CN102245296A - 负载型钯-金催化剂及乙酸乙烯酯的制备 - Google Patents
负载型钯-金催化剂及乙酸乙烯酯的制备 Download PDFInfo
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Abstract
公开了催化剂。该催化剂包括钯、金和载体，该载体包括二氧化钛和三氧化钨。该载体优选包括75wt％至99wt％的二氧化钛和1wt％至25wt％的三氧化钨。同样公开了一种制备催化剂的方法。该方法包括使用钯化合物和金化合物浸渍载体，煅烧该浸渍的载体，然后还原该煅烧的载体。进一步公开了使用该催化剂制备乙酸乙烯酯的方法。催化剂展现了改进的催化活性和选择性。
Description
技术领域
本发明涉及负载型钯-金催化剂。更特别地，本发明涉及具有增强的催化活性和乙酰氧基化选择性的负载型钯-金催化剂。
背景技术
钯-金催化剂是已知的。它们被用于乙酰氧基化。例如，在钯-金催化剂和乙酸存在下氧化乙烯制备乙酸乙烯酯，其是聚合物工业有用的单体。乙酰氧基化通常使用负载型钯-金催化剂通过气相反应来实现。负载钯-金催化剂的方法是已知的。通常，该方法包括沉积钯和金的化合物的混合物到载体上，然后还原钯和金成为金属。
钯和金均为贵金属。因此，已经做出很多努力以增加催化活性和减少所需的催化剂的用量。例如，美国专利第6,022,823教导了在还原金属之前，煅烧浸渍了钯和金化合物的载体。该催化剂显示出改进了的活性。
工业上仍面对的一个挑战是负载型钯-金催化剂的乙酰氧基化的低选择性。由于低选择性，大量的乙烯氧化为二氧化碳。因此，增加负载型钯-金催化剂的催化活性和选择性对于工业是很重要的。
发明内容
本发明为催化剂。该催化剂包括钯和金。该催化剂负载于包括二氧化钛和三氧化钨的载体上。优选地，该载体包括75wt％至99wt％的二氧化钛和1wt％至25wt％的三氧化钨。本发明包括制备催化剂的方法。该方法包括用钯化合物和金化合物浸渍载体。煅烧浸渍的载体，然后将其还原以将钯和金化合物转变为金属。本发明还包括使用本发明的催化剂制备乙酸乙烯酯的方法。该方法包括在乙酸和催化剂存在下氧化乙烯。本发明的催化剂显著地改善了催化活性和氧的选择性以形成乙酸乙烯酯。
发明详述
本发明为催化剂。该催化剂包括钯和金，并负载于包括二氧化钛和三氧化钨的载体上。优选地，该载体包括75wt％至99wt％的二氧化钛和1wt％至25wt％的三氧化钨。更优选地，该载体包括80wt％至99wt％的二氧化钛和1wt％至20wt％的三氧化钨。最优选地，该载体包括80wt％至95wt％的二氧化钛和5wt％至20wt％的三氧化钨。特别适合的载体是那些市售的，例如Millennium Inorganic Chemicals公司的DT-52TM二氧化钛。优选地，本发明的催化剂包括0.1wt％至3wt％的钯和0.1wt％至3wt％的金，且钯同金的重量比的范围在5∶1至1∶3之间。更优选地，该催化剂包括0.5wt％至1.5wt％的钯和0.25wt％至0.75wt％的金，且钯同金的重量比的范围在2.5∶11至1∶1.5之间。
该载体使用钯化合物、金化合物和任选的碱金属或铵化合物浸渍。可使用任何适合的浸渍方法。该载体可同时地或接连地用钯化合物、金化合物和任选的碱金属或铵化合物浸渍。优选地，该浸渍在溶液中进行。适合的钯化合物包括氯化钯、氯亚钯酸钠、硝酸钯、硫酸钯，其类似物，及其混合物。适合的金化合物包括氯化金、四氯金酸，四氯金酸钠等，及其混合物。四氯金酸钠和氯化钯或氯亚钯酸钠是最常使用的。适合的碱金属或铵化合物包括碱金属或铵氢氧化物，碱金属或铵碳酸盐，碱金属或铵碳酸氢盐，碱金属或铵偏硅酸盐，其类似物，及其混合物。
浸渍载体的方法包括：首先使用碱金属或铵化合物的溶液处理载体。然后使用含有钯和金化合物的溶液浸渍该载体。另一种方法，在使用碱金属或铵化合物的溶液处理之前进行钯和金溶液的浸渍。在这个步骤中，载体的孔基本上完全被钯和金化合物的溶液所填充。典型地，这通过将溶液滴到载体上直到实现初始润湿来完成。浸渍了钯和金化合物的载体随后同碱金属或铵化合物接触。第三种方法包括在接触载体之前将碱或铵化合物同钯和金化合物混合。同载体的接触可通过将混合物滴或喷到载体上直到初始润湿或在溶液中制成该载体的淤浆来完成。
浸渍的载体优选用水清洗以去除碱金属化合物，例如在浸渍期间形成的氯化物，并在煅烧之前干燥。煅烧浸渍的载体，即在非还原气氛中在高温下加热。优选地，煅烧在这样的条件下进行，以将一部分钯和金化合物分解。更优选地，至少10％的钯和金化合物在煅烧期间分解。优选地，浸渍载体的煅烧是在约100℃至约600℃的温度范围内进行。更优选地，温度范围为100℃至300℃。最优选地，温度范围为150℃至250℃。煅烧所使用的适合的非还原气体包括惰性或氧化气体，例如氦气、氮气、氩气、氖气、氮氧化物、氧气、空气、二氧化碳，其类似物，及其混合物。优选地，煅烧在氮气、氧气或空气或其混合物的气氛下进行。
