CN101402056B - 催化剂设计和蒸汽转化催化剂制备方法 - Google Patents

催化剂设计和蒸汽转化催化剂制备方法 Download PDF

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CN101402056B
CN101402056B CN2008101669296A CN200810166929A CN101402056B CN 101402056 B CN101402056 B CN 101402056B CN 2008101669296 A CN2008101669296 A CN 2008101669296A CN 200810166929 A CN200810166929 A CN 200810166929A CN 101402056 B CN101402056 B CN 101402056B
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沃尔夫冈·加布里尔
英戈·汉克
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Abstract

本发明涉及具有大面积结构的新型催化剂，尤其是蒸汽转化催化剂，其特征在于，所述大面积结构由许多具有圆形或者多边形截面的平行穿透孔构成，其中所述催化剂用注模方法制备，催化剂载体用修补基面涂层覆层，并且接着用活性成分浸渍所述催化剂载体包含至少一种可烧结材料，并且具有至少700N的侧耐压强度此外本发明还涉及一种制备这样的催化剂的方法和其在一种反应器中的应用

Description

催化剂设计和蒸汽转化催化剂制备方法
本发明涉及一种有大面积结构的新型催化剂设计。此外本发明还涉及所述新型催化剂的制备方法和其在蒸汽转化反应、ATR和在催化部分氧化反应(CPOX)中的应用。
蒸汽转化是从轻碳水化合物和水蒸汽中产生富氢的合成气体的广泛使用的方法。配料，例如天然气、液化气体、石油并且还有甲烷与水蒸汽在催化反应器中吸热地转化成高氢含量的合成气体。过程热和烟气热，例如用于产生蒸汽或者用于预热各种过程和水流。该过程多数在大技术设备中于约550-900℃的温度并且在约25至60巴的压力下进行，在ATR(自热转化)的情况下甚至达到约80巴。
这样的转化的反应通式为：
CnHm+n H2O＝＞n CO2+(n+m/2)H2
例如甲烷的蒸汽转化反应为：
(1)CH4+H2O→CO+3H2   ΔH＝+49.2kcal/mol
(2)CO+H2O→CO2+H2    ΔH＝-9.8kcal/mol
第一个反应是一种强吸热反应，这种强吸热反应一般地需要一个转化催化剂(例如一个镍催化剂)。
放热地催化转化所产生的一氧化碳和水蒸汽的第二个过程步骤也称为转移反应。
用常规的催化剂几何条件，例如在固定床反应器或者管式反应器中，存在的一个课题是压力损失的最小化。在有较大表面积的小催化剂的情况下往往由于催化剂装料而增加压力损失，因此降低了反应的利用率。在蒸汽转化的情况下附加地热加料是一个限制因素(吸热反应)。在此值得追求良好导热的催化剂载体。这例如可以通过使用导热陶瓷(例如SiC)或者在注模制备它之前向陶瓷坯料中添加金属(陶瓷/金属混合物)达到。
为了降低压力损失，以前用圆筒形的空心体(Rashig-Ringe)。然而为了在这种情况下还试图得到足够大的表面积，就要把该圆筒的壁做得薄，例如在US 4,089,941A，US 4,233,187A，GB 1,513,544和FR 2,375,138中的说明。然而这样做会导致这种催化剂机械稳定性下降。
为了得到足够的机械稳定性，例如EP 0 192 314A1描述了一种鞍形催化剂，所述催化剂用一种煅烧的铝酸钙陶瓷坯料制备。然而这样一种催化剂的反应表面积如同所述空心圆桶一样受限。
