.% 热解SiO2/ZrO2共混氧化物(94wt.%SiO2,6wt.%ZrO2)
5.0wt.% 甲基羟乙基纤维素
2.0wt.% 蜡
3.0wt.% 聚乙二醇在添加水的条件下密实,于100℃干燥,粉碎以得到可流动的粉体,并采用偏心式压机成型为模塑物。粗片体在400℃煅烧10小时。实施例6
92.6wt.% 热解SiO2/ZrO2共混氧化物(94wt.%SiO2,6wt.%ZrO2)
0.9wt.% 甲基羟乙基纤维素
6.5wt.% 蜡在添加水的条件下密实,于100℃干燥,粉碎以得到可流动的粉体,并采用偏心式压机成型为模塑物。粗片体在400℃煅烧10小时。
按照实施例1-6制备的模塑物具有如下的物化指标:
实施例 | 1 | 2 | 3 | 4 | 5 | 6 |
片体形状 | 圆柱 | 圆柱 | 圆柱 | 圆柱 | 环状 | 环状 |
外径×高度×内径(mm) | 5×5 | 6×5.5 | 6×5.5 | 5×5 | 8×5×3 | 8×5×3 |
BET表面积(m2/g) | 86 | 101 | 209 | 191 | 44 | 46 |
孔体积(ml/g) | 0.69 | 0.59 | 0.83 | 0.72 | 0.34 | 0.42 |
断裂强度(N) | 21 | 34 | 37 | 66 | 15 | 12 |
堆积密度(g/l) | n.d. | 610 | 505 | n.d. | 860 | 800 |
本发明催化剂老化稳定性的研究:
通过测定老化催化剂的孔结构,即在载体用磷酸浸渍和水热老化之后,对本发明催化剂和现有技术的对比催化剂在水热条件下的老化稳定性进行研究。以汞孔度仪测定孔结构。未老化的催化剂(本发明和对比催化剂)具有介于0.01-0.05μm的孔隙。
图示
图1 本发明实施例1模塑物上老化催化剂的孔尺寸分布
图2 本发明实施例2模塑物上老化催化剂的孔尺寸分布
图3 本发明实施例3模塑物上老化催化剂的孔尺寸分布
图4 本发明实施例8模塑物上老化催化剂的孔尺寸分布
图1-4所示的孔尺寸分布曲线表明,汞的微分渗透度(浸入度)是孔直径的函数。微分浸入度以任意单位表示,曲线在每种情况下都跨越整个图例的有效面积。
实施例7
实施例1、2和3的催化剂载体分别浸入60wt.%的磷酸溶液,然后在高压设备中暴露于压力15巴和温度350℃的水蒸气中40小时。以汞孔度仪测定老化催化剂的孔尺寸分布。
图1-3是图示的结果。如图可见,已产生了孔隙增大现象,因为如前文所述,未老化物质的孔隙在范围0.01-0.05μm内。实施例8(比较例)
已知的压缩模塑物(催化剂载体350,Degussa,含有0.4wt.%的Mg(元素),BET比表面积180m2/g,堆积密度490g/l,总孔体积0.8cm3/g,片体直径6mm及高度5.5mm)装载磷酸(60wt.%)后,在高压设备中暴露于压力15巴和温度350℃的水蒸气中41小时。以汞孔度仪测定老化催化剂的孔尺寸分布。图4是图示的结果。
水热老化的载体在孔径20-30μm区域出现孔尺寸分布的最大值。同图1-3的本发明的物质相比,直径小于10μm的孔隙的比例相当低。因此,本发明的物质明显地对水热老化更稳定。
Claims (11)
1.基于热成法共混氧化物的模塑物,具有如下的物化指标:
外径 0.8-25mm
BET表面积 5-400m2/g
孔体积 0.2-1.8ml/g
断裂强度 5-350N
组成 SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能
的组合,只是SiO2/Al2O3共混氧化物例外,其中含
有>75wt.%的SiO2,
其它成份 <1wt.%
堆积密度 250-1500g/l
2.权利要求1的基于热成法共混氧化物的模塑物的制备工艺,模塑物
具有如下的物化指标:
外径 0.8-25mm
BET表面积 5-400m2/g
孔体积 0.2-1.8ml/g
断裂强度 5-350N
组成 SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能
的组合,只是SiO2/Al2O3共混氧化物例外,其中含
有>75wt.%的SiO2,其它成份 <1wt.%堆积密度 250-1500g/l
其特征在于热成法共混氧化物,借助选自甲基纤维素、甲基羟乙基纤维素、蜡、聚乙二醇、硬脂酸镁或硬脂酸铝的一种或多种化合物以及水的添加而按要求匀质化,在70-150℃的温度下干燥,可选粉碎以得到粉体,粉体经压缩模塑得到模塑物,并且在400-1200℃的温度下热处理0.5-10小时。
3.权利要求1的基于热成法共混氧化物的模塑物的制备工艺,模塑物
具有如下的物化指标:
外径 0.8-25mm
BET表面积 5-400m2/g
孔体积 0.2-1.8ml/g
断裂强度 5-350N
组成 SiO2、Al2O3、TiO2和ZrO2中至少两个的任何可能
的组合,只是SiO2/Al2O3共混氧化物例外,其中含
有>75wt.%的SiO2,
其它成份 <1wt.%
堆积密度 250-1500g/l
其特征在于热成法共混氧化物,借助选自甲基纤维素、甲基羟乙基纤维素、蜡、聚乙二醇、硬脂酸镁或硬脂酸铝的一种或多种化合物以及水的添加而按要求匀质化,经过捏合及成型加工后挤出,挤出物可选切割或粉碎成所要求的长度,在70-150℃的温度下干燥,并且在400-1200℃的温度下热处理0.5-10小时。
4.权利要求1模塑物的用途,作为催化剂或催化剂载体。
5.磷酸催化剂,其含有1-50wt.%的H3PO4,相对于催化剂总量,装载在成型的无机载体上,其特征在于载体由权利要求1的模塑物组成。
6.催化剂用于水热条件下催化反应的用途,其所含的活性成份载在权利要求1的模塑物上。
7.权利要求6的用途,用于烯烃水合。
8.权利要求7的用途,其特征在于磷酸作为活性成份。
9.权利要求7的用途,其特征在于杂多酸被涂覆作为活性成份。
10.权利要求8或9的用途,用以水合乙烯制备乙醇和乙醚。
11.权利要求8或9的用途,用以水合丙烯制备异丙醇。
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DE19843845.1 | 1998-09-24 | ||
DE19843845A DE19843845A1 (de) | 1998-09-24 | 1998-09-24 | Formkörper, bestehend aus pyrogenem Mischoxid und deren Verwendung |
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CN1250761A true CN1250761A (zh) | 2000-04-19 |
Family
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CN99120378A Pending CN1250761A (zh) | 1998-09-24 | 1999-09-24 | 含有热解共混氧化物的模塑物及其用途 |
