CN100430725C - 催化剂的测定方法和装置 - Google Patents

催化剂的测定方法和装置 Download PDF

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CN100430725C
CN100430725C CNB971920168A CN97192016A CN100430725C CN 100430725 C CN100430725 C CN 100430725C CN B971920168 A CNB971920168 A CN B971920168A CN 97192016 A CN97192016 A CN 97192016A CN 100430725 C CN100430725 C CN 100430725C
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R·C·威里森三世
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Abstract

将一种网格支架(10)如蜂窝体或平板，或各个载体颗粒的集合，用催化剂组分的溶液/悬浮液处理，以产生具有不同组分的多个网格、斑点或小丸(12)。这些许多网格、斑点或小丸被干燥、煅烧或处理以使组分稳定并与可能的反应进料流或反应物料接触。测量或分析在每个网格(12)中发生的反应以确定在每个组合物中催化剂的相对功效。通过一些不同的方法进行测量或分析，这些方法包括对产物或剩余反应物或所取样品进行进一步分析的红外温度测量法(14)和光谱法。在形成的网格、斑点或小丸(12)中可使用自动控制技术。

Description

催化剂的测定方法和装置
发明领域
本发明涉及一般催化剂的测定领域，本发明通常分类在美国专利分类号502或252中。本发明涉及一般催化剂的测定领域，本发明通常分类在美国专利分类号502或252中。
现有技术介绍
现有技术包括：96年1月8日的C&E News第30页的内容，该内容教导了反应性塑料及许多对于石油炼制领域公知的催化剂测试设备和方法；1995年第60卷的J.Org.Chem第6666-6667页的F.M.Menger、A.V.Eliseev和V.A.Migulin的“通过组合的有机化学开发的磷酸酶催化剂”(“Phosphatase catalysts developed viacombinatoriol organic chemistry”)；Xiang，268 Science 1738和Briceno，270 Science 273，两者都是关于固态化合物的组合文库；组合技术的Sullivan，Today’s Chem.At Work 14；组合文库标记为4723的Nessler 59 J.Org.Chem.；组合文库5588的Baldwin，117J.Amer.Chem.Soc..
现有技术存在的问题
常规催化剂测试是在试验室规模或较大的中试装置中完成的，在反应条件下进料与催化剂在这些装置中接触，一般对流出产物取样，经常对该取样进行分析，对其结果进行数据解析技术处理。这样的程序对一种催化剂的一次实验运行可需一天或一天以上的时间。虽然上述技术在精确调整最佳阵列、小丸(pellet)形状等方面具有重要作用，但本发明可在一次评选中对数十种催化剂进行扫描，通常比用传统方法评估一种催化剂所需要的时间要少。而且，当在其优选的自动控制(robotic)的实施方案中实践时，本发明明显地减少了每种催化剂筛选的工作成本。
发明简介
发明的一般描述