另一种公知的常规蒸汽转化用的催化剂是Süd-Chemie AG公司的G-90LDP，例如该公司在WO 2006/016983A2中所公开的那样。该催化剂用一个高耗费的多级方法制备。这样一种催化剂同样地存有在其上进行催化反应的外表面的大小有限的缺点。
从而值得追求一种催化剂，所述催化剂提供一个较大的化学反应表面积、具有较大的机械耐受性并且制备简单。
该任务通过一种有大面积结构的催化剂完成，所述催化剂的特征在于，所述大面积结构由许多有圆形或者多边形截面的平行穿透孔构成，其中所述催化剂包含至少一种可烧结材料并且有至少700N的侧耐压强度。优选的是该大面积结构具有一种蜂窝形状(honeycomb)。
该大表面积结构通过一种成型法，优选的是在一个注模模具中注入至少一种可烧结材料，其中所述注模方法允许任意的成型。本发明中“大面积”的概念指的是，所述结构每cm2绕流面积有10-300个穿透孔。
从而同样属于本发明的范畴的是制备一种大面积结构的催化剂的方法，该结构具有侧耐压强度至少700N，包含步骤：
a)把一种可烧结材料碾成粉末；
b)在所述可烧结材料中掺入一个弥散剂；
c)加热并且混合所得到的配料以得出一种塑性的坯料；
d)把所述塑料坯料注入一个注模模具中；和
e)冷却、出模并煅烧该坯料。
同样地可以向所述可烧结材料中添加一种导热的材料，例如一种金属，譬如镍等。
混合所述配料，也就是把所述可烧结材料与弥散剂混合，优选地在加热30至150℃的条件下进行。所述弥散剂起的作用是，能够把所述可烧结材料和其它的成分转变成一个塑性的坯料。优选的弥散剂是白油
Figure GSB00000353191400021
然而同样也可以采用其它的弥散剂，譬如聚烯烃-蜡混合物、多元醇、聚乙烯醇等。
加热和混合所述配料以得到所述塑性坏料，可以最简单地在一个挤压机中进行，由此可达到非常均匀的混合。作为可供选择的替代方案还可以使用其它的方法，例如在一个混合器、一个碾机或者一个搅拌机上进行。
浇注模具应当构成得使催化剂的所述大面积结构每cm2绕流面积具有10-300个自由穿透孔，优选每cm2绕流面积具有20-250个自由穿透孔，并且尤其优选的是所述结构每cm2绕流面积具有25-225个穿透孔。该具有大面积结构的催化剂产生优选地垂直的圆筒，其中圆筒的直径为5至25mm，尤其是10至20mm，尤其优选的是10至19mm，并且圆筒的高度为5至25mm，尤其是10至16mm。然而通过该注模方法可能有所有可想像的形状。穿透孔的截面可以构成圆的、三角的、四角的和/或六角的。尤其优选的是所述大面积结构是一种蜂窝状结构。
所述催化剂的至少一种可烧结材料是一种金属氧化物和/或一种陶瓷。优选的是至少一种可煅烧的材料，选自铝酸盐、硅酸盐、钛酸盐，选自二氧化钛、氧化铝、氧化镁、氧化锆、钛酸铝、压电陶瓷、工艺瓷、滑石、菫青石、富铝红柱石陶瓷、碳化物、碳化硅、碳化硼、氮化物、氮化硅、硝酸铝、氧氮硅铝、铝酸钙、铝酸钾或者铝酸镁或者其组合。
陶瓷是最优选的。氧化陶瓷含至少90％单相的或者单成分的金属氧化物。最重要的代表是氧化铝(Al2O3)、氧化镁(MgO)、氧化锆(ZrO2)、钛酸铝(Al2TiO5)和压电陶瓷。属于硅酸盐陶瓷例如是工艺瓷、滑石、堇青石和富红柱石陶瓷。主要组分作为硅酸盐载体的是陶土和高岭土，以及长石和滑石。属于非氧化物陶瓷的，例如是碳化物(不同制备方法的碳化硅。碳化硼)和氮化物(氮化钙、硝酸铝、氧氮化硅)。较高成分的共价化合物也赋于所述材料在高温条件下非常良好的机械特性。
可烧结材料可以占催化剂重量的＞0至100重量百分比，优选10至99重量百分比，更优选的是50至95重量百分比。