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US (1) | US6432869B1 (zh) |
EP (1) | EP0997193A1 (zh) |
JP (1) | JP2000095571A (zh) |
KR (1) | KR20000023397A (zh) |
CN (1) | CN1250761A (zh) |
CA (1) | CA2283040A1 (zh) |
DE (1) | DE19843845A1 (zh) |
ID (1) | ID26671A (zh) |
NO (1) | NO994625L (zh) |
SG (1) | SG92657A1 (zh) |
Cited By (1)
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CN1780827B (zh) * | 2003-05-02 | 2010-06-16 | 帝斯曼知识产权资产管理有限公司 | 母育酚酰化物和生育酚酰化物的制备方法 |
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EP1162179B1 (de) * | 2000-06-10 | 2004-09-15 | Degussa AG | Photokatalytisches Verfahren |
EP1240943A1 (en) * | 2000-10-21 | 2002-09-18 | Degussa AG | Catalyst support |
DE10135452A1 (de) * | 2001-07-20 | 2003-02-06 | Degussa | Pyrogen hergestellte Aluminium-Silicium-Mischoxide |
KR101317503B1 (ko) * | 2004-11-19 | 2013-10-15 | 파나소닉 주식회사 | 난연성 수지 조성물, 그 제조 방법 및 그 성형 방법 |
US7820583B2 (en) * | 2006-08-24 | 2010-10-26 | Millennium Inorganic Chemicals, Inc. | Nanocomposite particle and process of preparing the same |
WO2012114396A1 (ja) | 2011-02-24 | 2012-08-30 | パナソニック株式会社 | 外装体およびその製造方法 |
JP5616972B2 (ja) | 2011-02-24 | 2014-10-29 | パナソニック株式会社 | 外装体およびその製造方法 |
DE102011005608A1 (de) * | 2011-03-16 | 2012-09-20 | Evonik Oxeno Gmbh | Mischoxidzusammensetzungen und Verfahren zur Herstellung von Isoolefinen |
CN103638983B (zh) * | 2013-11-29 | 2017-07-11 | 宁波科森净化器制造有限公司 | 一种使用双层薄板制作的催化剂载体及其制备方法 |
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JPS5335705A (en) * | 1976-09-14 | 1978-04-03 | Toa Nenryo Kogyo Kk | Hydrogenation and purification of petroleum wax |
DE3132674C2 (de) | 1981-08-19 | 1983-12-08 | Degussa Ag, 6000 Frankfurt | Verfahren zur Herstellung von Preßlingen |
DE3406185A1 (de) * | 1984-02-21 | 1985-09-05 | Degussa Ag, 6000 Frankfurt | Verfahren zur herstellung von presslingen aus pyrogen hergestellten oxiden |
DE3611449A1 (de) * | 1986-04-05 | 1987-10-15 | Degussa | Grundstoff zur herstellung von keramischen werkstoffen |
DE3803897A1 (de) | 1988-02-09 | 1989-08-10 | Degussa | Presslinge auf basis von pyrogen hergestelltem aluminiumoxid, verfahren zu ihrer herstellung und ihre verwendung |
DE3803895C1 (zh) * | 1988-02-09 | 1989-04-13 | Degussa Ag, 6000 Frankfurt, De | |
DE3803898A1 (de) | 1988-02-09 | 1989-08-10 | Degussa | Presslinge auf basis von pyrogen hergestelltem zirkondioxid, verfahren zu ihrer herstellung und ihre anwendung |
DE3803894A1 (de) | 1988-02-09 | 1989-08-10 | Degussa | Presslinge auf basis von pyrogen hergestelltem titandioxid, verfahren zu ihrer herstellung und ihre verwendung |
DE3803899C1 (zh) * | 1988-02-09 | 1989-04-13 | Degussa Ag, 6000 Frankfurt, De | |
GB8906726D0 (en) * | 1989-03-23 | 1989-05-10 | Shell Int Research | Titania extrudates |
DE3912504A1 (de) | 1989-04-17 | 1990-10-18 | Degussa | Presslinge auf basis von pyrogen hergestelltem siliciumdioxid, verfahren zu ihrer herstellung und ihre verwendung |
US5231067A (en) | 1989-04-27 | 1993-07-27 | Degussa Ag | Shaped articles based on pyrogenically produced titanium dioxide, method of their production and their use |