根据本发明，对多样品支架(载体)，例如蜂窝体或平板，或者各个载体颗粒的集合用催化剂成分的溶液/悬浮液处理，以填充板上的凹坑(well)，或产生网格(cell)、斑点(spot)或小丸来承载各种催化剂成分组合中的每一种，对载体进行干燥、焙烧或进行其它必要处理以使网格、斑点或小丸中的成分稳定，然后使载体与可能的反应进料流或批料(例如，瓦斯油、氢气和氧气、乙烯或其它可聚合单体、丙烯加氧气，或CCl2F2及氢气)接触，以催化生物化学反应，该反应由蛋白质、细胞、酶催化。对在每个网格中发生的反应例如通过红外线温度测量法、光谱法、电化学法、测光法、热传导法或其它方法来检测产物或剩余反应物，或通过例如多路(multistreaming)小体积样管法，从每种组合物附近取样，然后进行分析，例如光谱分析、色谱分析等，或通过例如热敏技术观察催化剂附近的温度变化来测量，以确定在每种组合物中的催化剂的相对效率。在形成网格、斑点、小丸等中可采用自动控制技术。
下面讨论这些参数：
催化剂：生物技术催化剂包括蛋白质、细胞、酶等。化学转化催化剂包括在反应条件下为固态的元素周期表中的绝大多数元素。烃类转化催化剂包括Bi、Sn、Sb、Ti、Zr、Pt、稀土及其它许多可能的候选催化剂，这些候选催化剂对于特定反应的潜能还没有被认识到。许多协同作用的组合是有用的。被负载的金属和金属络合物是优选的。化学催化剂可以作为元素、或作为在稳定步骤的温度下分解使元素或其氧化物沉积在基体上的有机或无机化合物、或作为稳定的化合物加在基体(载体)上。
载体：载体可以是惰性粘土、沸石、陶瓷、碳、如反应性塑料类的塑料、稳定的非反应性金属或上述的组合物。它们的形状可以是被通道穿过的多孔蜂窝体、颗粒(小丸)、或在上面沉积有许多催化剂候选物的小块(斑点)的平板、或平板中的凹坑。普通的催化剂基体材料尤其优选采用例如沸石USY类的沸石、高岭石、氧化铝等，因为它们可以模拟商业催化剂。
制备：候选催化剂的前体可以通过任何方便的技术沉积在载体上，优选通过吸管或吸垫(absorbing stamp)(类似橡皮垫(rubber stamp))或丝网。在优选实施方案中，沉积过程可在自动控制下进行，就象在生物化学测试中在多网格板上装填催化剂一样。催化剂的许多斑点可通过几次分别的沉积而得到，如穿过蜂窝体的通道可在其长度的三分之一处被堵塞住，在通道的上端三分之一充满催化剂溶液，然后堵塞物移到通道的三分之二处，吸管吸入第二种催化剂，然后去除堵塞物，加入第三种催化剂溶液，得到这样一种通道，当反应物流经通道时，它们依次与三种催化剂接触。催化剂也可通过离子交换、固体沉积、浸渍或这些方法的结合来加入。优选利用组合的化学或生物制备技术以制备本发明阵列的候选催化剂。两种或两种以上催化剂的共沉淀物可被淤浆化再涂布到载体上，需要时再活化。催化剂可用丝网负载到载体板上或载体通道的内部，并可用逐次遮蔽把不同的催化剂组合物加到不同的斑点上。
稳定步骤：一旦使催化剂负载在载体上，本领域公知的任何合适的技术可用于稳定和/或活化选择的特定的催化剂，以便使它们在反应步骤中保持在原位。尤其优选在原位进行焙烧、汽蒸处理、熔化、干燥、沉积和反应。
反应物：本发明对在催化剂存在下可被促进的任何反应都有利用价值，包括生物反应和无机及有机化学反应。化学反应包括聚合反应、卤化反应、氧化反应、水解反应、酯化反应、还原及任何其它可以从催化剂中获益的常规反应。如用于石油炼制中的烃类转化反应是本发明的一个重要的应用，包括重整、流化催化裂化、氢化、加氢裂化、加氢处理、加氢脱硫、烷基化和汽油脱硫处理。
传感器：用于在候选催化剂中检测催化活性的多个传感器并没有严格的限制，但是优选简单实用。特别优选采用多个色谱仪、多个温度传感器和多个光谱仪，尤其是那些适于例如通过多路技术、多道操作技术(multitasking)、取样技术、光纤或激光技术来测量靠近每种特定的催化剂斑点的温度和/或产物的那些。特别优选采用通过红外相机同时在多个催化剂位点记录温度的温度测量法。其它合适的多个传感器包括电化学传感器、荧光检测器、NMR检测器、NIR检测器、FTNIR检测器、Raman检测器、火焰离子化检测器、热传导检测器、质量检测器、粘度检测器和受激电子或X-射线发射检测器。多个传感器可检测气体或液体流或载体表面上的产物。在最好的催化剂处吸热反应表现为温度降低。一些传感器使用附加的检测试剂如臭氧来产生化学发光(chemiluminesce)。
