CN102612407A - 放热工艺催化剂的载体及其制备的催化剂 - Google Patents
放热工艺催化剂的载体及其制备的催化剂 Download PDFInfo
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- CN102612407A CN102612407A CN2010800351313A CN201080035131A CN102612407A CN 102612407 A CN102612407 A CN 102612407A CN 2010800351313 A CN2010800351313 A CN 2010800351313A CN 201080035131 A CN201080035131 A CN 201080035131A CN 102612407 A CN102612407 A CN 102612407A
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- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- 230000002269 spontaneous effect Effects 0.000 description 1
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Abstract
本发明涉及石油化学、气体化学，并披露了一种用于放热工艺催化剂的载体，特别是费希尔-托罗普希工艺、甲醇合成、氢化、废气净化。所述用于催化剂的载体包括分散的片状和球形铝粉末混合物形式的金属铝并且载体为小球，优选为圆柱体、片状体、丸形体，通过挤压，制粒，压片，加工成圆或液态成型而获得。制备在载体上的催化剂包括选自Co、Fe、Ni、Ru、Rh、Pt、Pd、Cu和/或其混合物的组的活性金属。
Description
技术领域
本发明涉及石油化学、气体化学，并披露了一种用于放热工艺催化剂的载体，特别是费希尔-托罗普希工艺、甲醇合成、氢化、废气净化，并且本发明还披露了一种载于其上的催化剂。
背景技术
众所周知的，在流化床反应器、浆态反应器和固定床反应器中进行多相放热工艺技术上是可行。固定床反应器是催化技术领域中最常遇到的系统。这种反应器是一种多相的系统，至少有两相组成：催化剂的固体粒子及之间的气体和/或液体形式的反应混合物流动的空隙。同时，在反应器中的催化剂表面发生化学转换和随后的物理工艺：反应组分和产物在床中转移，热交换和气体流动等。
在管式反应器中，反应混合物和冷却介质间的热交换通过反应器壁实现。催化剂装进小直径(2-8cm)管中；冷却介质(比如高压蒸汽)在管间的空间内循环。管式反应器的重要优点在于对催化剂散热的有利条件，因为冷却表面相对于催化剂量的比例远远超过在其他设备中的。
催化剂床中的最佳温度范围的形成是催化管式反应器发展中主要面对的问题之一。在每个催化剂颗粒中的传热和传质的提升推进了该问题。通过使用一个置催化剂于高导热材料的载体来提升传热是可能的，并且通过使用一个具有各向同性性能的载体能够改善传质。
US 20040024274涉及一种单环或多环芳族烃氢化的催化剂，包括至少一种周期表VIII过渡金属族的金属和结构性载体或整料载体。这种结构性载体具有规则的两维或三维结构并因此有别于固定床反应器中通常所用的粒子状催化剂。这种结构性载体或整料可包括金属、无机、有机或合成材料或这些材料的组合。金属材料的例子是纯金属，比如铁、铜、镍、银、铝和钛或者合金，比如钢，例如镍钢，铬钢和钼钢，黄铜，磷青铜，镍合金和镍银。比如，催化剂本体可由包括不锈钢的金属的结构性载体或整料制成，当在空气中在1-20小时内加热到400-1100℃并随后冷却至室温，所述不锈钢较好的显示表面的糙化。此外，该表面变得富含合金组分(比如铝或铬，由它们形成相应的Al2O3或Cr2O3表面层)。除了热糙化以外，糙化也可通过机械方式形成来代替热糙化。优选使用结构性载体的形式包括织造的金属网或织物、编织的金属网或织物或金属毡、织造的碳纤维或碳纤维毡或织物或编织的聚合物织物或网。
无机材料的例子是陶瓷材料，比如氧化铝，二氧化硅，二氧化锆，堇青石和滑石。也可以使用碳。合成载体材料例子是，例如聚合物或玻璃纤维。
