CN1226966A - 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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CN1226966A
CN1226966A CN97192016A CN97192016A CN1226966A CN 1226966 A CN1226966 A CN 1226966A CN 97192016 A CN97192016 A CN 97192016A CN 97192016 A CN97192016 A CN 97192016A CN 1226966 A CN1226966 A CN 1226966A
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R·C·威里森三世
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Abstract

将一种多孔支撑体(10)如蜂窝体或平板,或单独载体颗粒的聚集体,用催化剂组分的溶液/悬浊液处理,以产生具有不同组分的多个网格、点滴或小丸(12)。这些许多网格、点滴或小丸被干燥、煅烧或处理以使组分稳定并与可能反应的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采样品进行进一步分析的红外温度记录法(14)和光谱法。在形成的网格、点滴或小丸(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，该内容公开了活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“通过组合有机化学来开发磷酸酶催化剂”(“Phosphatase catalysts developed via combina toriol organic chemistry”)；Xiang,268 Science 1738和Briceno,270 Science 273，两者都在固态化合物的组合文库中；在组合技术中的Sullivan,Today’Chem.At Work 14；在组合文库的标记中的Nessler 59 J.Org.Chem.4723；在组合文库中的Baldwin.117 J.Amer.Chem.Soc.5588。现有技术存在的问题
常规催化剂测试是在试验台上或较大的实验设备上完成的，在反应条件下进料与催化剂在这些设备上接触，一般对流出产物取样，经常对该取样进行分析，对其结果进行数据鉴别技术处理。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，但本发明可在一个装置中对多种催化剂进行扫描，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，当在其最佳自动控制的实施例中实践时，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，对例如蜂窝体或平板，或者单个承载颗粒的收集体等多样品支承物(载体)用带催化剂成分的溶液/悬浊液处理，以填充板上的孔(well)，或使网格状(cell)、点滴(spot)或小丸承载催化剂成分中的每种组分，对载体进行干燥，煅烧或进行其它必要处理以使网格、点滴或小丸中的成分稳定，然后使载体与可能反应的例如进料流或批料接触，以催化生物化学反应，该反应由蛋白质、细胞(cells)、酶、汽油、氢气和氧气、乙烯或其它可聚单体、丙烯加氧气，或CCl2F2及氢气催化。对在每个网格中发生的反应例如通过红外线温度记录法、分光光度法、电化学法、光电法、热传导法或其它方法对产物或剩余反应物的检测来测量，或通过例如经低容量管道多股进料，从每种组合物附近采样，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，以确定在每种组合物中的催化剂的相对效果。在形成网格、点滴、小丸等中可采用自动控制技术。
下面讨论这些参数：
催化剂：生物工艺学催化剂包括蛋白质、细胞、酶等等。化学转换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，这些候选对于特定反应的潜能还没有被认识到。许多复合组合物是有用的。被负载的金属和金属复合物是优选的。化学催化剂可以作为元素、有机或无机化合物加在基体(载体)上，使元素或其氧化物沉积在基体上，该有机或无机化合物在稳定步骤的温度下分解，或作为稳定的化合物加在基体上。