此外所述催化剂还可以含有一种粘合剂。适合的粘合剂是，例如高岭土、陶土或者釉料。粘合剂还可以是一种溶胶，例如Al2O3的纳米颗粒制备的溶胶(例如Sasol公司的
Figure GSB00000353191400031
)，ZrO2(例如Mel-Chemicals的Zr-乙酸盐，
Figure GSB00000353191400032
产品)。此外优选的是氧化铈-溶胶(例如NYACOL制备的)，二氧化硅-溶胶(例如
Figure GSB00000353191400033
)和二氧化钛-溶胶(例如Sachleben-Chemie制备的)。溶胶应当理解为均质清彻的溶液，所述纳米颗粒在约2-50-nm的范围。市售溶胶通常涉及乙酸稳定了的溶胶或者硝酸盐稳定了的溶胶(硝酸)。
附加地还可以向粘合剂添加一种烧尽材料，例如纤维素。这样做的优点是，在煅烧步骤以后烧尽材料燃烧掉，从而提高催化剂的微孔容积。然而这样做的前提是完全地燃烧掉所述燃尽材料，从而不留下可能阻塞微孔的任何残余物。因此还可以添加满足完全烧尽的要求的其它的化合物，尤其是有机化合物，作为燃尽材料，譬如石蜡、蜂蜡、热塑塑料等。添加粘合媒介和其它现有技术公知的添加剂、辅料、填料、催化剂等等可能也是有利的。
所述催化剂的微孔容积应当优选地在0.2cm3/g至1cm3/g的范围，尤其是在0.2cm3/g至0.5cm3/g的范围。尤其优选的是微孔容积在0.2cm3/g至0.4cm3/g之间的范围。所述微孔容积按根据DIN 66133的快速银侵入法测定。微孔容积尤其涉及特定的总微孔容积(基于半径3.7-7500nm的微孔)。微孔半径可以采用根据DIN 66133的Washburn-平衡式确定。
所述催化剂或者说所述至少一种可烧结材料还包含一种催化活性的、或者说可活化的材料。优选的是，所述催化活性的、或者说可活化的材料选自镍、铂、钯、铑、钌、铜、银、金、钴、锰或者铁的氧化物的一种金属氧化物。尤其优选的是镍、铂和铑氧化物。对于ATR和CPOX最为优选的是铑。这些氧化物典型的是在把所述催化剂装入反应器中以后才激活，就是说，例如借助于氢还原成真正的催化活性金属。
所述催化剂可以附加地包含一个覆层。该覆层通常在煅烧以后敷设在所述催化剂上。为此，可以采用现有技术公知的方法，例如敷设一种修补基面涂层或者喷射浸渍。所述覆层用于提高所述催化剂的BET-表面积，以及抑制不利的烟灰生成，并且优选的是选自稀土氧化物(例如镧、铈或者铈/镧稳定的加玛氧化铝)铝酸盐、钛酸盐、二氧化钛、氧化铝、氧化镁、氧化锆，钛酸铝、铝酸钙、铝酸钾或者铝酸镁或者其组合。尤其优选的是铈/镧稳定的加玛氧化铝。
所述覆层还可以含有一种粘合剂。适合的粘合剂是，例如高岭土、陶土或者釉料。所述粘合剂还可以是一种溶胶，例如Al2O3的纳米颗粒制备的溶胶(例如Sasol公司的
Figure GSB00000353191400041
)，ZrO2(例如Mel-Chemicals的锆乙酸盐，
Figure GSB00000353191400042
产品)。此外优选的是氧化铈-溶胶(例如NYACOL制备的)，二氧化硅-溶胶(例如)和二氧化钛溶胶(例如Sachtleben-Chemie制备的)。此外所述溶胶还可以是一种饱和的金属盐溶液。
一种特别优选的粘合剂是饱和的硝酸铝溶液，所述硝酸铝溶液在煅烧时形成纳米级的氧化铝颗粒，所述氧化铝又起修补基面涂层粉末与浇注载体之间的粘合剂的作用。
所述催化剂载体和/或覆层可以含有其它镧系元素(稀土)，以及第I或者第II主族的元素(例如钾或者锶)，以稳定所述特定的表面，并且在另一个方面抑制不利的烟灰形成的副反应。
在此，优选的是一个尽可能高的BET表面，总体上说是高于0.4m2/g的BET表面，尤其是在0.5至300m2/g，并且尤其优选的是1至50m2/g之间的BET表面。所述BET表面按照根据DIN 66132的氮单点法测定。一个50m2/g的BET表面在运行所述催化剂可以在900℃的温度。