标记物：标记物(示踪物)可任选地加入以便识别特定的催化剂，特别是颗粒作为催化剂载体的情况。这些标记物可以是如文献中已经讨论过的常规标记物。标记物可以是在反应条件下稳定的化学品，或可以是带有特征发射的放射性物质。组合化学的技术可使标记物以及选择的催化剂适用于通过催化剂得到加强的特定反应。
间歇或连续：虽然本发明优选建立在流动的基础上，在反应条件下反应物通过催化剂斑点流动，但也可使用例如在搅动的高压釜或搅拌的容器内的间歇测试，特别是在生物反应中。
温度、压力、空速和其它反应条件：这些条件由反应物和反应来确定。通过把载体放入一种反应室中，该反应室具有用于传感装置观测的蓝宝石或类似视窗或沿反应器壁有密闭铅封(pressure-tightlead)，从而可提供高压的反应条件。
发明的利用
本发明可用于促进气相或液相反应的生物技术的催化剂的测试；适用于测试在间歇或优选连续物料流条件下的催化剂；适用于在高压、低压或常压条件下测试；本发明节省了用于筛选改进催化剂以促进需要的反应所耗的时间和劳动。
附图简介
图1是优选的蜂窝状载体的示意图，自动控制的移液设备将不同催化剂成分的组合物沉积在每个穿过蜂窝状载体的通道中，然后煅烧该载体使在每个通道中的催化剂稳定。
图2是示意地示出了与流经通道的反应物接触的图1的蜂窝状载体。
图3a和3b为图2蜂窝状载体的一个通道的可选择的示意图，检测器通过测量经过产物或通道的激光束的吸收来检测离开通道的产物。
图4a示意地示出了在接收催化剂溶液之前中点处被堵塞住的通道，以及图4b示出了堵塞物移到通道的末端，于是形成了在其一半长度具有一种催化剂，在其另一半长度中具有另一种催化剂的通道。
图5图示出了一片载体，其中有15个不同催化剂组合物的斑点沉积在其上，这些正如在实施例1中讨论的。
图6a示出了在反应器中合适位置的载体的颗粒(小丸)的阵列，该阵列是在不同小丸(在图中小丸上用不同标记示出)已与不同催化剂组合物进行离子交换后的状态。图6b示出了一装填的反应器，该反应器不是优选的，因为上游的小丸接触新鲜的进料，而下游小丸部分接触已反应的进料。
优选实施方案说明
实施例1
参见图5，α型氧化铝10的片通过标准的方法洗涂(wash coat)上多孔的γ型氧化铝的颗粒。在聚苯乙烯制成的24孔微量滴定盘的孔中制备12种不同过渡金属元素的草酸盐溶液。使用Beckman Biomek2000自动控制的自动液体处理系统再次在微量滴定盘的孔中从原料制备稀释液和混合物。将自动装置用于在氧化铝载体10的表面的规定位置12(斑点)处沉积所得的每种溶液的20微升等分样，该载体10然后干燥、煅烧并插入到可在100到350摄氏度之间进行温度控制的反应器之中。在还原后，将可能的氧气和氢气的反应混合物送入反应器中。Agema红外传感相机14用于借助抛光的金属镜通过透红外线的蓝宝石视窗来观察氧化铝载体。设定相机，使其动态范围的下限与比进料温度低约40摄氏度的温度相对应，和最大信号涉及比进料温度高约200度的温度。催化剂组合物的斑点12周围局部温度的升高(对于吸热反应则降低)揭示了该组合物催化该反应，如相片18所示。
实施例1a
通过在强紫外线和/或可见光的照射下进行反应而交替地鉴别催化剂，其中红外线温度测量在照射停止后立即进行，或者通过在照射源上使用短路滤光片以消除对红外射线的污染。
实施例2
参见图2，多孔氧化铝整体物(monolith)20(Corning)具有穿过其整个厚度的以规则阵列延伸的方形或圆形截面通道，该整体物20在每个通道里用不同组合物的催化剂前体溶液处理，其中每种组合物在其自身通道里被隔开。在干燥，煅烧等后，在高温下，活化的整体物与流动的可能的反应混合物接触，并用Agema型相机在红外区中观察。反应的热函在显示催化活性的组合物附近产生局部的温差，这些作为靠近通道出口的温度变化而被观察到。
实施例3