载体：载体可以是惰性粘土、沸石、陶瓷、碳、如活性塑料类的塑料、稳定的非活性金属或上述的组合物。它们的形状可以是被孔道、颗粒(小丸)穿过的多孔蜂窝体，也可以是平板，在平板上候选催化剂的碎片(点滴)沉积在平板内的孔中。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内，优选通过吸管或吸垫(类似橡皮垫)或丝网。在优选实施方案中，沉积过程可在自动控制下进行，就象过去在生物化学测试中在多孔板上装填催化剂一样。催化剂的许多点滴可通过分别沉积而得到，如穿过蜂窝体的孔道可在其长度的三分之一处塞住，在孔道的三分之一上方充满催化剂溶液，然后柱塞移到孔道的三分之二处，吸管吸入第二种催化剂，然后去除柱塞，加入第三种催化剂溶液，结果在孔道中反应物连续与流经孔道的三种催化剂接触。催化剂可通过离子交换，固体沉积、注入或这些结合来加入。优选利用组合化学或生物制备技术以制备本发明的候选催化剂系。两种或两种以上的催化剂的共沉淀可混合，加在载体上，需要时激活。催化剂可用丝网筛选到载体板上或载体孔道的内部，相继的筛选可用于把不同的催化剂组合物加到不同点滴上。
稳定步骤：一旦使催化剂定在载体上，本领域公知的任何合适的技术可用于稳定和/或激活选择的特定的催化剂，以便使它们在反应阶段保持定位。优其优选在适当位置上进行的煅烧、蒸发、熔化、干燥，沉积和反应。
反应物：本发明对在催化剂存在的情况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、还原及任何其它常规反应，这些均从催化剂中获益。在石油炼制中烃类转换反应是本发明的一个重要的应用，包括重整、液体催化裂化、氢化、加氢裂化、加氢处理、氢化脱硫，烷基化和汽油加氢处理。
传感器：用于在候选催化剂中探测催化剂行为的传感器并没有严格的限制，但是优选简单实用。特别优选采用色谱仪、温度传感器和光谱仪，尤其是那些适于例如通过多股投料、多次处理、采样、光纤或激光技术来测量靠近每种特定的催化剂点滴的温度和/或产物的仪器。特别优选采用通过红外摄象机同时在多个催化剂位置记录温度的温度记录器。其它合适的传感器包括电化学传感器、荧光检测器、NMR、NIR、FTNIR、Raman、火焰电离检测器、热传导检测器、质谱、粘度检测器和模拟电子或X-线发射检测器。传感器可检测气体或液体流或载体表面上的产物。在最好的催化剂下吸热反应使温度降低。一些传感器使用附加的检测试剂如臭氧来产生化学发光(cheimiluminesce)。
标记：标记(label)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。这些常规的标记在文献中已经讨论过了。标记可以是化学品，这些化学品在反应条件下是稳定的或可以是带有特征放射的放射性的。带标记的组合化学技术和使用选择的催化剂的组合化学技术都可应用于通过催化剂得到加强的特定反应。
分批或连续：当本发明优选在流动的基础上时，即在反应条件下反应物通过催化剂点滴流动时，可使用例如在搅动的高压罐或搅拌的容器内的分批测试，特别是在生物反应中。
温度、压力、空间速度和其它反应条件：这些条件由反应物和反应来确定。通过把载体放入一种特定反应容器中，该反应容器具有用于由传感装置观察的蓝色窗口或类似的窗口或沿反应器壁有耐压铝封，从而可将高压作为反应条件。发明的利用
本发明可用于生物工艺的催化剂的测试，用于促进气相或液相反应，这些用途应用在分批或优选连续物料流的条件下，在高压、低压或常压条件下；本发明节省了用于改进催化剂以促进需要的反应而进行筛选所耗的时间和劳动。
附图简介
图1是优选的蜂窝载体的示意图，该载体带有使不同催化剂成分的组合物沉积在每个蜂窝载体的孔道上的自动吸管装置，然后煅烧该载体使在每个孔道中的催化剂稳定。
图2是示意地示出了通过与流经孔道中的反应物接触的图1中的蜂窝载体。
图3a和3b为图2中蜂窝载体的一个孔道的可替代的示意图，该孔道带有一个用于检测产物通过孔道的检测器，该检测器通过测量直接经过产物或经孔道的激光束的吸收来进行检测。
图4a示意地示出了在接纳催化剂溶液之前中间塞住的孔道，以及图4b示出了移到孔道的末端的柱塞，于是形成了在一半长度具有一种催化剂，在另一半长度中具有另外催化剂。
图5大致示出了载体板，在板上有15个不同催化剂混合物沉积其上的点滴，这些将在实施例1中讨论。
图6a示出了在反应器中的一个位置的载体的颗粒(小丸)的阵列，该阵列是在不同小丸(在图中小丸上大致用不同标记示出)与不同催化剂组合物进行离子交换后的状态。图6b示出了组合反应器，该反应器不是优选的，因为上游可见新鲜的进料，而下游小丸可见为部分反应的进料。
优选实施方案说明