催化剂可进一步含有助催化剂，比如碱金属和/或碱土金属(如锂、钠、钾、铷、铯、镁、钙、锶和钡)；硅、碳、钛、锆、钨和镧系元素和锕系元素；货币金属，如铜、银和/或金、锌、锡、铋、锑、钼、钨和/或其他助催化剂比如硫和/或硒。
在应用活性组分之前，结构性载体或整料可通过溅射涂布一种、两种或多种氧化物。活性金属可通过浸染含有活性组分的水或有机溶液或悬浮液应用于载体。
进行氢化最好是在50-200℃和小于50帕的压强下。因此像正链烷烃这样的不良的副产物的形成是几乎不存在的，以至于净化变得不必要，这使得过程非常经济。当工艺持续的进行，被氢化的合成物的数量最好是每小时约0.05到约3公斤/升的催化剂。此外，转换苯和环己烷的收率为99.99％。时空产率为0.928kg/(l·h)。
此催化剂和载体的缺点如下：载体的性质不允许获得反应体积中的高浓度的活性组分的催化剂；减少工艺产率并导致反应器尺寸的增加。
EP 1994982涉及一种净化废气的催化剂，包括其上具有微孔的阳极氧化层(通过阳极氧化处理构架式金属形成)，和微孔中的催化活性金属。在阳极氧化处理中，构架式金属表面变得由氧化膜覆盖；该金属包括铝、钽、铌、钛、铪、锆、锌、钨、铋、锑，优选铝，包括纯铝和合金。至少有一个选自由K、Ba、La、Ca、L、Ce、Zr、Pr、Nd、Te、Sm和Gd组成的组的元素的氧化物(能够吸附NOx)，含量至少为0.01g/m2/μm，以及至少一个选自Pd、Pt、Rh、Ru、Ir、Ag和Ga组成的组的元素，含量至少为0.15g/m2/μm，作为催化活性金属。催化剂进一步包括具有吸附氨能力的多孔材料，该材料应用于阳极氧化层上。如下制备阳极氧化层：首先载体进行处理以表面糙化，然后进行阳极氧化处理。多孔材料应用于阳极氧化铝层上，为包含复合有至少一种磷酸和/或硅胶和/或勃姆石溶胶的一种沸石的混合物。多孔材料的含量由阳极氧化层的厚度和孔隙度的需要决定。催化剂体表面具有50-10000孔/μm2的微孔密度，并且微孔优选占据20-80％的表面区域。
此催化剂包括少量的贵金属，并且甚至在相对低的温度(150-250℃)，可有效净化柴油机废气中氮氧化物(NOX)。
此催化剂和载体的缺点在于获得方法的巨大困难。方法包括如下阶段：
1)构架式金属的热处理；
2)糙化表面形成；
3)阳极氧化处理；
4)阳极氧化层的酸或碱处理；
5)水合处理；
6)能够吸附NOX的氧化物的应用；
7)活性金属的应用；
8)能够吸附氨的多孔材料的应用。
此多阶段方法使得该催化剂在工业规模上生产很难。
EP2033709提供了一种含载体和催化组分的催化剂。该载体为含铝表面的金属基体；该金属基体被处理成在其表面上形成粗糙层。金属基体为金属纤维、金属薄片、金属网或金属板。基体的粗糙表面包含铝，铝表面呈鳞形(片状)。金属基体通过浸入含亲水性的醇或碳氢化合物的溶液中从而受到超声或微波处理，然后该基体在300-500℃下焙烧0.5-1.0小时。超声或微波处理的期间优选设定在一个范围，使铁或铬的析出量小于铝的析出量。贵金属，如铂、钯和铑用于催化组分；氧化物被用作载体。载体包括铈、铈、锆、碱金属、碱土金属及氧化物，例如，氧化铝。这种催化剂可用于废气净化工艺。CO的转化率为83-99％，并且其取决于催化剂层的厚度。
所有提及的催化剂具有结构性或整料载体，应用的催化剂材料的制备是非常困难的。这一事实限制了该类催化剂的实际应用。
以含铝粉末(由片状或鳞形的颗粒组成)或含片状铝的小球作为载体组分的催化剂不具有该缺点。此外，金属铝具有高导热性，并可提高反应区域的传热。这一事实增加催化剂性能的稳定性。
RU2326732提供了一种用于费希尔-托罗普希法合成的催化剂，包括一种门捷列夫元素周期表第VIII族的金属作为活性组分，一种载体包含氧化物组分和片状金属铝。活性组分含量为整个催化剂重量的5-40％。氧化物组分包含铝氧化物和/或硅氧化物和/或钛氧化物和/或锆氧化物。片状铝的含量为整个催化剂重量的1-25％。门捷列夫元素周期表第VII-VIII族的金属和/或氧化物被用作助催化剂。
载体通过糊状物的挤出，随后的热处理和所需大小的碎片的分解而获得。糊状物包括氧化物组分、片状金属铝、乙醚、水和粘结剂。整个催化剂重量的5-15％重量比的勃姆石可作为粘结剂使用。活性组分和助催化剂通过浸染、随后干燥、在空气流动中煅烧被引入。