煅烧之后，浸渍的载体被还原以将钯和金化合物转变为相应的金属。还原通过在还原剂存在的条件下加热进行。适合的还原剂包括氨、一氧化碳、氢气、碳氢化合物(hydrocarbons)、烯烃、醛、醇、肼、伯胺、羧酸、羧酸盐、羧酸酯，其类似物，及其混合物。氢气、乙烯、丙烯、碱性肼和碱性甲醛是优选的还原剂，乙烯和氢气是特别优选的。还原温度可为环境温度至约600℃。优选地，还原温度的范围为300℃至600℃。更优选地，还原温度的范围为450℃至550℃。还原得到了本发明的负载催化剂。
本发明的催化剂具有很多用途。可用于，例如，部分氧化、加氢反应、羰基化反应、氨合成、选择加氢、乙酰氧基化、催化燃烧或完全氧化、三效催化(three way catalysis)、NOx去除、甲醇合成、过氧化氢合成、加氢甲酰基化、烷基化和烷基转移、氧化羰基化、烯烃与芳烃的耦合、由丙酮制备甲基异丁基酮。本发明的催化剂特别适用于乙酸乙烯酯和乙酸烯丙酯的制备。用于制备乙酸乙烯酯和乙酸烯丙酯的各种工艺是已知的。例如，美国专利第3,743,607号和第3,775,342号教导了如何使用钯-金催化剂制备乙酸乙烯酯。
为了用于制备乙酸乙烯酯和乙酸烯丙酯，该催化剂优选使用钾化合物如乙酸钾处理。钾处理可通过混合催化剂和乙酸钾溶液、过滤、并干燥处理的催化剂而完成。通常，乙酸乙烯酯可通过在乙酸和催化剂存在的条件下氧化乙烯而得到。乙酸烯丙酯可通过相似的方法，但使用丙烯替代乙烯而得到。出人意料地发现，本发明的催化剂不仅提供了高的催化活性而且具有高的乙酰氧基化的选择性。
以下实施例仅仅用于说明本发明。本领域技术人员应该理解在本发明的精神和权利要求书的范围内的许多变形。
实施例1
负载于二氧化钛-氧化钨载体上的钯-金催化剂
在700℃下煅烧载体(30克，DT-52TM，Millennium Inorganic Chemicals公司的产品，包含10wt％的三氧化钨和90wt％的二氧化钛)6小时。煅烧的载体置于具有挡板的旋转玻璃皿内，其帮助在金属浸渍期间翻转该载体。含有10.4mL水、294mg NaAuCI4(Alfa)和799mg Na2PdCI4(Alfa)的溶液置于具有磁力搅拌棒的250mL烧杯内，并搅拌2分钟以确保所有金属化合物溶解。向溶液中分3份加入813mg碳酸氢钠(Fisher的产品)，并继续搅拌3分钟直到观察不到气体形成为止。然后使用吸液管将溶液逐滴地加到载体上，同时载体以35rpm在玻璃皿中旋转。当溶液完全加入时，向烧杯中加入2mL去离子(Dl)水以冲洗烧杯壁(sides)，然后逐滴地加入到旋转的载体中。将玻璃皿置于80℃的烘箱中持续24小时之前，可旋转玻璃皿15分钟同时使用热风枪缓和地加热以促进Pd和Au结合到该载体上。此后从烘箱中取出材料，并置于过滤器中，使用2000mL的90℃的DI水冲洗以去除氯化钠。滤出液使用硝酸银测试，一直冲洗直到观察不到沉淀为止。清洗之后，浸渍的载体置于80℃的烘箱中干燥过夜。干燥之后，将催化剂置于石英管中，将石英管插入三区电炉中，在120mL/min流速下的干燥空气中加热到230℃持续3小时。3小时之后，使用氮气清洗石英管30分钟，温度增加到500℃，并在120mL/min流速下的含有5％氢气的氦气中保持3小时。在这三小时之后，引入氮气，温度降至25℃。冷却之后，负载型催化剂浸入到装有200mL的5wt％/0.5wt％的乙酸钾/氢氧化钾溶液中20分钟。20分钟之后，倒出溶液，将烧杯置于80℃的烘箱中24小时进行干燥。干燥之后，负载型催化剂置于塑料瓶中储存。
上述制备的负载型催化剂在连续的小型乙酸乙烯酯设备中测试。乙烯、乙酸蒸气和氧气通过负载型催化剂反应制备乙烯乙酸酯。反应在35至110psig的压力范围内和110至180℃的温度范围内进行。反应物向下通过催化剂床。所有的供料气使用质量流量控制器监测。乙酸通过计量泵供料。乙烯、氧气、氮气和氦气通过伴热管(heat traced tube)预先混合并供料至反应器。氧气供料来自混合钢瓶(cylinder)，由20％氧气、10％氮气、和70％氦气组成。乙酸单独地通过加热的管线供料，以确保完全汽化，并在反应器顶部同供料气体混合。流出物的压力下降，且该流出物通过伴热管送至分析系统(气相色谱法)。分析过的气流送至分离罐，作为有机废物收集。未冷凝物直接送至通风橱的排风烟道(vent stack)处。反应器浸入并被空气流化沙浴(air fluidized sand bath)加热。压力通过反应器入口的电子传感器检测。转化、选择性和回收数据通过已知量的计量的供料和反应器流出物的GC分析获得。来自氧气/氮气/氦气混合物的氮气充当内标。结果列于表1和表2中。氧气选择性是转化为乙烯乙酸酯的氧/总消耗氧的比率。
对比实施例2
常规的负载于二氧化钛上的钯-金催化剂