                       实施例1
参见图1,α型氧化铝板10的片(sheet)通过标准的方法刷涂上多孔的γ型氧化铝的颗粒。在聚苯乙烯制成的24孔微量滴定(microtiter)盘的孔中制备12种不同的过渡金属的草酸盐溶液。将Beckman Biomek 2000自动控制的自动液体处理系统用于从仍然在微量滴定盘的孔中的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的表面的确定位置12(点滴)处沉积所得的每种溶液的20微升试样。该载体10于是干燥、煅烧，然后插入到可在100到350摄氏度之间进行温度控制的反应器之中。在还原后，可能反应的氧气和氢气的混合物进入反应器中。Agema红外传感摄象机14用于借助磨光的金属镜通过透红外的蓝色窗来观察氧化铝载体。调节摄象机，使动态范围的下限与在进料温度之下的大约40摄氏度的温度相应，最大值信号与大约200度以上的温度相对应。催化反应的组合物通过提高(对于吸热反应则降低)该组合物第12点滴附近的局部温度显示出来，如图片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，其中红外线温度记录在照射停止后立即进行，或者通过在照射源上使用窄通带(short pass)的滤光器以减少对红外照射的污染。
                       实施例2
参见图2，多孔氧化铝整体(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孔道，该整体20在每个孔道里用不同组分的催化剂前体溶液处理，其中每种组分在各自孔道里是隔离的。在干燥，煅烧等等后，在高温下，激活的整体与流动的可能反应的混合物接触，并用Agema摄象机在红外线中观察到。反应的热函在显示催化活性的组合物附近产生局部温度差，这些作为靠近孔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20在其孔道中装有不同的催化剂组合物，将该整体安装在反应器(图中未示出)中，使每个孔道的整个长度可在反应器的一端通过蓝色窗口观察到。宽带热红外线光源安装于反应器的一端并给定表面红外线能流密度。固定AgemaIR传感摄象机以便能观察直接通过主要孔的红外线光源。将干涉仪或其它过滤器安装在摄象机和红外光源之间的反应器的一侧，以便从光源到达摄象机上的光基本上限于4到4.5微米之间的波长。在此波长范围的吸附剂的观察用于比较候选催化剂组合物，比较的基础是二氧化碳的产生和预计的反应中的不期望的副产物。找出用于低二氧化碳生成的催化剂组合物(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记录器进行测量)以便获得具有比二氧化碳副产物有更高选择性的所需产物。
                     实施例4
催化剂前体组合物的聚集体通过自动液体操纵装置进行制备，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激活之后，催化剂小丸在表面上排列，暴露于可能反应的环境，它们的活性由红外温度记录器确定。
                     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标记材料(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制品接触并被激活。小丸然后在某一时刻与可能反应的混合物接触(例如，通过沉积到封闭的体积内)以及对其活性测量(通过温度记录器，通过产物的光谱测量，或者周围气相或液相的采样)。收集显示活性的颗粒以及对标记材料的含量进行单独分析，以便确定所需催化剂活性的组合物。
                     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，因此可使未变型的整体孔洞的观察值作为一个对照光学均一性的参照标准。
                       实施例7
通过在没有反应物的情况和预定的实验温度下支持整体，在有用的波长范围绘制实施例2载体的整体小孔的放射性。以数字形式存储的放射性的图形用于使在实验条件下测量的红外能通量标准化，以提高精度，并可估算到局部的温度。
                       实施例8
较高的、基本上均一的放射性表面位于实施例2的整体的末端，远离摄象机，靠近与整体孔道材料进行散热转换/接触处。观测最靠近每个管道开口端的表面温度。在这种情况下，有必要使气体经过均一放射表面进入孔道中，可借助于小孔或借助于放射表面和整体之间的小偏移(offset)来实现。
