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CN1083742A - 双功能多金属氧化物催化剂 - Google Patents

双功能多金属氧化物催化剂 Download PDF

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CN1083742A
CN1083742A CN93109023A CN93109023A CN1083742A CN 1083742 A CN1083742 A CN 1083742A CN 93109023 A CN93109023 A CN 93109023A CN 93109023 A CN93109023 A CN 93109023A CN 1083742 A CN1083742 A CN 1083742A
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周红星
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Priority to AU72624/94A priority patent/AU7262494A/en
Priority to CN94192917A priority patent/CN1075961C/zh
Priority to DE69429268T priority patent/DE69429268T2/de
Priority to PCT/CN1994/000058 priority patent/WO1995003886A1/zh
Priority to EP94922817A priority patent/EP0712660B1/en
Priority to JP7505468A priority patent/JPH09501601A/ja
Priority to US08/586,913 priority patent/US5759947A/en
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Abstract

本发明涉及一种双功能多金属氧化物催化剂，其 特点是由氧化铝和氧化硅混合成型，其配合重量比为 1∶1.5～1∶2.5，确保在氧化气氛中以1000℃～ 1600℃温度下煅烧，再在活性组分金属元素的水溶 液中浸渍，加入络合剂，再次煅烧后烘干即成。本发 明适用于石油炼制、工业废气处理、有特殊要求的气 体净化，还可适用于含有氮的氧化物和硫的氧化物气 体的处理，同时可促使氧氮化物充分还原，因而也适 用于汽油发动机排出气体的净化。此外，本发明产品 可替代贵金属作为活性组分的催化剂。