在进行合成前，通过在氢气流(GHSV 100-5000l/h)、300-600℃的温度范围中还原0.5-5小时来活化催化剂。由CO∶H2合成的碳氢化合物的合成在具有催化剂的固定床的管式反应器中进行，置于0.1-4Mpa压力范围，和150-300℃温度范围下。合成气中CO∶H2的摩尔比范围在1∶1-1∶3。合成气可以包含多达25％的氮气。
该催化剂可以达到48-83％的CO转化率，6-12％的甲烷选择性，75-90％的C5+选择性和85-112kgC5+/m3/h的产率。
该催化剂和载体的缺点是巨大的小球径向方向的传质阻碍；事实的原因是，在取得载体时，含片状铝的糊状物在挤出时很容易整齐排列。因此该载体具有显著的强烈的各向异性的性质，即，在挤出体的移动方向的垂直和平行方向具有不同的性质。
同样片状铝的使用具有增加的风险，因为片状物的自燃会因此使得难以获得载体和催化剂。此外，当在催化剂床中的合成气GHSV大于3000l/h，为了提供活性中心所需的散热，铝含量是不足的。这是由于活性组分的主要部分置于铝的表面；事实上降低了使用活性组分的效率。
RU2256501涉及一种CO和H2合成烃的钴基的催化剂和载体。该催化剂包括金属铝粉末作为载体。该催化剂可以包括助催化剂，助催化剂选自金属氧化物的组，比如，ZrO2、La2O3或者K2O；或者金属的组，比如Re、Ru、Pd或者Pt。
如下制备该催化剂：铝粉末(根据GOST(国家标准，俄联邦)5494-95鳞状或片状颗粒组成的粉末)浸润在硝酸钴水溶液。然后浸润的粉末水浴干燥并在450℃的空气流中煅烧1小时。在氢气流(GHSV 100-3000l/h)还原活化该催化剂，温度范围为400-600℃，时间期间1-5小时。66-68mol.％H2和32-34mol.％CO的混合物合成碳氢化合物在大气压下进行，并且温度范围160-230℃，合成气GHSV为100l/h。
尽管与普通小球相比，改进了扩散传质，由于在催化剂床中的低的合成气GHSV并且无法提高，因此该催化剂的缺点在于合成的低活性和产率。
同样不可能的是在工业固定床反应器上使用该催化剂，因为载体和载体上的催化剂为粉末(粉碎的)形式。这一事实大大增加反应器中的压降到一个不被工艺性能允许的值。
因此在已知载体和催化剂中的使用片状粉末形式或颗粒粉末形态的金属铝未被披露。
但是片状铝的使用导致径向的传质问题，此由强烈的显著的各向异性性能决定。
应当注意的是片状铝粉末的使用的特点是增加风险，因为巨大的空隙，这一事实导致难以制备载体。
根据GOST 5494-95，片状铝粉末或包含片状(鳞形)颗粒的“铝粉”。它们的制成通过研磨根据GOST 11069至少A5等级或铝废料(废料的化学成分同A5等级的铝相同)的原铝。特别的，最大的生产商RUSAL制造如下5种等级的粉末：PAP-1、PAP-2、PAG-1、PAG-2、PAG-3。鳞形铝粉末用于制作“银色”颜料和国防工业。
同样球状颗粒中的“球形”铝粉末在烟火制造技术、有色冶金、化工、焊接工程中也是众所周知的。该粉末通过在惰性气体中粉碎熔融铝制成，惰性气体加热至融解温度，同时往雾化区提供冷的惰性气体(见RU2081733)。
特别的，根据48-5-226-87标准，最大的生产商RUSAL制造ASD等级的“球形”铝粉末。这些粉末具有较低的特有的粗糙表面，并因此它们的使用具有较低危险。
发明内容
根据本发明，提供了一种用于放热工艺催化剂的载体。该载体包括混合物形式的金属铝，该混合物为分散的片状和球形铝粉末及粘结剂，重量％百分比如下：
金属铝-25-95，
粘结剂—余量。
在本发明的一个较佳实施例中，相对于片状和球形铝粉末混合物的总重量，球形铝粉末的重量比为20-50％。
在本发明的一个较佳实施例中，粘结剂包含勃姆石、氧化硅或石墨。
在本发明的一个较佳实施例中，粘结剂包括助催化剂，该助催化剂选自Mg、Ca、Zn、Ba、Al、Si、Zr、Ti、Cr、Ce和/或它们的混合物的氧化物或混合的氧化物的组，并且该助催化剂的含量按重量不超过粘结剂重量的50％。
在本发明的一个较佳实施例中，所述载体为小球、圆柱体、片状体、丸形体，通过挤出，制粒，压片，加工成圆或液态成型而获得。