参见图3，实施例2中描述的多孔陶瓷整体物20在其通道中装有不同的催化剂组合物，将该整体物以这样的方式安装在反应器(图中未示出)中，使每个通道的整个长度可在反应器的末端通过蓝宝石视窗观测。宽谱热红外线源安装于反应器的一端，产生区域性红外能通量密度。这样安置Agema IR感光相机以便能通过大部分孔直接观测红外线光源。将干涉滤光片或其它滤光片安装在相机和红外光源之间的反应器一侧，以便从光源到达相机的光基本上限于4到4.5微米之间的波长。在此波长范围的吸收率的观测用于在CO2(一种目标反应非所需的副产物)生成量的基础上比较候选的催化剂组合物。发现所选的低二氧化碳生成量的催化剂组合物(与高的总转化活性结合，通过所需产物的红外吸收或红外温度测量法进行测量)对所需的产物相比于CO2副产物有高选择性。
实施例4
催化剂前体组合物的集合通过自动液体处理装置进行制备，催化剂载体颗粒与每种组合物接触。在进一步处理以使催化剂前体稳定和活化之后，将催化剂小丸在表面上排列，暴露于可能的反应性环境中，它们的活性由红外温度测量法确定。
实施例5
催化剂前体组合物的溶液在许多个单独容器中制备。每种组合物还包括少量的示踪材料(如不同比例的元素碳或硫的稳定同位素)。催化剂载体颗粒与催化剂前体的配方接触并被活化。小丸然后在某一时刻与可能的反应混合物接触(例如，通过淘析到封闭的体积内)以及对其活性测量(通过温度测量法，通过产物的光谱测量，或者气相或液相周围的取样)。收集显示活性的颗粒并对示踪材料的含量进行单独分析，以便确定给出所需催化活性的组合物。
实施例6
重复进行实施例2的操作，不同的是，只有一部分孔隙长度涂有候选催化剂，以便使未改性的整体物孔壁的观测值作为光学均匀性的参照标准。
实施例7
在没有反应物存在下，通过在所需的实验温度下保持整体物，在有用的波长范围绘制实施例2载体的载体整体物孔的热发射性(emissivity)。以数字形式存储的热发射性图用于使在实验条件下测量的红外能通量归一化，以提高可估计的局部温度的精度。
实施例8
高的、基本上均一的热发射性表面位于实施例2的整体物的末端，远离相机，靠近与整体物通道材料进行辐射传热/接触处。观测最靠近每个通道开口端的部分表面的温度。在这种情况下，有必要使气体经过均一辐射表面进入通道中，可借助于孔隙或借助于辐射表面和整体物之间的小偏移(offset)来实现。
实施例9
作为可选择的方案，催化剂的斑点可沉积在反应器如载体材料所形成的管子的内表面上，并且在反应器外侧的相应斑点的温度可测量到，从而通过热传导来确定各个催化剂在反应中温度是提高还是降低。
实施例10
重复实施例1的过程，不同的是，反应物处于液相，及液相分析用于测定各个催化剂候选物的活性。
实施例11
重复实施例4的实验，不同的是，金属载荷通过溶解小丸并直接分析该金属载荷来直接测量。
实施例12
α型氧化铝的片通过标准的方法用多孔γ型氧化铝的颗粒洗涂。在聚苯乙烯制成的24孔微量滴定盘的孔中制备12种不同种过渡金属元素的草酸盐溶液。使用Beckman Biomek 2000自动液体处理系统再次在微量滴定盘的孔中从原料制备稀释液和混合物。将Biomek自动装置用于在氧化铝载体表面的规定位置处沉积所得的每种溶液的40微升等分样，然后将该氧化铝载体干燥、煅烧，并插入到控制在200摄氏度的反应器之中。在200摄氏度下加入氢气(97.5％)和氧气(2.5％)的气态混合物。红外传感相机用于通过能透过红外线的蓝宝石视窗观测氧化铝载体。设定相机使其下限与进料温度相对应，并且最大信号与高出进料温度20度的温度相对应。通过组合物斑点附近的局部温度的升高而显示出组合物催化该反应。
实施例13
多孔氧化铝整体物具有沿其整个厚度以规则阵列延伸的方形孔，该孔分布的密度为每平方英寸25个，对该氧化铝整体物洗涂氧化铝颗粒。然后使通道部分地填满不同组合物的溶液，每种组合物包含一种或多种金属草酸盐或硝酸盐，每种组合物在其自身的通道或通道组中被隔开。在氢气存在下干燥和活化后，活化的整体物放入装有蓝宝石视窗的反应器中，在其中可使用红外传感相机在红外线中观测它。定位相机以便能观察到载体壁。载体在每一个象素下的相对热发射性通过整体物在红外线中的显像来确定，这时将反应器和整体物固定在几个恒定温度的每一个温度上，同时使氮气通过反应器。
