CN1247446C - 运转燃料电池的方法 - Google Patents

运转燃料电池的方法 Download PDF

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CN1247446C
CN1247446C CNB2003101245807A CN200310124580A CN1247446C CN 1247446 C CN1247446 C CN 1247446C CN B2003101245807 A CNB2003101245807 A CN B2003101245807A CN 200310124580 A CN200310124580 A CN 200310124580A CN 1247446 C CN1247446 C CN 1247446C
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孙祥宁
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ExxonMobil Chemical Patents Inc
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Abstract

本发明涉及甲醇与水的催化转化生成氢气和二氧化碳的一步方法，方法中使用不含氧化铜和/或氧化铬的催化剂，只生成微量的一氧化碳，并且催化剂不会迅速失活。

Description

运转燃料电池的方法
本申请要求1996年12月31日申请的美国临时专利申请60/034,114号的优先权。
                        发明领域
本发明涉及甲醇与水的催化转化生成氢气和二氧化碳的一步方法，方法中使用不含氧化铜和/或氧化铬的甲醇转化催化剂，只生成微量的一氧化碳，并且催化剂不会迅速失活。
                         发明背景
氢气可用于燃料电池或其它目的如与化学和动力有关的应用，其制备可以通过甲醇与蒸汽转化生成二氧化碳和氢气：
                     
一般需要两步反应。第一步，甲醇分解为氢气和一氧化碳：
                      (1)
第二步，即称为“水转换”的反应，一氧化碳与水反应生成二氧化碳和另外的氢气：
                     (2)
甲醇转化的一步方法成本上更合算并且适于更多的应用。
从理论上讲，由二氧化碳和水合成甲醇的催化剂也应能够转化甲醇，得到二氧化碳和氢气。但是，合成甲醇的催化剂在甲醇与蒸汽的转化过程中会迅速失活。可以一步转化甲醇又不会迅速失活的甲醇转化催化剂将是很理想的。
发明概要
本发明提供了转化甲醇生成氢气和二氧化碳的方法，包括使甲醇和水通过甲醇转化催化剂，催化剂中含有至少一种金属氧化物，不含有选自于氧化铜和氧化铬的金属氧化物，甲醇与水的比、温度、压力以及重量时空速度都足以使甲醇转化生成氢气和二氧化碳。
发明详述
大体上目前使用或文献中报道的所有甲醇转化催化剂都含有氧化铜和/或氧化铬。本发明人发现不含有氧化铜和/或氧化铬的甲醇转化催化剂对于转化甲醇生成二氧化碳和氢气更有效，而且这些催化剂不象含有氧化铜和/或氧化铬的催化剂那样迅速失活。
本发明的甲醇转化催化剂具有如下的组成通式(干基)：
XaYbZcOd
其中
X为选自于元素周期表中IA族、IB族、IIA族和IIB族的金属。
此类金属包括，但不一定限于铍、镁、钙、锶、钡、锌、镉、汞、铷、铯、银及其组合。在优选的实施方案中，X选自于锌、镉、汞及其组合；
Y选自于铍、镁、钙、锶、钡及其组合；
Z为载体、填料或粘结剂材料，材料中含有其它金属，如IIIA族IVA族金属，包括但不限于硼、硅、铝、硅铝酸盐、锆、钛、铪、镓、镧、钪、钇及其组合。在优选的实施方案中，由于铝和硅不易氧化或还原，Z选自于铝、硅及其组合；
a：b和a：c的比值为1∶0.001到1000，优选地为1∶0.01到100，最优选地为1∶0.1到10；并且
d随X、Y和Z的氧化态的不同而不同。
优选地，基于催化剂组合物(干基)总重，每种金属按照各自的金属氧化物计算的总金属承载量应约为50％。
用于制备催化剂的金属化合物可以为任何无机或有机金属物质，这种物质在暴露于足够的热和/或氧化剂时会分解，生成金属氧化物。可形成溶液的可溶性金属化合物为优选的，通过溶液，该化合物可以浸渍在固体载体上，然后进行热分解。水溶性金属盐为最优选的。这些物质的例子有有机盐，如乙酰丙酮、乙酸盐、甲酸盐、胺盐等等的络盐。硝酸盐为优选的，可以提供由金属的含水溶液浸渍到载体上的容易得到的、成本有效的方法。例如，氧化铝粉末可以与含锌化合物一同浸渍，并且浸渍粉末可以制成不同的形状，或者可以把锌浸渍到预先制备的有所需形状的载体上，如丸剂、颗粒、片剂、珠粒、挤出料、筛分颗粒等等。
可以通过本领域熟知的许多方法，如干法混合、起始湿法浸渍、离子交换、共沉淀等等，制备催化剂。就浸渍而言，应使干的固体载体与一种化合物或盐，如锌盐的溶液接触，然后与另一种化合物或盐，如钙盐的溶液接触，或反过来。固体载体也可与含有多于一种化合物或盐的溶液接触。优选地，固体载体应如下进行浸渍(a)通过起始湿法方法，需要最小量的溶液，以使全部溶液在最初或经过蒸发后被吸收，或(b)通过一种方法，需要从一种或数种溶液吸收，随后通过过滤或蒸发使成分全部吸收。可以在各种条件下进行浸渍，包括环境温度或高温，以及大气压或高压。然后可把浸渍载体干燥或煅烧。
此外，可以通过沉淀方法，制备无载体的催化剂。例如，可以通过把适当的试剂，如理想的金属成分的化合物或盐与碱，如氢氧化钠、碳酸钠、氢氧化铵等等混合制备催化剂。金属通过与碱性试剂接触，形成了共沉淀。
在浸渍或沉淀后，可在有氮气和/或氧气的气流中，或在真空中，在高于约25℃，优选地在约75℃到150℃的温度范围内加热，使催化剂干燥。应在足以使复合物或盐中的金属分解，以形成相应的金属氧化物的温度下煅烧催化剂。适宜的煅烧温度范围为约100℃到约700℃，优选地为约200℃到约500℃。应避免过高的温度。可在约200℃到约500℃，优选地在约250℃到约350℃的温度下，通过还原，优选地通过与氢气或含氢气气体接触还原，使催化剂活化。
催化剂一旦活化后，甲醇与水的混合物就可以与催化剂接触，优选地在固定床中(a)在催化区，温度范围为约100℃到约1000℃，优选地为约200℃到约800℃，最优选地为约400℃到约700℃，并且(b)压力范围为约0.068千帕到约6，800千帕(0.01-1000磅/平方英寸(绝压))，优选地为约0.68千帕到约5,440千帕(0.1-800磅/平方英寸(绝压))，最优选地为约3.9千帕到约1,700千帕(0.5-250磅/平方英寸(绝压))。甲醇与水的摩尔比应为约1或小于1，优选地为小于1。重量时空速度-即小时流速与甲醇重量和催化剂重量的比，范围应为约0.01小时-1到约500小时-1，优选地为约0.1小时-1到约200小时-1，最优选地为约0.3小时-1到约50小时-1。可通过改变反应参数，控制转化率。一般地，较低的重量时空速度和较高的温度下，可得到较高的转化率。
本发明适用于生产氢气燃料电池。燃料电池为把燃料的化学能直接地转化为电能和/或热能的电化学装置，如同Kirk-Othmer化工百科全书，1997年，第4版，John Wiley&Sons公司出版，第11卷，1098-1121页中介绍的，此处引用作为参考。
本发明可通过参考以下实施例，得到更好的理解。
                  实施例I-催化剂的制备
在室温下，通过在50毫升水中溶解6.97克二水合乙酸锌和4.21克一水合乙酸钙，制备了水溶液。在此溶液中加入1.5克135等级的氧化硅-氧化铝和0.5克951等级的硅，二者都是从Aldrich化学公司购买的。把此混合物在110℃下干燥，随后在550℃下煅烧16个小时。然后把催化剂研磨并造粒，以得到筛目为-16到+20的筛分颗粒，以进行进一步的评价。
                    实施例II-发明物
把5.0立方厘米(大约3.3克)的实施例I中制备的催化剂与15立方厘米的石英珠混合，并装填入由三区电炉加热的1.9厘米(3/4英寸)外径的316不锈钢管状反应器中。第一区作为预热区，使进料汽化。中心区的温度设置为480℃。压力保持在约134千帕(5磅/平方英寸(绝压))。在0.89小时-1的重量时空速度下，摩尔比为1∶1的甲醇/水混合物与催化剂相接触。以预定时间间隔，通过装有热导检测器和火焰离子化检测器的在线气相色谱分析流出物。甲醇生成二氧化碳和氢气的转化率基本上为100％。在流出物中只检测到了很少量的甲醇、CO和二甲醚。
本实施例说明，作为本发明的方法，一步转化方法是可以做到的。
本领域中具有一般技能的人会理解，在不违背本发明的精神和范围的前提下，可以对本发明做很多修改。此处介绍的实施方案只是用做例证，不应作为本发明的限制，这些在下面的权利要求中有说明。