所述催化活性或者说可活化的材料，既可以在制备催化剂载体时就已经向可烧结材料掺入，也可以在其后的催化剂覆层时向所述修补基面涂层掺入，或者也可以在用修补基面涂层进行了催化剂覆层以后，以一种浸渍的形式用一种金属盐溶液、例如对应的硝酸盐、乙酸盐等等敷设并且接着煅烧，从而出现对应的金属氧化物。在此可以采用现有技术公知的方法，例如浸泡或者喷射浸渍。此外还可以采取通用的所有变形。
这样得到的催化剂可以用作ATR的蒸汽转化催化剂或者用作催化部分氧化反应(CPOX)的催化剂。优选的是所述催化剂用于其中在催化反应之前首先通过就地还原，例如用氢还原产生催化活性金属的反应器中。可能的反应器是固定床反应器、管式反应器和管束式反应器。
为此所述具有大面积结构的催化剂可以以一种松散装料的形式放在所述反应器中。所述松散装料适用于固定床反应器和管式反应器。
实施例1：制备一种有蜂窝状结构的催化剂载体：
铝酸钙在一个球磨机中碾粉碎，掺入白油，并且在一个双螺旋挤压机中混合并且加热到150℃。把得到的混合物转送到一个有蜂窝结构的注模中。冷却所述模具并且出模该管式催化剂，然后烧结。根据本发明制备的载体见于图1中。
实施例2：制备一个有蜂窝结构的覆层的催化剂载体：
该催化剂载体的制备同实施例1，只是用氧化铝替代铝酸钙。在烧结以后用修补基面涂层Clay Met(稳定了的加玛氧化铝)覆层，干燥，然后煅烧。
实施例3：对三个不同催化剂的活性检测：
制备了三个样品。为此，把常规的G-90LDP载体(Sued-Chemie AG制备)和根据本发明注模制备的载体破碎到约5×5mm的大小，而不破坏所述蜂窝结构。
用硝酸镍溶液浸渍G-90LDP以及注模制备的载体的一个试样，其中达到相对于修补基面涂层10％的镍含量。
注模制备的载体的另一个试样用Sued-Chemie AG公司的修补基面涂层“Clay Met”覆层、煅烧并且接着同样地以一种硝酸镍溶液浸渍。
所有三个试样都进行活性检测。检测结果参见图2和图3。
可以清楚地看出，覆以修补基面涂层载体的甲烷转化比用常规的G-90LDP高约16％。压力下降也可以减少约10％。
仅浸渍注模制备的载体的较差的结果，归咎于仅0.4m2/g的比较小的BET表面积。
实施例4：测定侧耐压强度：
该方法用测量仪器“Mecmesin”进行。
所述测量仪器投入使用：
横截线(Traversen)应当设定在列表型上(参阅使用说明书)。拉出保险钮，并且把模式开关置于“单个循环”。在测力机上按“0n”和“reset”。
进行测量：
应当由力柱推高喷射护板。所述催化剂以纵侧放在台子上，并且重新向下推喷射护板。接着把“start/stop开关”压到“Dowm”，然后松手。在折断催化剂以后显示和记录测量值。在得到50个测量值以后，借助于一个计算机分析测量值。在所有情况下侧压力都在700N以上。
附图说明：
图1是根据本发明制备的有蜂窝状结构的催化剂载体；
图2是对三个不同催化剂的活性检测结果；
图3是测定的侧耐压强度结果。

Claims (30)

1.具有大面积结构的催化剂设计，其特征在于，所述大面积结构由许多有圆形或者多边形截面的平行穿透孔构成，其中所述催化剂包含至少一种可烧结材料并且有至少700N的侧耐压强度，其特征在于，所述大面积结构通过在一个注模模具中注模至少一种可烧结材料得到，并且是一种蜂窝状结构，该蜂窝状结构每cm2绕流面积有10-300个穿透孔，其中至少一种可烧结材料选自金属氧化物和/或陶瓷。
2.如权利要求1所述的催化剂，其特征在于，所述穿透孔的截面构成圆的、三角的、四角的和/或六角的。