一种用于放热工艺的催化剂被提供。所述催化剂包括活性金属和载体，所述活性金属选自Co、Fe、Ni、Ru、Rh、Pt、Pd、Cu和/或其混合物的组，所述载体包含混合物形式的金属铝，该混合物为分散的片状和球形铝粉末和粘结剂，其中活性金属含量为所述催化剂总重量的0.1-40％。
在本发明的一个较佳实施例中，所述催化剂进一步包括活性金属助催化剂，所述活性金属选自门捷列夫元素周期表的II-V和/或VI-VIII族的元素，含量为所述催化剂总重量的0.1-5％。
本发明的催化剂适合放热工艺，特别是费希尔-托罗普希工艺、甲醇合成、氢化、废气净化。
具体实施方式
发明人的大量研究令人惊讶的表明，如果片状和球形铝的分散粉末的混合物形式的金属铝用于放热工艺催化剂的载体，那么在催化剂中会形成不具有各向异性的地区。这一事实的理由明显的是载体结构的排列，以及它提供了一个使用金属铝优点的选择，而没有短缺，即有着高导热性。这些因素提升了反应区域的散热；载体取得了改善的各向同性的性能，此增加了催化剂内部的传热和传质。由于投入试剂的负载的提升，提供了更多了剧烈的化学反应并改善了工艺产率。
同样使用小球催化剂是可能的。小球形催化剂和载体的优点众所周知，包括小球形催化剂能够在反应器中形成具有低液压阻力的固定床。这类床允许有效的供应原料到催化剂的活性中心，并有效的带走产物。具有小球形催化剂的反应器简单、可靠并便宜；不需要特殊的混合设备和其它对分散颗粒或粉末形式的催化剂的反应器来说必不可少的难题。
因此由于已取得的各向同性，本发明的载体和催化剂增加了小球的催化表面的使用，并提供了更剧烈的化学反应。分散的片状和球形铝的粉末结合使用提供了导致小球内部传质提升的载体和催化剂的各向同性。同样片状铝含量的减少和其与球形铝粉末的结合显著降低了处理风险，并简化了载体的制备。
根据本发明，提供了一种放热工艺催化剂的载体。所述载体包括分散的片状和球形铝的粉末的混合物的金属铝及粘结剂，重量百分比如下：
金属铝-25-95
粘结剂-余量。
重量少于所述载体总重量25％的金属铝的含量不能提供具有所披露性能的催化剂；因为其制备的催化剂的低活性，大于95％的含量是不合适的。
分散的铝粉末为颗粒尺寸不超过100μm的颗粒粉末。
在本发明的一个较佳实施例中，按重量相对于片状和球形铝粉末的混合物的总重量，球形铝粉末的重量比为20-50％。
载体中球形铝重量比的减少小于20％不能提供所需的载体的各向同性性能，增加超过50％导致载体及其制备的催化剂的机械强度降低。
在本发明的一个较佳实施例中，粘结剂包括勃姆石或氧化硅或石墨。
在本发明的一个较佳实施例中，粘结剂包括助催化剂，选自Mg、Ca、Zn、Ba、Al、Si、Zr、Ti、Cr、Ce和/或它们的混合物的氧化物或混合的氧化物的组，并且该助催化剂的含量按重量不超过粘结剂重量的50％。
助催化剂的含量高于50％是不合理的，因为其不能改善催化剂的性能。
重要的是，载体可以制备成小球并且载体为圆柱体、片状体、丸形体，通过挤压，制粒，压片，加工成圆或液态成型而获得。
一种用于放热反应的催化剂被提供。所述催化剂包括活性金属和载体，所述活性金属选自Co、Fe、Ni、Ru、Rh、Pt、Pd、Cu和/或其混合物的组，所述载体包含混合物形式的金属铝，混合物为分散的片状和球状铝的粉末及粘结剂，其中活性金属含量为所述催化剂总重量的0.1-40％。活性金属通过浸染方法随着金属盐的水或有机溶液被注入。活性金属的含量小于0.1％无法获得具有所披露的性能的催化剂，并且含量多于40％是不适宜的，因为相对于活性的提升，催化剂的消耗量变得非常高。
在本发明的一个较佳实施例中，所述催化剂进一步包括活性金属助催化剂，所述活性金属选自门捷列夫元素周期表的II-V和/或VI-VIII族的元素，含量为所述催化剂总重量的0.1-5％。
本发明的载体的制备如下：
粘结剂(比如勃姆石)，分散的球形铝粉末和分散的片状铝粉末加入到硝酸HNO3(64％)、蒸馏水和三甘醇(TEG)的混合物中；随后搅拌直到形成均匀混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备催化剂是通过载体浸染在六水硝酸钴Co(NO3)2·6H2O的水溶液以产生20-wt％的钴。然后小球在水浴中干燥并在400℃下空气流中焙烧3小时，空气流中冷却至室温。催化剂装载进固定床反应器并在400℃下氢气流中活化1小时。