Claims (8)

1.一种用氢气运转燃料电池的方法，其中所述氢气是通过转化甲醇生成氢气和二氧化碳的方法而获得的，所述转化方法包括使甲醇和水通过甲醇转化催化剂，催化剂中含有至少一种金属氧化物，在小于1的甲醇与水摩尔比下以及有效的条件下，使甲醇直接转化生成氢气和二氧化碳，其中甲醇转化催化剂具有如下的干基组成通式：
                     XaYbZcOd
其中
X为选自于锌、镉、汞及其组合的金属；
Y为选自于铍、镁、钙、锶、钡及其组合的金属；
Z为选自于硼、硅、铝、锆、钛、铪、镓、镧、钪、钇及其组合的物质；
O为氧；并且
a∶b和a∶c的比值为1∶0.001-1000，d的取值为平衡X、Y和Z的氧化态，
其中所述有效的条件包括
温度的范围为100℃到1000℃；
压力的范围为0.068千帕到6,800千帕；而且
重量时空速度的范围为0.01到500小时-1。
2.权利要求1的方法，其中大体上全部甲醇转化生成氢气和二氧化碳。
3.权利要求1的方法，其中X包括锌。
4.权利要求1的方法，其中Z为选自于铝、硅及其组合的物质。
5.权利要求1的方法，其中a∶b和a∶c的比值为1∶0.01-100。
6.权利要求1的方法，其中温度范围为200℃到800℃。
7.权利要求1的方法，其中压力的范围为0.68千帕到5,440千帕。
8.权利要求1的方法，其中重量时空速度的范围为0.1小时-1到200小时-1。
CNB2003101245807A 1996-12-31 1997-12-31 运转燃料电池的方法 Expired - Fee Related CN1247446C (zh)

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SA98181082B1 (ar) 2006-03-15
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EP0950017A1 (en) 1999-10-20
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NO993228L (no) 1999-08-30
CA2275210A1 (en) 1998-07-09
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US6057261A (en) 2000-05-02
CN1133577C (zh) 2004-01-07
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AU731867B2 (en) 2001-04-05
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