然后向反应器通入在氢气中含有2.5％(摩尔)氧气的气体混合物。反应器和进料温度开始设定在40摄氏度，然后逐渐增加，此时装有催化剂的整体物重复地在红外线中显像。在每个网格中的温度可通过观测靠近通道的催化剂前体涂布区的末端的网格，或者通过由在非反应条件下所摄的图象计算出的热发射率使观测到的红外能发射归一化来判断。表明最早升温超过反应器温度的网格中的组合物可用作氢氧化催化剂。
实施例14
用氧化铝颗粒洗涂多孔氧化铝整体物，该多孔氧化铝整体物具有沿其整个10厘米厚度以规则阵列延伸的方形通道，其通道的密度为每平方英寸25个。然后对通道部分地填满不同组合物的溶液，每种组合物包含一种或多种金属盐，而在某些情况下还包括如钡、铯或钾化合物的候选改性剂，每种组合物在自身的通道或通道组中被隔开。
在氢气存在下进行干燥和还原后，将活化的整体物置于反应器中，在其中可通过使用红外相机经过蓝宝石视窗来观测它。第一个视窗位于距整体物的表面0.5厘米处。设置该相机，使得可通过视窗、通过载体的通道和通过第二个蓝宝石视窗朝向红外放射源来观察。
然后向反应器通入混有氧气和氩气的甲烷气，并使该气体朝向相机流经整体物的通道。将选择性地使波长为4.3微米的红外线射线通过的光学滤光片插到红外光源和相机之间，其中所述的波长可被二氧化碳强烈吸收。在每个通道中的二氧化碳的有效浓度可从在该通道中的4.3微米的红外强度推算出。每个象素在4.3微米处的读数除以从滤光片所得的读数以校正可能的光学假像的影响，该滤光片对于4.3微米附近但不能被二氧化碳、甲烷或水强烈吸收的红外波长有选择性。
在长期暴露于工作条件后，具有高浓度二氧化碳的组合物可用于甲烷的催化氧化。
实施例15
催化剂前体的组合物的溶液在各种单独的容器中制备。每种组合物还包括少量示踪材料(如只有每种组合物才有的不同比例的硫元素的稳定同位素)。使催化剂载体颗粒与催化剂前体组合物的配方接触，并活化。然后使小丸在某一时刻与可能的反应混合物接触(例如，通过淘析到封闭的体积内)以及测量其活性(通过温度测量法，通过产物的光谱测量，或者气相或液相周围的取样)。显示活性的颗粒被收集，并对示踪材料的含量进行单独分析，然后确定给出所需催化活性的组合物。
实施例16
以这样的方式制备具有以规则阵列沿其整个厚度延伸的方形通道和密度为每平方英寸9个通道的聚四氟乙烯块体，使在其每个通道的底部存在有浅洞。每个洞装有在其表面上带有磺酸基的不同的聚合物配方，并安装多孔定位筛网以保持聚合物样品在适当的位置。
载有催化剂的整体物放入反应器中，在其中可通过位于距块体表面0.5厘米处的视窗观测它。配置相机，以便可通过蓝宝视窗，通过载体的通道及通过第二视窗朝偏振光源观察，把起偏器安装在块体和相机之间。
向反应器供给蔗糖溶液，以便使其流过块体的通道。通过旋转起偏器到不同的角度并观察通过每个通道的光的亮度变化来测量偏振光在通过每个通道中的液体时旋转的角度。在旋转角度变化最大的通道中发现的候选催化剂可用作蔗糖水解的催化剂。
实施例17
在强紫外线和/或可见光照射存在下，通过在实施例16的装置中进行反应识别用于己烷光氧化的催化剂，其中在照射停止后，立即进行红外温度测量，或者通过在照射源上用短路滤光片来消除对红外射线的污染。
实施例18
将溴化氰活化的交联琼脂糖小球的样品暴露在不同pH值、盐浓度和酶浓度的醇氧化酶的溶液中。在酶偶联后，将残留的活性基团用乙醇胺抑制，对小球进行清洗，把每种样品放置在多凹坑板的分开的凹坑中。将该板暴露于含有乙醇蒸汽的流动空气流中，并用Amber红外传感相机观测。把温度增加最多的样品选择为高活性固定化醇氧化酶催化剂。
实施例19
将溴化氰活化的交联琼脂糖小球的样品暴露在不同pH值、盐浓度和抗体浓度的抗醇氧化酶抗体溶液中。在酶偶联后，将残留的活性基团用乙醇胺抑制。对小球进行清洗，暴露于醇氧化酶的溶液中，再次清洗，并将每种样品放置在多凹坑板的分开的凹坑中。将该板暴露于含有乙醇蒸汽的流动空气流中，并用Amber红外传感相机观测。把温度增加最多的样品选择为高活性固定化醇氧化酶催化剂。
实施例20