在费希尔-托罗普希工艺中，在235℃、2MPa、合成气每小时流速(GHSV)为4000l/h、H2/CO体积比为2条件下下测试该催化剂。
在进行合成之前，该催化剂的样品通过在大气压下、温度范围250-450℃(优选350-450℃)的氢气流(GHSV 1000-10000l/h)中还原0.5-10小时被活化。
为了进一步说明本发明的各种实施例，下面提供了非限制的例子：
例1
制备载体样品(75％Al+25％粘结剂)如下：
2.5g勃姆石，1.5g ASD-1等级的球形铝粉末和6g PAP-2等级的片状铝粉末加入到0.45ml HNO3(64％)、10ml蒸馏水和0.6ml亚甲基乙二醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后将挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
通过在六水硝酸钴Co(NO3)2·6H2O的水溶液中浸润载体(75％Al+25％粘结剂)而得到20-wt％Co来制备20％Co/载体的催化剂；小球在水浴中干燥并在400℃空气流中焙烧3小时，然后空气流中冷却至室温。催化剂装载进固定床反应器并在400℃氢气流中活化1小时。
通过在235℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化70％、C5+选择率60％和产率349kg/m3/h。
例2
制备载体样品(25％Al+75％粘结剂)如下：
含3.75g勃姆石和3.75gMgO的7.5g粘结剂、1.25g ASD-1等级的球形铝粉末和1.25g PAP-2等级的片状铝粉末加入到0.675ml HNO3(64％)、12ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后将挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备含30％Co-2.5％Al/载体的催化剂如下：
通过在硝酸铝的水溶液中浸润已得的载体(25％Al+75％粘结剂)以得到2.5-wt％Al，在水浴中干燥并在400℃空气流中焙烧3小时。所得材料在六水硝酸钴Co(NO3)2·6H2O的水溶液中浸润以得到30-wt％Co，小球在水浴中干燥并在400℃空气流中焙烧1小时，然后空气流中冷却至室温。将催化剂装载进固定床反应器并在400℃氢气流中活化1小时。
通过在235℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化64％、C5+选择率62％和产率330kg/m3/h。
例3
制备载体样品(50％Al+50％粘结剂)如下：
含2.5g勃姆石和2.5g具有模块20的沸石粉HY的5g粘结剂、1.5g ASD-6等级的球形铝粉末和3.5g PAP-2等级的片状铝粉末加入到0.45mlHNO3(64％)、10ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120摄氏度空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后将挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备含20％Co/载体的催化剂如下：
通过在六水硝酸钴Co(NO3)2·6H2O的水溶液中浸润已得载体(50％Al+50％粘结剂)以得到20-wt％Co；小球在水浴中干燥并在250℃空气流中焙烧1小时，然后空气流中冷却至室温。催化剂装载进固定床反应器并在400℃下氢气流中活化1小时。
通过在235℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化70％、C5+选择率68％和产率396kg/m3/h。
例4
制备载体样品(50％Al+50％粘结剂)如下：
含3g勃姆石和2g硅胶的5g粘结剂、1.5g ASD-6等级的球形铝粉末和3.5gPAP-1等级的片状铝粉末加入到0.54mlHNO3(64％)、10ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备含10％Co-5％Zr/载体的催化剂如下：