                       实施例9
作为可选择的方案，催化剂的点滴可沉积在反应器如载体材料的所形成的圆管内表面上，并且在反应器外侧的相应点滴的温度可测量到，从而通过传导来确定各自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单独催化剂候选的活性。
                       实施例11
重复实施例4的实验，不同的是，金属填充量通过溶解小丸直接测量并直接分析该金属填充量。
                        实施例12
α型氧化铝板通过标准的方法刷上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有12种不同种过渡金属的草酸盐溶液。将Beckman Biomek 2000自动液体处理系统用于从仍然在微量滴定盘的孔中的原料制备稀释液和混合物。Biomek自动装置用于在氧化铝载体的表面的确定位置处沉积所得的每种溶液的40微升试样。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。红外传感摄象机用于通过能透过红外线的蓝色窗口观察氧化铝载体。调整摄象机使得其下限与进料温度相对应，并且最大值信号与20度以上的温度相对应。通过组合物的点滴附近的局部温度的升高而显示出组合物正催化反应。
                       实施例13
多孔氧化铝整体具有沿其整个厚度以规则阵列延伸的方形细孔，该细孔分布的密度为每平方英寸25个，对该氧化铝整体刷涂一层氧化铝颗粒涂层。然后使孔道部分充有不同组合物的溶液，每种组合物包含一种或多种金属草酸盐或硝酸盐，每种组合物隔离在其各自的孔道或孔道组中。在氢气存在下干燥和激活后，激活的整体放入装有蓝色窗口的反应器中，该反应器可使用红外传感摄象机在红外线中观察到。定位摄象机以便能观察到载体壁。每一个象素的相对放射率通过在红外线中整体的显像来确定，这时将反应器和整体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重复在红外中显像。在每个网格中的温度可通过观察靠近孔道的涂有催化剂前体的一端的网格来判断，或者通过由在非反应状态下所摄的图象计算出的放射率使观测到的红外能量放射正常化。在网格中的组合物显示在反应器温度之上的最早温度增量，这种组合物可用作氢氧化催化剂。
                     实施例14
用氧化铝颗粒刷涂多孔氧化铝整体，该多孔氧化铝整体具有沿其整个10厘米厚度以规则阵列延伸的方形孔道，其孔道的密度为每平方英寸25个。然后对孔道部分填充不同组合物的溶液，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，每种组合物隔离在各自的孔道或孔道组中。
在氢气存在下进行干燥和还原后，将激活的整体置于反应器中，该反应器可通过使用红外摄象机经过蓝色窗口来观测到。第一个窗口位于距整体的表面0.5厘米处。固定该摄象机，使得可通过窗口、通过载体的孔道和通过第二个蓝色窗口朝红外放射源来观察。
然后向反应器通入混有氧气和氩气的甲烷气，并使该气体流经朝向摄象机的整体的孔道。选择地使波长为4.3微米的红外线射线通过的光学过滤器插到红外光源和摄象机之间，其中所述的波长可被二氧化碳强烈吸收。在每个孔道中的二氧化碳的有效浓度可从在其孔道中的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光滤器所得的读数以补偿可能的光学制品，该光滤器用于4.3微米附近的红外波长，但该波长不能被二氧化碳、甲烷或水强烈地吸收。
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
催化剂的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标记材料(如根据每种组合物变化比例的硫元素的稳定同位素)。使催化剂载体颗粒与催化剂的前体的制备品接触，并被激活。然后使小丸在某一时刻与可能反应的混合物接触(例如，通过沉淀到封闭的体积内)以及测量其活性(通过温度记录器，通过产物的光谱测量，或者周围气相或液相的采样)。显示活性的颗粒被收集，并对标记材料的含量进行单独分析，然后确定给定的需要催化剂活性的组合物。
                     实施例16