对具有穿过其整个厚度以正交行/列格式排列的通道的陶瓷整体物洗涂多孔的氧化铝颗粒，在每列中的所有通道用同一催化剂前体处理，进行活化。可能的反应物流流经整体物的通道，多波长射线束平行每一列穿过整体物的表面，到达位于该列末端的检测器。离开那个列细孔的物流的组成通过处理检测器的输出而进行估计，该检测器输出包括傅利叶转换和/或在不同波长下的强度的加权求和/求差。
实施例21
将带有能催化反应物的D-和L-立体异构体转化的催化活性基团的小丸用各种可能择优抑制(临时或永久)该化合物的L-立体异构体被催化剂转化的物质进行处理。该小丸分布在多凹坑板的凹坑中，并暴露于待改性的化合物的异构体的混合物中。使L-异构体的转化活性有最大下降的用抑制剂进行处理的小丸可用于D-异构体的立体选择性改进。
实施例22
将具有穿过其整个厚度以正交行/列的格式排列的通道的陶瓷整体物洗涂多孔的氧化铝颗粒，通道用催化剂前体处理，进行活化。可能的反应物流流经整体物的通道。由阵列管子组成的歧管用于把含有臭氧的物流引导到流过每个通道靠近其出口的物流中，其中所述的每一个管子比单独通道的尺寸小。引入的臭氧与所需的产物的反应会发出光，该光可由朝向整体物的相机检测到。发出最强烈光输出的催化剂组合物是将反应物转化成臭氧反应性的所需产物的很有用的催化剂。
实施例23
将具有穿过其整个厚度以正交行/列的格式排列的通道的陶瓷整体物洗涂多孔的氧化铝颗粒，通道用催化剂前体处理，活化，然后暴露于可能的去活化物质中。可能的反应物流流经整体物的通道。由阵列管子组成的歧管用于对流经每个通道内的物流进行取样，其中所述的每一个管子比单独通道的尺寸小。取自每个通道的样品通过开关阀门装置依次引导到联用的气相色谱-质谱仪中，提供所需产物的最大产率的催化剂组合物可用于该反应物流的转化。
变化实施方案
这里讨论的特定组合物、方法或实施方案只是用来说明本说明书公开的本发明。在本说明书教导的基础上对本领域的技术人员来说对这些组合物、方法或实施方案的改变是很容易实现的，因此这些变化也包括在本发明公开的部分内。例如统计设计的实验和自动的反复实验过程方法可用于使测试时间进一步缩短。优选通过沉淀或沉积法将预先形成的催化元素(特别是沉淀物，还有单分子和络合物如金属茂)连接/排列在载体上的方案在许多情况下是有用的。
检测可包括把一些试剂加到离开每个候选物的物流中，试剂通过染色或反应提供一个可检测的产物例如光等对催化剂产物进行检测。
载体可包括为使流动均匀分布而设定的特定排列的阵列，例如插入到块体每个通道中的多个输送管的集管。
检测装置可包括电化学装置、或用于金属累积测量的γ相机；通过中子激活及通过胶片或发射的放射性存储板成像的成像元素的分析；通过声频高温测定的温度测量、辐射热测量法、电化学检测法、传导性检测法、液相测定、优选溶解载体小丸和直接分析金属载荷；测量在液相中的折射率；在没有通常的发射源而替代地使用以特征波长发射的辐射热气体来直接观察产物气体的红外发射。
其它变型可包括在使一些位点故意中毒后进行选择性测试，特别是在手性催化等中。
配方可以斑点或层的形式负载在包含孔或通道，或穿过载体整个范围的通道的载体表面上。该载体可包括碳、沸石和/或塑料。该塑料可包括反应物。载体可支撑由共沉淀物或铝或颗粒制成的催化剂的形式。
至少一种配方可优选地包括选自下组的一种材料：过渡金属、铂、铁、铑、锰、金属茂、锌、铜、氯化钾、钙、锌、钼、银、钨、钴和它们的混合物。
示踪物可包括不同同位素或同位素的不同混合物。反应条件可包括比1巴的绝对压力大的压力，并且可在比100摄氏度高的温度下接触。
该方法可包括对在各个配方的附近由于反应吸热或放热导致的温度变化进行检测。该方法可包括用还原剂处理。接触步骤可在改变金属在多孔载体内的分布的化合物存在下进行。候选催化剂配方可以斑点或层的形式在载体表面上被接触，该载体含有由底层支持的洗涂层(washcoat)。
稳定步骤可在温度梯度下或借助其它方法进行，从而使某些候选催化剂配方暴露于不同的温度下。稳定化包括焙烧、汽蒸处理、干燥、反应、离子交换和/或沉淀。在检测由于反应引起的温度变化时，可以利用与化学组成差异有关的热发射性误差的校正。
待测试的配方的阵列可包括固定在载体上的预先形成的金属茂或其它催化络合物。