遵循实施例1的总体的步骤，但是使用二氧化钛(DT-51TM，Millennium Inorganic Chemicals公司的产品)。负载型的催化剂遵循实施例1的步骤用于制备乙烯乙酸酯。结果列于表1和表2中。
表1对比了本发明的负载型钯-金催化剂同常规的负载于二氧化钛上的催化剂在基本上相同的氧选择性下的催化活性。结果表明了当保持相同的(123℃)沙浴温度时，本发明的负载型催化剂的反应器内部温度高于常规的催化剂约13℃。该温度增长表明本发明的负载型催化剂的活性呈数量级地高出(an order of magnitude more reactive than)较常规的催化剂的活性。
表1
本发明的负载型催化剂同常规催化剂的催化活性的对比*
*该表中所示的数据是催化剂加入30小时之后的10小时平均值。这时，反应器内部温度保持基本恒定。
表2对比了本发明的负载型催化剂同常规的催化剂在基本上相同的催化活性下的氧选择性。通过提高常规催化剂的沙浴温度到一个程度实现了相同的催化活性，在该程度下常规催化剂显示了同本发明的催化剂相同的催化活性。结果表明本发明的负载型催化剂具有显著提高的氧选择性。
表2
本发明的负载型催化剂同常规催化剂的选择性的对比
Claims (15)
1.催化剂，包括钯、金和载体，该载体包括二氧化钛和三氧化钨。
2.权利要求1的催化剂，其中该载体包括75wt％至99wt％的二氧化钛和1wt％至25wt％的三氧化钨。
3.权利要求2的催化剂，其中该载体包括80wt％至99wt％的二氧化钛和1wt％至20wt％的三氧化钨。
4.权利要求3的催化剂，其中该载体包括80wt％至95wt％的二氧化钛和5wt％至20wt％的三氧化钨。
5.权利要求1的催化剂，其包括0.1wt％至3wt％的钯和0.1wt％至3wt％的金。
6.制备催化剂的方法，所述方法包括：
(a)用钯化合物、金化合物和任选的碱金属或铵化合物浸渍包括二氧化钛和三氧化钨的载体；
(b)煅烧该浸渍的载体；和
(c)还原该钯和金化合物为金属。
7.权利要求6的方法，其中该钯化合物选自由氯化钯、氯亚钯酸钠、硝酸钯、硫酸钯及其混合物的组成的组，和该金化合物选自由氯化金、四氯金酸，四氯金酸钠及其混合物所组成的组。
8.权利要求6的方法，其中该载体包括85wt％至95wt％的二氧化钛和5wt％至15wt％的三氧化钨。
9.权利要求6的方法，其中该煅烧是在100℃至600℃的温度范围内进行。
10.权利要求6的方法，其中该还原是在300℃至600℃的温度范围内在氢气存在下进行。
11.制备乙酸乙烯酯的方法，包括在乙酸和催化剂存在下氧化乙烯，该催化剂包括钯、金和载体，该载体包括二氧化钛和三氧化钨。
12.权利要求11的方法，其中该载体包括75wt％至99wt％的二氧化钛和1wt％至25wt％的三氧化钨。
13.权利要求11的方法，其中该载体包括80wt％至99wt％的二氧化钛和1wt％至20wt％的三氧化钨。
14.权利要求11的方法，其中该载体包括80wt％至95wt％的二氧化钛和5wt％至20wt％的三氧化钨。
15.权利要求11的方法，其中该催化剂包括0.1wt％至3wt％的钯和0.1wt％至3wt％的金。
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| US12/291628 | 2008-11-12 | ||
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| US12/291,628 US20100121100A1 (en) | 2008-11-12 | 2008-11-12 | Supported palladium-gold catalysts and preparation of vinyl acetate therewith |
| PCT/US2009/005828 WO2010056275A1 (en) | 2008-11-12 | 2009-10-27 | Supported palladium-gold catalysts and preparation of vinyl acetate therewith |
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| US8273682B2 (en) * | 2009-12-16 | 2012-09-25 | Lyondell Chemical Technology, L.P. | Preparation of palladium-gold catalyst |
| US8507720B2 (en) * | 2010-01-29 | 2013-08-13 | Lyondell Chemical Technology, L.P. | Titania-alumina supported palladium catalyst |