通过在硝酸锆的水溶液中浸润已得的载体(50％Al+50％粘结剂)以得到5-wt％Zr，在水浴中干燥并在400℃空气流中焙烧3小时。所得材料在六水硝酸钴Co(NO3)2·6H2O的水溶液中浸润以得到10-wt％Co，小球在水浴中干燥并在250℃空气流中焙烧1小时，然后空气流中冷却至室温。将催化剂装载进固定床反应器并在400℃氢气流中活化1小时。
通过在235℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化65％、C5+选择率61％和产率330kg/m3/h。
例5
制备载体样品(50％Al+50％粘结剂)如下：
含4g勃姆石和1g TiO2的5g粘结剂、1.5g PAG-1等级的球形铝粉末和3.5gPAP-1等级的片状铝粉末加入到0.72mlHNO3(64％)、11ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。将挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备含20％Fe-2％Mg/载体的催化剂如下：
通过在硝酸镁的水溶液中浸润已得的载体(50％Al+50％粘结剂)以得到2-wt％Mg，在水浴中干燥并在400℃空气流中焙烧1小时。所得材料在Fe(NO3)3-9H2O的水溶液中浸润以得到20-wt％Fe，小球在水浴中干燥并在250℃空气流中焙烧1小时，然后在空气流中冷却至室温。催化剂装载进固定床反应器并在350℃下氢气流中活化1小时。
通过在240℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化63％、C5+选择率60％和产率314kg/m3/h。
例6
制备载体样品(50％Al+50％粘结剂)如下：
含2g勃姆石和2g Al2O3及1g CaO的5g粘结剂、2g ASP-0-63等级的球形铝粉末和3g PAP-2等级的片状铝粉末加入到0.45ml HNO3(64％)、10ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备含15％Ru-1％Cr/载体的催化剂如下：
通过在硝酸铬的水溶液中浸润已得的载体(50％Al+50％粘结剂)以得到1-wt％Cr，在水浴中干燥并在400℃空气流中焙烧1小时。所得材料在RuCl3乙醇溶液中浸润以得到15-wt％Ru，小球在水浴中干燥并在400℃空气流中焙烧1小时，然后空气流中冷却至室温。催化剂装载进固定床反应器并在400℃氢气流中活化1小时。
通过在245℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化66％、C5+选择率59％和产率324kg/m3/h。
例7
制备载体样品(40％Al+60％粘结剂)如下：
含3g勃姆石和2g SiO2及1g ZrO2的6g粘结剂、1g ASP-0-63等级的球形铝粉末和3g PAP-2等级的片状铝粉末加入到0.54ml HNO3(64％)、10ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备含20％Co-0.1％Re/载体的催化剂如下：
通过在铼氨的水溶液中浸润已得的载体(40％Al+60％粘结剂)以得到0.1-wt％Re，在水浴中干燥并在400℃空气流中焙烧1小时。所得材料在六水硝酸钴Co(NO3)2·6H2O的水溶液中浸润以得到20-wt％Co，小球在水浴中干燥并在400℃空气流中焙烧1小时，然后空气流中冷却至室温。催化剂装载进固定床反应器并在400℃氢气流中活化1小时。
通过在235℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化66％、C5+选择率72％和产率389kg/m3/h。
例8
制备载体样品(60％Al+40％粘结剂)如下：
含2g硅胶和2g具有模块20的沸石粉HMor的4g粘结剂、1.2g PAG-1等级的球形铝粉末和4.8g PAP-2等级的片状铝粉末加入到1.5ml NH4OH(30％)、9.5ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径2.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中450℃空气中焙烧5小时。然后挤出后的物体冷却至室温并切成2.5×2.5mm的小球。