红外射线可通过非色散的红外光谱或红外传感照相胶片来进行检测。该检测器装置包括用于在候选配方的阵列上进行物理扫描的装置。
多波长的观测值可通过数学处理来加工，如转换、加权求和和/或求差等。反应活性、反应物或产物可通过附加的反应来检测，该附加的反应可发出反应或特定化合物或化合物种类存在的信号。化学发光可用作反应活性或特定化合物或化合物种类的指示剂。大致上准直的发射源可用于产物检测/成像。多管取样可将样品引入质谱仪、色谱仪或光学监测器中。为模拟老化等，配方可暴露于可使至少一种配方的活性减少至少10％的有害试剂中，然后任选地暴露于水蒸汽、热、氢气、空气、液体水或其它不同的物质中或条件下，这些物质或条件可使集合的至少一种组分的活性比从前减少的活性增加至少10％，由此可测量再生、再活化、除焦或其它催化剂的性能。有害试剂可包括高温、V、Pb、Ni、As、Sb、Sn、Hg、Fe、S或其它金属、H2S、氯气、氧气、Cl和/或一氧化碳。
本说明书中参照的专利或文献纳入本文作为参考。

Claims (27)

1.一种从至少两种候选配方的集合中测试或选择能催化转化给定反应物或反应物混合物的多个催化剂配方的方法，其中至少一种反应物为液相，该方法包括以下步骤的组合：
a)将多个不同催化剂配方分开负载在一种或多种载体上；
b)在反应条件下在共同的反应器中使所述多个负载的配方与一种或多种反应物同时接触，每个候选的催化剂在其自己的反应部位；和
c)通过以下方法测定所述多个候选催化剂配方的相对效率：
(i)通过色谱法分析多个产物或多个未反应的反应物；或
(ii)通过光谱法同时分析多个产物或多个未反应的反应物，
其中所述多个候选催化剂配方在有一个或多个射线-透射视窗的反应器中同时接触，所述多个反应产物或多个未反应的反应物由射线穿过一个或多个射线-透射视窗照射，并且由光谱法穿过一个或多个射线-透射视窗检测所述多个反应产物或多个未反应的反应物而确定所述多个候选催化剂配方的相对效率。
2.权利要求1的方法，其中通过紧靠所述各个负载配方处进行取样或观测，并使用色谱法或光谱法分析所述样品以获取产物或反应物组成来测定候选催化剂配方的相对效率。
3.权利要求1的方法，其中所述多个催化剂配方以在共同载体的表面上的阵列反应部位的形式被接触。
4.权利要求1的方法，其中多个所述催化剂配方负载在为惰性粘土、沸石、陶瓷、碳或塑料的载体上，所述载体的形状可为通道贯穿的蜂窝状、颗粒、板或板中的凹坑。
5.权利要求1的方法，其中各个配方通过它们在载体上不同催化剂配方排列中的位置和/或通过分析与每一配方物理相关的独特标记物来鉴定。
6.权利要求1的方法，还包括将所述多个催化剂配方暴露到使至少一种配方的活性下降至少10％的物质中或条件下，然后测量活性来测量稳定性。
7.权利要求1的方法，其中所述负载步骤包括使多孔载体与金属盐的溶液接触或与氢接触。
8.权利要求1的方法，还包括将所述多个负载的候选催化剂配方暴露于不同的温度、焙烧、汽蒸、干燥、反应、离子交换和/或沉淀的条件下。
9.权利要求1的方法，其中通过对所述多个反应产物或多个未反应的反应物进行多波长的光谱分析确定候选催化剂配方的相对效率。
10.权利要求1的方法，其中所述多个产物或多个反应物由选自红外光谱、核磁共振光谱(NMR)、拉曼光谱、激光光谱、光谱法和质谱的技术检测。
11.权利要求1的方法，其中所述多个候选催化剂配方在有用于对多个反应部位每一个部位的包含产物的物流进行取样的多个取样管的反应器中同时接触，并且多个取样管适于：(i)在多个反应部位和多个光谱仪或色谱仪之间提供流体连通，所述光谱仪或色谱仪用于多路检测多个流出的含有产物的物流的每一个物流中的反应产物或未反应的反应物，或(ii)在多个反应部位和将多个含有产物的物流送入多个光谱仪或色谱仪的转换阀排列之间提供流体连通。
12.权利要求1的方法，其中所述多个候选催化剂配方在反应器中同时接触，其中检测器包括用于对多个反应通道的每一个通道中含有产物的物流进行取样的阵列管子，和其中所述多个候选催化剂的相对效率用光谱法同时分析所述多个产物或多个未反应的反应物来检测，该分析方法还包括物理扫描所述阵列管子并将所述多个含有产物的物流送入到光谱仪中。