Description

本发明涉及一种双功能多金属氧化物催化剂，它用于石油炼制、工业废气处理，和有特殊要求的气体净化领域。
当今，许多国家在石油化工、化学工业、环境保护、工业废气治理等方面所涉及的化学氧化过程和化学还原过程中，普遍采用了催化技术，但所用催化剂的活性组份主要为铂、铑、钌、钇等贵金属。以复合氧化物替代贵金属作催化剂活性组份的研究工作还停留在试验阶段，未获理想的结果。
本发明的目的是要提供一种双功能多金属氧化物催化剂，它不仅可充分使一氧化碳、烷烃、烯烃、芳烃及各种有机物完全氧化，同时还可促使氮氧化物的充分还原，还可充分使氮的氧化物、硫的氧化物分解。
本发明的目的是这样实现的：它是由氧化铝和氧化硅混合成型，其配合重量比为1∶1.5～1∶2.5;确保在氧化气氛中以1000～1600℃温度下煅烧，然后取催化剂活性组份所用金属元素的硝酸盐或醋酸盐溶液处理第一次煅烧的载体;在确保还原气氛的条件下再次煅烧，再在催化剂活性组份金属元素的硝酸盐或醋酸盐溶液中浸渍，在浸渍液中加入络合剂，烘干后经活化制成产品。氧化铝和氧化硅按重量比混合后，经喷雾干燥成微球粉末状，或圆柱、圆环、球形、片状、蜂窝状。硝酸锰、硝酸钴、硝酸铈混合溶液和硝酸铜、硝酸铬、硝酸铈混合溶液等均可用作浸渍液，其配合重量比为1∶1∶0.3～0.5;混合液的摩尔浓度为1～2.5M。高温煅烧时间需两小时以上。络合剂拧檬酸加入量为金属离子总浓度的1/4～3/4。多金属氧化物的金属元素数目可以是3、4或5，但至少是2。多金属氧化物的金属元素专指具有3d亚层电子的过渡金属元素和具有4f亚层电子的镧系过渡金属元素，这些金属元素作为活性组份的存在形式是各金属元素的氧化物。
由于采用上述方案，本发明具有以下优点：
1.双功能多金属氧化物催化剂在适宜的条件下，可充分促使一氧化碳、烷烃、烯烃、芳烃及各种有机物的完全氧化，适用于石油炼制、工业废气处理、有特殊要求的气体净化。
2.双功能多金属氧化物催化剂在适宜的条件下，可充分促使氮的氧化物、硫的氧化物分解。适用于含有氮的氧化物和硫的氧化物气体的处理。
3.双功能多金属氧化物催化剂在适宜的条件下，在促使一氧化碳、碳氢化合物充分氧化的同时促使氮氧化物充分还原。特别适用于汽油发动机排出气体的净化。
4.双功能多金属氧化物催化剂在上述领域中可替代以铂、铑、钌、钇等贵金属作为活性组份的催化剂，并且较之贵金属催化剂有更完美的催化性能。
下面将通过实施例对本发明进一步详细说明。
双功能多金属氧化物催化剂活性组份的存在形式是所用的金属元素的氧化物，而不是以ABO、ABO、AB        O等复合氧化物的形式存在。
双功能多金属氧化物催化剂是一种经浸渍法制备的负载型催化剂。
该催化剂是以金属元素的氧化物作为活性组份。
金属氧化物的金属元素专指具有3d亚层电子的过渡金属元素（3d        transition        metal        sesies）和4f亚层电子的镧系过渡金属元素（inner        transition        metals）。
多金属氧化物的金属元素数目可以是3、4或5，但至少是2。
作为活性组份的金属元素依各种反应要求的不同选择最佳的组合。
活性组份金属氧化物间的摩尔比依获最佳反应结果而确定。
本催化剂的活性组份是通过浸渍法附着在催化剂载体上。
选作活性组份的金属元素，用其硝酸盐或醋酸盐水溶液配制成浸渍液。
在浸渍液中加入络合剂，可使溶液性质稳定，并且非常有利于活性组份附着在载体上的均匀性。
浸渍液中加入络合剂，是本催化剂制备工艺所采用的特有方法。其中以柠檬酸作为首选的络合剂。
浸渍工艺根据需要可采取常压浸渍或减压浸渍。
本催化剂的活性组份以金属元素氧化物的形式均匀的分布并牢固的附着在催化剂载体的外表面或催化剂载体的外表面和内表面。活性组份不是以ABO2、ABO3、AB2O4等复合氧化物的形式存在。
双功能多金属氧化物催化剂所用的载体是一种氧化铝和氧化硅按1∶1.5～1∶2.5的比例混合成型，经高温煅烧而成。
本催化剂的载体根据需要可制成微球粉末、圆柱、圆环、球形、片状、蜂窝状等形式。
本催化剂的载体制备与众不同处在于：高温煅烧时必须确保氧化气氛、经1000～1600℃温度下，不少于2小时的煅烧;然后取催化剂活性组份所用金属元素的硝酸盐或醋酸盐溶液处理第一次煅烧后的载体，在确保还原气氛的条件下再次煅烧，才获合格的载体。
载体经浸渍后，于动态下烘干。在200～800℃温度下活化，制备成最终产品。
本实例没有囊括双功能多金属氧化物催化剂的使用范围，对催化剂的制备工艺条件也不做任何限定。
实施例一：石油炼制中流化催化裂化过程再生时所用的助燃催化剂
取氢氧化铝和白土依氧化铝和氧化硅的重量比1∶1.5～1∶2.5混合;经喷雾干燥成微球粉末;依上述载体制备条件煅烧成微球粉末载体。
取硝酸锰、硝酸钴、硝酸铈溶液1∶1∶0.5的比例配成混合液，混合液的摩尔浓度为1～2.5M。往混合液中加入络合剂柠檬酸，柠檬酸的加入量为金属离子总浓度的1/4～3/4。完成上述步骤后获浸渍液。
取微球粉末载体，经常压浸渍。烘干后在200～800℃的温度下活化1～4小时，得成品助燃催化剂。
取助燃催化剂按1∶10稀释的样品，装入小型固定流化床。反应气体组成：O23%;CO 4%;其余为N2，反应温度（催化剂床层温度）300℃;空速（体积）50000hr-1的反应条件下，CO转化率100%。
实施例二：汽油发动机排出气体净化催化剂
取氢氧化铝和白土依氧化铝和氧化硅的重量比1∶1.5～1∶2.5混合;经机械挤条，切割整形成圆球状。依上述催化剂载体制备条件煅烧成球形载体。
取硝酸铜、硝酸铬、硝酸铈溶液1∶1∶0.3的比例配成混合液，混合液的摩尔浓度为1～2.5M。往混合液中加入络合剂柠檬酸，柠檬酸的加入量为金属离子总浓度的1/4～3/4。完成上述步骤后获浸渍液。
取球形载体经减压浸渍、烘干。在200～800℃的温度下活化1～4小时，得成品汽油发动机排出气体净化催化剂。
取催化剂30g，装入φ30m/m的反应器中，反应气体组成：
CO 3%、He 1500ppm、NOx500ppm、O21.5%，其余为N2。空速（体积）20000hr-1;在温度（催化剂床层温度）250℃的反应条件下：CO转化率＞95%;He转化率＞70%，NOx转化率＞70%。
取催化剂30g，装入φ30m/m的反应器中，反应气体组成：
CO 1%、He 1000ppm、NOx2000ppm、O20.6%，其余为N2。空速（体积）20000hr-1;在温度（催化剂床层温度）650℃的反应条件下：CO 转化率＞95%;He转化率＞75%，NOx转化率＞75%。