制备具有以规则阵列沿其整个厚度延伸的方形孔道和密度为每平方英寸9个的聚四氟乙烯块体，使在其每个孔道的底部存在有浅洞，每个洞充有表面上带有磺酸基的不同的聚合物制剂，并安装多孔保持网格以保持聚合物样品定位。
充有催化剂的整体放入反应器中，该反应器可通过位于距块体表面0.5厘米处的窗口观测到。配置摄象机，以便可通过蓝色窗口，通过载体的孔道及通过第二窗口朝偏振光源观察，把偏振器安装在块体和摄象机之间。
向反应器供给蔗糖溶液，以便使其流过块体的孔道。通过旋转偏振片到不同的角度测量在通过每个孔道中液体的偏振光旋转的角度并观察通过每个孔道的光的亮度变化。在旋转角度变化最大的孔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，立即进行红外温度记录，或者通过在照射源上用窄通带滤光器来减少对红外线发射的污染。
                      实施例18
将溴化氰激活的交联琼脂糖颗粒的样品暴露在不同pH值、盐浓度和酶浓度的醇氧化酶的溶液中。
在酶偶联后，将激活的残基用乙醇胺急剧冷却，对颗粒进行清洗，把每种样品放置在多孔板的单独孔中。将该板暴露于含有乙醇蒸汽的流动气流中，并用Amber红外传感摄象机观察。把温度增加最多的样品选择为高活性固定醇氧化酶的催化剂。
                     实施例19
将溴化氰激活的交联琼脂糖颗粒的样品暴露在不同pH值、盐浓度和抗体浓度的抗醇氧化酶的抗体溶液中。在酶偶联后，将激活的残基用乙醇胺急剧冷却，对颗粒进行清洗，以及每种样品放置在多孔板的单独孔中。将该板暴露于含有乙醇蒸汽的流动气流中，并用Amber红外传感摄象机观察。把温度增加最多的样品选择为高活性固定醇氧化酶的催化剂。
                     实施例20
对具有穿过其整个厚度以垂直行/列的格式布置的孔道的陶瓷整体涂覆多孔的氧化铝颗粒，在每个列的所有孔道上用被激活的同一催化剂前体处理。可能反应的物流流经整体的孔道，发射的多波长的光束平行每一列穿过整体的表面，到达位于该列的末端探测器。离开那个列细孔的物流的组分通过调整检测器输出进行估计，该检测器输出包括傅立叶转换和/或在不同波长下的强度的加权累计/求差。
                     实施例21
将能催化反应物D-和L-立体异构体转换的、带有催化活性基团的小丸通过催化剂，用不同的可能择优抑制(临时或永久)该化合物的L-立体异构体转换的物质进行处理。该小丸分布在多孔盘的孔之间，并暴露于待改良的化合物的异构体的混合物中。用抑制剂进行处理的小丸(在用于L-异构体的转换活性中具有最大的还原性)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垂直行/列的格式布置的孔道的陶瓷整体刷涂多孔的氧化铝颗粒，孔道用被激活的催化剂前体处理。可能反应的物流流经整体的孔道。由孔道阵列组成的总孔道用于把含有臭氧的物流引导到通过每个孔道靠近其出口的物流中，其中所述的每一个孔道比单独孔道的尺寸小。在需要的产物中引入臭氧的反应会发出光，该光可由朝向整体的摄象机检测到。发出最强烈光的催化剂组合物是将反应物转换成臭氧活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垂直行/列的格式布置的孔道的陶瓷整体刷涂多孔的氧化铝颗粒，孔道用激活的催化剂前体处理，然后暴露于可能的减活化物质中。可能反应的物流流经整体的孔道中。由孔道阵列组成的总孔道用于对流经每个孔道内的物流进行采样，其中所述的每一个孔道比单独孔道的尺寸小。取自每个孔道的样品通过开关阀门装置依次引导到气相色谱一质谱仪中，提供所需产物最大产量的催化剂组合物可用于该反应物流的转换中。
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可用于用来说明本发明。在本说明书的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及时测试所获得的进一步的还原。优选通过沉淀或沉积法将预先形成的催化剂成分(特别是沉淀物，还有单分子和配合物如金属茂)附在/布置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，例如插入到载体每个孔道中的多个供给管道的集气管。
探测装置可包括电化学装置或γ摄象机，用于金属聚集测量；通过中子激活进行成像元素的分析及通过胶片或可发射的放射性存储板成像；通过声频高温测定、辐射热测定、电化学探测、传导探测、液相测定、优选溶解载体小丸和直接分析金属负载而进行的温度测量；测量在液相中的折射率；在没有通常的光源而替代地使用以特定波长放射的热气来直接观察产物气体的红外发射。