13.权利要求1的方法，其中所述多个候选催化剂配方在反应器中同时接触，其中检测器包括用于对多个反应通道的每一个通道中含有产物的物流进行取样的阵列管子，和其中所述多个候选催化剂的相对效率用色谱法分析所述多个产物或多个未反应的反应物来检测，该分析方法还包括物理扫描所述阵列管子并将所述多个含有产物的物流送入到色谱仪中。
14.权利要求1的方法，其中所述的检测步骤包括测量偏振光的旋转角。
15.权利要求1的方法，其中反应条件包括高于100℃的温度，和/或大于1bar的压力。
16.权利要求1的方法，其中所述多个催化剂配方负载在多样品支架上。
17.权利要求16的方法，还包括处理所述多样品支架上的所述多个负载的催化剂配方，然后在多样品支架上在反应条件下同时使所述处理后的催化剂配方与反应物或反应混合物接触。
18.用于评价多个不同候选催化剂配方催化效能的设备，该设备包括：
共同的反应器，其包括在一种或多种载体上的多个分开的反应部位，多个反应部位的每一个部位都包含不同的候选催化剂配方，该反应器适合使得所述多个候选催化剂配方在反应条件下同时与一种或多种反应物接触；和
用于测定所述多个候选催化剂配方相对效率的检测器，
该检测器的特征在于：该检测器适合分析所述多个反应、多个反应产物或多个未反应的反应物，并且在于：该检测器包括(i)使用光谱法对由所述多个候选催化剂催化的所述多个反应中的所述多个反应产物或多个未反应的反应物同时进行分析的多个光谱仪，或(ii)使用色谱法对由所述多个候选催化剂催化的所述多个反应中的所述多个反应产物或多个未反应的反应物进行分析的色谱仪，
其中检测器包括用光谱法同时分析用所述多个候选催化剂催化的所述多个反应的所述多个反应产物或多个未反应的反应物的光谱仪，该设备还包括适合穿过一个或多个射线-透射视窗用射线同时照射多个反应产物的辐射源，并且该检测器适合同时测定在反应过程中穿过一个或多个射线-透射视窗由反应产物或未反应的反应物吸收或发射的射线。
19.权利要求18的设备，其中所述的反应器还包括共同的载体，所述载体具有用于所述多个候选催化剂配方的反应部位。
20.权利要求18或19的设备，其中所述的反应器包括多个具有不同组成的候选催化剂，和包有所述多个候选催化剂的反应室，该反应室适合使得其能够被包括一种或多种反应物的气体加压以使所述一种或多种反应物在反应条件下同时接触多个候选催化剂。
21.权利要求18的设备，其中辐射源是适合用偏振光同时照射多个反应产物的偏振光源，并且该检测器包括在反应过程中测定偏振光旋转角的偏振器，以确定所述多个候选催化剂的相对效率。
22.权利要求18的设备，其中反应器是流动反应器，所述流动反应器还包括为含有反应物的物流流过多个反应部位的每一个部位提供均匀流动的流体分配系统。
23.权利要求18的设备，其中反应器是流动反应器，所述流动反应器还包括适合在多个反应部位和多个光谱仪或色谱仪之间提供流体连通的多个取样管，所述光谱仪或色谱仪用于多路检测多个流出的含有产物的物流的每一个物流中的反应产物或未反应的反应物。
24.权利要求18的设备，其中反应器是流动反应器，所述流动反应器还包括用于从多个反应部位的每一个部位的含有产物的物流中取样的多个管子，和将多个含有产物的物流引入多个光谱仪或多个色谱仪的转换阀排列。
25.权利要求18的设备，其中反应器是流动反应器，所述流动反应器包括用于从多个反应部位的每一个部位的含有产物的物流中取样的阵列管子，和物理扫描所述阵列管子并将所述多个含有产物的物流引入光谱仪或色谱仪的装置。
26.权利要求18的设备，其中反应器适合提供包括高于100℃的温度和/或大于1bar的压力的反应条件。
27.权利要求18的设备，其中所述的检测器包括红外敏感型照相机、拉曼光谱仪、FTIR光谱仪、质谱仪、气相色谱仪或液相色谱仪。
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