| US8329611B2 (en) * | 2009-12-16 | 2012-12-11 | Lyondell Chemical Technology, L,P. | Titania-containing extrudate |
| US20110306748A1 (en) * | 2010-06-11 | 2011-12-15 | Daniel Travis Shay | Titania-alumina-tungsta extrudate and its use |
-
2008
- 2008-11-12 US US12/291,628 patent/US20100121100A1/en not_active Abandoned
-
2009
- 2009-10-27 MY MYPI2011001937A patent/MY158126A/en unknown
- 2009-10-27 WO PCT/US2009/005828 patent/WO2010056275A1/en active Application Filing
- 2009-10-27 EP EP09748865.4A patent/EP2364208B1/en not_active Not-in-force
- 2009-10-27 CN CN200980145301.0A patent/CN102245296B/zh not_active Expired - Fee Related
- 2009-10-27 ES ES09748865.4T patent/ES2532401T3/es active Active
- 2009-10-27 KR KR1020117010261A patent/KR101699559B1/ko active IP Right Grant
- 2009-10-27 CA CA2742615A patent/CA2742615C/en not_active Expired - Fee Related
- 2009-10-27 BR BRPI0921892-0A patent/BRPI0921892B1/pt not_active IP Right Cessation
- 2009-10-27 SG SG2013015961A patent/SG188844A1/en unknown
- 2009-10-27 SG SG2014005334A patent/SG2014005334A/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1345256A (zh) * | 1999-03-27 | 2002-04-17 | 人造丝化学欧洲有限公司 | 乙烯和乙酸气相氧化为乙酸乙烯酯所用催化剂及其制法和用途 |
| JP2001286733A (ja) * | 2000-04-06 | 2001-10-16 | Mitsubishi Chemicals Corp | 塩素化有機化合物の分解方法および燃焼排ガスの処理方法 |
| US20070179310A1 (en) * | 2006-02-02 | 2007-08-02 | Augustine Steven M | Preparation of palladium-gold catalysts |
Also Published As
| Publication number | Publication date |
|---|---|
| SG2014005334A (en) | 2014-03-28 |
| CA2742615C (en) | 2017-01-17 |
| CN102245296B (zh) | 2014-12-24 |
| BRPI0921892B1 (pt) | 2018-04-17 |
| ES2532401T3 (es) | 2015-03-26 |
| KR101699559B1 (ko) | 2017-01-24 |
| WO2010056275A1 (en) | 2010-05-20 |
| US20100121100A1 (en) | 2010-05-13 |
| MY158126A (en) | 2016-08-30 |
| CA2742615A1 (en) | 2010-05-20 |
| KR20110089268A (ko) | 2011-08-05 |
| EP2364208A1 (en) | 2011-09-14 |
| BRPI0921892A2 (pt) | 2015-12-29 |
| SG188844A1 (en) | 2013-04-30 |
| EP2364208B1 (en) | 2015-01-14 |
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