Claims (7)

1、一种双功能多金属氧化物催化剂，其特征在于它是由氧化铝和氧化硅混合成型，其配合重量比为1∶1.5～1∶2.5；确保在氧化气氛中以1000～1600℃温度下煅烧，然后取催化剂活性组份所用金属元素的硝酸盐或醋酸盐溶液处理第一次煅烧的载体；在确保还原气氛的条件下再次煅烧，再在催化剂活性组份金属元素的硝酸盐或醋酸盐溶液中浸渍，在浸渍液中加入络合剂，烘干后经活化制成产品。
2、如权利要求1所述的双功能多金属氧化物催化剂，其特征是氧化铝和氧化硅按重量比混合后，经喷雾干燥成微球粉末状，或圆柱、圆环、球形、片状、蜂窝状。
3、如权利要求1所述的双功能多金属氧化物催化剂，其特征是硝酸锰、硝酸钴、硝酸铈混合溶液和硝酸铜、硝酸铬、硝酸铈混合溶液等均可用作浸渍液，其配合重量比为1∶1∶0.3～0.5;混合液的摩尔浓度为1～2.5M。
4、如权利要求1所述的双功能多金属氧化物催化剂，其特征是高温煅烧时间需两小时以上。
5、如权利要求1所述的双功能多金属氧化物催化剂，其特征是络合剂拧檬酸加入量为金属离子总浓度的1/4～3/4。
6、如权利要求1所述的双功能多金属氧化物催化剂，其特征是多金属氧化物的金属元素数目可以是3、4或5，但至少是2。
7、如权利要求1所述的双功能多金属氧化物催化剂，其特征是多金属氧化物的金属元素专指具有3d亚层电子的过渡金属元素和具有4f亚层电子的镧系过渡金属元素，这些金属元素作为活性组份的存在形式是各金属元素的氧化物。
CN93109023A 1993-07-29 1993-07-29 双功能多金属氧化物催化剂 Pending CN1083742A (zh)

Priority Applications (8)

Application Number Priority Date Filing Date Title
CN93109023A CN1083742A (zh) 1993-07-29 1993-07-29 双功能多金属氧化物催化剂
AU72624/94A AU7262494A (en) 1993-07-29 1994-07-29 Bifunctional catalyst containing multimetal oxides
CN94192917A CN1075961C (zh) 1993-07-29 1994-07-29 双功能多金属氧化物催化剂
DE69429268T DE69429268T2 (de) 1993-07-29 1994-07-29 Multimetallhaltiger bifunktioneller katalysator
PCT/CN1994/000058 WO1995003886A1 (fr) 1993-07-29 1994-07-29 Catalyseur bifonctionnel renfermant plusieurs oxydes metalliques
EP94922817A EP0712660B1 (en) 1993-07-29 1994-07-29 Bifunctional catalyst containing multimetal oxides
JP7505468A JPH09501601A (ja) 1993-07-29 1994-07-29 複数の金属酸化物を含有する２機能型触媒
US08/586,913 US5759947A (en) 1993-07-29 1996-03-18 Bifunctional catalyst containing multimetal oxides

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US6326329B1 (en) * 1996-02-21 2001-12-04 Asec Manufacturing Highly dispersed substantially uniform mixed-metal-oxide composite supports for exhaust conversion catalysts
CN100453175C (zh) * 2004-09-30 2009-01-21 友联有机合成化学有限公司 催化剂及其制备方法以及所述催化剂在生产5H-二苯并-(b,f)-氮杂中的应用
CN101376083B (zh) * 2007-08-27 2011-10-12 中国石油化工股份有限公司 含硫化合物废气催化焚烧催化剂及制备方法
CN106466608A (zh) * 2015-08-20 2017-03-01 中国石油化工股份有限公司 一氧化碳催化还原氮氧化物的催化剂及其制备方法
CN106466608B (zh) * 2015-08-20 2020-10-16 中国石油化工股份有限公司 一氧化碳催化还原氮氧化物的催化剂及其制备方法

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JPH09501601A (ja) 1997-02-18
EP0712660A4 (en) 1997-02-04
WO1995003886A1 (fr) 1995-02-09
DE69429268D1 (de) 2002-01-10
DE69429268T2 (de) 2002-07-18
EP0712660B1 (en) 2001-11-28
EP0712660A1 (en) 1996-05-22
US5759947A (en) 1998-06-02
AU7262494A (en) 1995-02-28

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