DE3913938A1 (de) * | 1989-04-27 | 1990-10-31 | Degussa | Presslinge auf basis von pyrogen hergestelltem titandioxid, verfahren zu ihrer herstellung sowie ihre verwendung |
DE3919524A1 (de) * | 1989-06-15 | 1990-12-20 | Hoechst Ag | Verfahren zur herstellung von vinylacetat |
DE4012479A1 (de) * | 1990-04-19 | 1991-10-24 | Degussa | Titandioxidpresslinge, verfahren zu ihrer herstellung sowie ihre verwendung |
DE4120492A1 (de) * | 1991-06-21 | 1992-12-24 | Hoechst Ag | Verfahren zur herstellung von vinylacetat |
GB9214688D0 (en) | 1992-07-10 | 1992-08-19 | Bp Chem Int Ltd | Olfin hydration catalysts |
DE4427574C2 (de) * | 1994-08-04 | 1997-08-14 | Degussa | Preßlinge auf Basis von pyrogen hergestelltem Siliciumdioxid |
GB9419387D0 (en) * | 1994-09-26 | 1994-11-09 | Bp Chem Int Ltd | Olefin hydration process |
DE19501891C1 (de) | 1995-01-23 | 1996-09-26 | Degussa | Verfahren zur Herstellung eines Trägerkatalysators und seine Verwendung für die Produktion von Vinylacetat |
ES2154748T3 (es) * | 1995-02-04 | 2001-04-16 | Degussa | Granulados a base de dioxido de silicio preparado por via pirogena, procedimiento para su preparacion y su empleo. |
DE19607494A1 (de) * | 1996-02-28 | 1997-09-04 | Degussa | Verwendung von Katalysatoren auf Basis von Siliziumdioxid enthaltenden Katalysatorträgern für katalytische Umsetzungen unter hydrothermalen Bedingungen |
DE19612783A1 (de) * | 1996-03-29 | 1997-10-02 | Degussa | Phosphorsäurekatalysator und seine Verwendung |
DE19619961A1 (de) | 1996-05-17 | 1997-11-20 | Degussa | Preßlinge auf Basis von pyrogen hergestelltem Siliciumdioxid |
-
1998
- 1998-09-24 DE DE19843845A patent/DE19843845A1/de not_active Withdrawn
-
1999
- 1999-08-26 EP EP99116664A patent/EP0997193A1/de not_active Withdrawn
- 1999-09-17 ID IDP990868D patent/ID26671A/id unknown
- 1999-09-22 KR KR1019990040949A patent/KR20000023397A/ko not_active Application Discontinuation
- 1999-09-22 JP JP11269052A patent/JP2000095571A/ja active Pending
- 1999-09-22 US US09/401,498 patent/US6432869B1/en not_active Expired - Fee Related
- 1999-09-23 NO NO994625A patent/NO994625L/no not_active Application Discontinuation
- 1999-09-23 CA CA002283040A patent/CA2283040A1/en not_active Abandoned
- 1999-09-24 CN CN99120378A patent/CN1250761A/zh active Pending
- 1999-09-24 SG SG9904825A patent/SG92657A1/en unknown
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1780827B (zh) * | 2003-05-02 | 2010-06-16 | 帝斯曼知识产权资产管理有限公司 | 母育酚酰化物和生育酚酰化物的制备方法 |
CN101899032B (zh) * | 2003-05-02 | 2012-05-30 | 帝斯曼知识产权资产管理有限公司 | 母育酚酰化物和生育酚酰化物的制备方法 |
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EP0997193A1 (de) | 2000-05-03 |
JP2000095571A (ja) | 2000-04-04 |
NO994625D0 (no) | 1999-09-23 |
DE19843845A1 (de) | 2000-03-30 |
NO994625L (no) | 2000-03-27 |
US6432869B1 (en) | 2002-08-13 |
SG92657A1 (en) | 2002-11-19 |
CA2283040A1 (en) | 2000-03-24 |
KR20000023397A (ko) | 2000-04-25 |
ID26671A (id) | 2001-01-25 |
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