其它变型可包括用于在仔细对某些部位毒化候选择性测试，特别是在手性的催化剂等中。
制剂可以以点滴或层的形式负载在包含孔或孔道，或穿过载体整个范围的孔道的载体表面上。该载体可包括碳、沸石和/或塑料。该塑料可包括反应物。载体可支撑由共同沉淀物或氧化铝或颗粒制成的催化剂。
至少一种制剂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。
标记材料可包括不同同位素或同位素的不同混合物。反应条件可包括比一个巴绝对压力大的压力，并且可在比100摄氏度高的温度下接触。
该方法可包括对在相应组分的附近由于反应吸热和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。接触步骤可在化合物存在的情况下进行，该化合物可改变在多孔载体内的金属的分布。候选催化剂制剂可以点滴或层的形式在载体表面上接触，该载体含有由一底基层支持的刷涂层(washcoat)。
稳定步骤可在温度梯度下或借助其它方法实现，从而某些候选催化剂制剂暴露于不同的温度下。稳定步骤包括煅烧、蒸发、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，可以利用发射特征相对于不同化学组成而变化的较正结果。
待测试的制剂的阵列可包括预先形成的金属茂或其它附着在载体上的催化剂配合物。
红外发射可通过非散开红外光谱学的应用或红外传感照相胶片来进行探测，该探测器装置包括用于在候选制剂的阵列上进行物理扫描的装置。
在多波长中的观察可通过数学变换来完成，如转换、加权相加和/或相减等等。反应活性、反应物或产物可通过附加的反应来检测，该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器。大致上准直的发射源可用作产物检测或成像。多管采样可直接将样品引入质谱仪、色谱仪或光学监测器中。为模拟衰变等等，制剂可暴露于可使至少一种组分的活度减少10％的有毒剂，然后任选地暴露于蒸汽、热、氢气、空气、液体水或其它不同的物质或条件，这些物质或条件可使至少一种聚集物的活度比从前减少的活度增加至少10％，由此可测量再生、再活化、除焦或其它催化剂功能。有毒剂可包括高温、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 (20)

1、一种从至少两种候选制剂的聚集体中同时测试或选择催化剂制剂的方法，该催化剂制剂能对给定的反应物或反应物的混合物的转换进行催化，该方法包括：
(1)把所述制剂分别负载在一个或多个载体上；
(2)如需要使所述制剂稳定地固定在载体上；
(3)在反应条件下使负载的制剂与反应物或反应物组接触；
(4)在反应过程中和/或在分析位于各个负载制剂附近的产物或反应物的过程中，观察由各个制剂释放或吸收的热量。
2、根据权利要求1所述的方法，该方法包括在大致靠近各个负载制剂的附近采样，并分析产物或反应物制剂的样品。
3、根据权利要求1所述的方法，其中使制剂在载体的表面上以点滴或层的阵列形式接触。
4、根据权利要求1所述的方法，该方法包括使用包括硅、铬、锆和/或碳的载体。
5、根据权利要求1所述的方法，其中各个制剂可通过在载体上的不同催化剂制剂的排列位置和/或与每种制剂有物理关联的唯一标记的分析来识别。
6、根据权利要求1所述的方法，该方法还包括通过使催化剂制剂暴露于一种(或多种)物质或一种(或多种)条件来测量稳定性，其中所述的物质和条件可使至少一种制剂减少至少10％的活性，然后测量活性。
7、包括催化剂制剂的阵列的装置，包括载体装置；一组不同的制剂各自固定在所述载体上的装置，该装置适于在反应条件下与含反应物或反应物组的所述制剂接触；还包括探测装置，该装置适于在反应条件下检测在阵列中的单独制剂的相对温度或热吸收或释放。
8、根据权利要求7所述的装置，其中所述的检测装置包括红外传感摄象机装置、扫描二极管、Raman、FTIR、NMR、ESR、GC、质谱仪、GC/MS、液相色谱仪、酶、细胞、抗体、发光光谱仪、为检测或识别反应或产物的附加试剂、红外发射传感元件、热电元件、斯特林(Stirling)制冷装置和/或其它光谱装置或温度记录装置。
9、一种催化剂，该催化剂包括根据权利要求1的方法所选择制剂。
10、根据权利要求1所述的方法，该方法包括使多孔载体与金属盐的溶液接触。
11、根据权利要求8所述的装置，其中所述的检测装置包括在阵列中识别候选物的装置，所述的识别通过对电子图象的相应部分进行确定来完成。