3.如权利要求1和2中任一项所述的催化剂，其特征在于，所述至少一种可烧结的材料选自铝酸盐、硅酸盐、钛酸盐，选自二氧化钛、氧化铝、氧化镁、氧化锆、压电陶瓷、工艺瓷、滑石、堇青石、富铝红柱石陶瓷、碳化物、氮化物、或者其组合。
4.如以上权利要求中任一项所述的催化剂，其特征在于，所述至少一种可烧结的材料包含一种催化活性的材料。
5.如权利要求4所述的催化剂，其特征在于，所述催化活性的材料选自镍、铂、钯、铑、钌、铜、银、金、钴、锰或者铁。
6.如权利要求1至5中任一项所述的催化剂，其特征在于，所述可烧结材料占催化剂重量的大于0小于等于100重量百分比。
7.如权利要求1至6中任一项所述的催化剂，其特征在于，所述催化剂附加地包含一个修补基面涂覆层。
8.如权利要求7所述的催化剂，其特征在于，所述修补基面涂覆层具有一种大的BET表面积，并且包含稀土。
9.如权利要求7或8所述的催化剂，其特征在于，所述修补基面涂覆层包含粘合剂以提高修补涂层附着性。
10.如权利要求9所述的催化剂，其特征在于，所述粘合剂是一种溶胶和/或一种金属盐溶液。
11.如权利要求10所述的催化剂，其特征在于，所述溶胶选自铝化合物或者锆化合物。
12.如权利要求11所述的催化剂，其特征在于，所述溶胶是一种饱和的硝酸铝溶液。
13.如权利要求7至12中任一项所述的催化剂，其特征在于，所述覆层是一种催化活性的材料，所述催化活性的材料选自镍、铂、钯、铑、钌、铜、银、金、钴、锰或者铁。
14.制备具有一种蜂窝状结构的催化剂的方法，该结构具有侧耐压强度至少700N，包含步骤：
a)把一种可烧结材料碾成粉末；
b)在所述可烧结材料中掺入一个弥散剂；
c)加热并且混合所得到的配料，以得出一种塑性的坯料；
d)把所述塑料坯料注入一个注模模具中；
e)冷却、出模并且煅烧该坯料。
15.如权利要求14所述的方法，其中在步骤e)的煅烧后在所述催化剂上敷设一个覆层。
16.如权利要求14所述的方法，其中所述覆层用修补基面涂覆层进行。
17.如权利要求15至16中任一项所述的方法，其中所述催化剂在覆层以后煅烧。
18.如权利要求15至17中任一项所述的方法，其中所述催化活性材料在覆层之前固定在修补基面涂覆层的固体组分上。
19.如权利要求18所述的方法，其中所述催化活性的材料选自镍、铂、钯、铑、钌、铜、银、金、钴、锰或者铁。
20.如权利要求14至19中任一项所述的方法，其中所述至少一种可烧结材料选自金属氧化物和/或陶瓷。
21.如权利要求14至20中任一项所述的方法，其中所述至少一种可烧结材料选自铝酸盐、硅酸盐、钛酸盐、二氧化钛、氧化铝、氧化镁、氧化锆、压电陶瓷、工艺瓷、滑石、堇青石、富铝红柱石陶瓷、碳化物、氮化物、或者其组合。
22.如权利要求14至21中任一项所述的方法，其中所述至少一种可烧结的材料附加地包含一种催化活性的材料。
23.如权利要求22所述的方法，其中所述催化活性的材料选自镍、铂、钯、铑、钌、铜、银、金、钴、锰或者铁。
24.如权利要求14至23中任一项所述的方法，其中所述弥散剂包含白油。
25.如权利要求14至24中任一项所述的方法，其中所述配料的加热在30至150℃的温度进行。
26.如权利要求14至25中任一项所述的方法，其中所述配料的加热和混合以得到所述塑性坯料在一个挤压机中进行。
27.把如权利要求1至13中任一项所述的或者根据权利要求14至26中任一项所述方法得到的催化剂，用作蒸汽转化催化剂。
28.把如权利要求27所述的催化剂，用在一个反应器中。
29.如权利要求28所述的应用，其中所述反应器是固定床反应器、管式反应器和管束式反应器。
30.如权利要求28或29所述的应用，其中所述有蜂窝状或者有其它大面积结构的催化剂，以一种松散装料的形式放在所述反应器中。
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