制备含20％Co-3％Fe/载体的催化剂如下：
通过在硝酸亚铁(III)的水溶液中浸润已得的载体(60％Al+40％粘结剂)以得到3-wt％Fe，在水浴中干燥并在400℃空气流中焙烧1小时。所得材料在六水硝酸钴Co(NO3)2·6H2O的水溶液中浸润以得到20-wt％Co，小球在水浴中干燥并在250℃空气流中焙烧1小时，然后空气流中冷却至室温。催化剂装载进固定床反应器并在400℃氢气流中活化1小时。
通过在235℃、2MPa、合成气的气体小时流速(GHSV)为4000l/h和H2/CO体积比为2的费希尔-托罗普希工艺中测试该催化剂，表明：CO转化67％、C5+选择率71％和产率396kg/m3/h。
例9
制备载体样本(80％Al+20％粘结剂)如下：
含1g勃姆石和1g Cr2O3粉的2g粘结剂、1.6g ASP-0-63等级的球形铝粉末和6.4g PAP-2等级的片状铝粉末加入到0.2ml HNO3(64％)、9ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物通过直径1.5mm的冲模挤出。挤出后的物体在120℃空气中干燥6小时，在干燥箱中400℃空气中焙烧5小时。然后挤出后的物体冷却至室温并切成1.5×3-5mm的小球。
制备含5％Ni/载体的催化剂如下：
通过在硝酸镍的水溶液中浸润已得的载体(80％Al+20％粘结剂)以得到5-wt％Ni，小球在水浴中干燥并在400℃空气流中焙烧1小时，然后空气流中冷却至室温。催化剂装载进固定床反应器并在400℃下氢气流中活化1小时。
通过在1100℃、1MPa、苯流率为900kg/dm3/h的苯氢化中测试该催化剂，表明：苯转化98％、环己烷选择率90％和产率940kg/m3/h。
例10
制备载体样品(40％Al+60％粘结剂)如下：
含3g勃姆石和2.5g ZnO及0.5g BaO的6g粘结剂、1g ASP-0-63等级的球形铝粉末和3g PAP-2等级的片状铝粉末加入到0.5ml HNO3(64％)、15ml蒸馏水和0.6ml三甘醇(TEG)，并随后搅拌直至形成均匀的混合物。然后混合物液态成型得到直径3mm的球形小球。小球在120℃空气中干燥3小时，在干燥箱中400℃空气中焙烧5小时并冷却至室温。
制备含40％Cu/载体的催化剂如下：
通过在硝酸铜的水溶液中浸润已得的载体(40％Al+60％粘结剂)以得到40-wt％Cu，在水浴中干燥并在400℃空气流中焙烧1小时，然后空气流中冷却至室温。将催化剂装载进固定床反应器并在220℃氢气流中活化6小时。
通过在180℃、5MPa、合成气GHSV为10000l/h和H2/CO体积比为2的CO和H2合成甲醇中测试该催化剂，表明：CO转化77％、甲醇选择率81％和产率2.96kg/m3/h。
例11
制备载体样品(80％Al+20％粘结剂)如下：
搅拌含1g石墨和1g CeO2粉的2g粘结剂、2g PAG-1等级的球形铝粉末和6g PAP-2等级的片状铝粉末以获得均匀的混合物。通过按压成片形成2mm大小的小球，混合物制成直径和高度为5mm的圆柱体。小球在干燥箱中400℃惰性气体中焙烧5小时。然后小球冷却至室温。
制备含0.1％Pt/载体的催化剂如下：
通过在氯铂酸的水溶液中浸润已得的载体(80％Al+20％粘结剂)以得到0.1-wt％Pt，小球在水浴中干燥并在400℃氮气流中焙烧1小时，然后空气流中冷却至室温。将催化剂装载进固定床反应器并在250℃氢气流中活化3小时。
通过在180℃、0.1MPa、GHSV为10000l/h的类似柴油发动机的废气成分的气体混合物的净化中测试该催化剂，表明：CO净化效率99％、NOx为98％。
例12
制备载体样品(95％Al+5％粘结剂)如下：
搅拌含石墨的0.5g粘结剂、1.9g ASD-1等级的球形铝粉末和8.1g PAP-1等级的片状铝粉末以获得均匀的混合物。通过按压成片形成2mm大小的小球，混合物制成直径和高度为3mm的圆柱体。小球在干燥箱中400℃惰性气体中焙烧5小时。然后冷却小球至室温。
制备含0.2％Pd/载体的催化剂如下：