12、根据权利要求8所述的装置，其中所述的探测装置包括电化学装置或者γ摄象机，用于金属积聚测量；通过中子激活进行图象元素分析和通过胶片或可发射的放射性存储板进行显像；通过声频高温测定、辐射热测定、电化学探测、传导探测、液相测定、优选溶解载体小丸和直接分析金属负载而进行的温度测量；测量在液相中的折射率；和/或在没有通常的光源而替代地使用以特有的波长放射的热气时直接观察产物气体的红外发射。
13、根据权利要求8所述的装置，其中所述的探测器装置包括可用作反应活度或特定化合物或化合物种类的指示器的测量化学发光的装置、准直的发射源、多管采样、质谱仪、色谱仪或光学监测器；加在离开每个候选物的物流中的一些试剂、通过染色或反应提供可探测到的产物例如光等从而使催化剂得到探测的试剂；和/或载体，该载体包括为使流动均一分布而设定的特定排列的阵列，例如插入到载体每个孔道中的多个供给管道的集气管。
14、根据权利要求1所述的方法，包括使所述制剂在温度梯度下或其它装置下稳定，从而某些候选催化剂制剂暴露于不同的温度下，进行煅烧、蒸发、干燥、反应、离子交换和/或沉淀。
15、根据权利要求1所述的方法，包括通过把制剂暴露于可使至少一种组分的活度减少至少10％的有毒剂，有毒剂可包括例如高温、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；然后暴露于蒸汽、热、氢气、空气、液体水或其它不同的物质或条件，这些物质或条件可使至少一种聚集物的活度比从前减少的活度增加至少10％，由此可测量再生、再活化、除焦或其它催化剂功能。
16、根据权利要求1所述的方法，包括检测由于反应引起的温度的变化，在该检测中利用了发射特征相对于不同化学组成而变化的较正结果。
17、根据权利要求1所述的方法，其中所述的制剂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。
18、根据权利要求1所述的方法，包括对在相应制剂的附近由于吸热和放热引起的温度变化进行检测。该方法可包括用还原剂处理。接触步骤可在化合物存在的情况下进行，该化合物可改变在多孔载体内的金属的分布。候选催化剂制剂可以点滴或层的形式在载体表面上接触，该载体含有由一底基层支持的刷涂层。
19、根据权利要求1所述的方法，包括通过数学变换进行过程观察，如转换、加权相加和/或相减等等；可通过附加的反应探测反应活度、反应物或产物，该附加的反应可发出反应物或特定化合物或化合物种类存在的信号；和/或将化学发光用作反应活度的指示器。
20、本文描述的每个发明。
CNB971920168A 1996-02-28 1997-02-25 催化剂的测定方法和装置 Expired - Fee Related CN100430725C (zh)

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CN100430725C (zh) * 1996-02-28 2008-11-05 休斯顿大学 催化剂的测定方法和装置
CN110869761A (zh) * 2017-06-02 2020-03-06 尤尼威蒂恩技术有限责任公司 确定催化剂溶液中的催化剂的催化功效相对降低的方法
CN110869761B (zh) * 2017-06-02 2023-01-31 尤尼威蒂恩技术有限责任公司 确定催化剂溶液中的催化剂的催化功效相对降低的方法
CN114113213A (zh) * 2020-08-28 2022-03-01 西门子股份公司 用于确定含碳氢化合物的燃料气体的总热值或净热值的测量装置

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US6908768B2 (en) 2005-06-21
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US6605470B1 (en) 2003-08-12
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AU1967997A (en) 1997-09-16
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US6063633A (en) 2000-05-16
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US6333196B1 (en) 2001-12-25
US6514764B1 (en) 2003-02-04

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