通过在氯化钯的水溶液中浸润已得的载体(95％Al+5％粘结剂)以得到0.2-wt％Pd，小球在水浴中干燥并在400℃氮气流中焙烧1小时，然后空气流中冷却至室温。催化剂装载进固定床反应器并在250℃氢气流中活化3小时。
通过在180℃、0.1MPa、GHSV为10000l/h的类似柴油发动机的废气成分的气体混合物的净化中测试该催化剂，表明：CO和NOx的净化效率为99％。
这些例子表明所请求保护的用于放热工艺的载体和催化剂具有各向同性的性能，提升催化剂小球内部的传质。由于投入试剂的GHSV的增加，提供了更剧烈的化学反应并提高了工艺产率。
所请求保护的载体及其制备的催化剂在放热工艺中的使用，特别是费希尔-托罗普希工艺、合成甲醇、氢化、废气净化，将导致原料负载量增加时固定床反应器中催化剂的高活性和产率。
Claims (7)
1.一种用于放热工艺催化剂的载体包括金属铝和粘结剂，其特征在于，金属铝为分散的片状和球形铝粉末混合物的形式，铝和粘结剂的比例如下，重量百分比：
金属铝-25-95，
粘结剂-余量。
2.如权利要求1所述的载体，其特征在于，相对于片状和球形铝粉末混合物的总重量，球形铝粉末的重量比为20-50％。
3.如权利要求1所述的载体，其特征在于，勃姆石、氧化硅或石墨被用作粘结剂。
4.如权利要求3所述的载体，其特征在于，粘结剂包括助催化剂，所述助催化剂从由Mg、Ca、Zn、Ba、Al、Si、Zr、Ti、Cr、Ce和/或它们的混合物的氧化物或混合的氧化物的组成的组中选出，并且所述助催化剂的含量按重量不超过粘结剂重量的50％。
5.如权利要求1所述的载体，其特征在于，所述载体为小球，优选为圆柱体、片状体、丸形体，通过挤出、造粒、压片、加工成圆或液态成型而获得。
6.一种用于放热工艺的催化剂，包括活性金属和如权利要求1所述的载体，所述活性金属选从由Co、Fe、Ni、Ru、Rh、Pt、Pd、Cu和/或其混合物的组成的组中选出，其特征在于，活性金属含量为所述催化剂总重量的0.1-40％。
7.如权利要求6所述的催化剂，进一步包括活性金属的助催化剂，所述活性金属选自门捷列夫元素周期表的II-V和/或VI-VIII族的元素，含量为所述催化剂总重量的0.1-5％。
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| CN104994953A (zh) * | 2013-11-19 | 2015-10-21 | 气体化学技术有限责任公司 | 制备用于烃部分氧化成合成气的以耐热合金为基底的多金属氧化物催化剂的方法 |
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| KR101405517B1 (ko) | 2013-05-22 | 2014-06-11 | 한국과학기술연구원 | 혼합 개질 반응에 이용되는 니켈계 촉매의 제조방법 |
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| US9446396B2 (en) | 2016-09-20 |
| RU2414300C1 (ru) | 2011-03-20 |
| US20120122674A1 (en) | 2012-05-17 |
| AU2010279755B2 (en) | 2016-07-07 |
| JP2013500859A (ja) | 2013-01-10 |
| WO2011016759A1 (en) | 2011-02-10 |
| CN102612407B (zh) | 2015-11-25 |
| JP5584891B2 (ja) | 2014-09-10 |
| CA2770020C (en) | 2014-09-09 |
| CA2770020A1 (en) | 2011-02-10 |
| EP2461906A1 (en) | 2012-06-13 |
| RU2009129645A (ru) | 2011-02-10 |
| ZA201200712B (en) | 2012-10-31 |
| AU2010279755A1 (en) | 2012-02-16 |
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