CN106563458A - 生物质高压液化催化剂的制法及应用 - Google Patents
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Abstract
本发明涉及一种生物质高压液化催化剂的制法及应用，属于生物质高压液化催化剂技术领域，其特征是，采用共沉淀法制备介孔La0.6Pr0.4FeO3钙钛矿型催化剂，包括如下步骤：将硝酸镧、硝酸镨和硝酸铁按物质的量为(0.5‑0.6):(0.4‑0.5):1的摩尔比配制混合溶液，缓慢滴加氨水溶液至pH＝8‑9，共沉淀开始就加入CTAB，抽滤，沉淀物干燥后，在550‑600℃下预烧6‑8h以除去有机模板剂，然后750‑800℃煅烧3‑5h，得催化剂，其中，CTAB用量按照硝酸镧与CTAB物质的量之比为(8‑9):1。本发明的催化剂应用于生物质高压液化反应，其液化率为59.68‑64.76％，残渣率为11.62‑13.41％，酯类物质收率50.65‑56.94％。
Description
技术领域
本发明涉及一种生物质高压液化催化剂的制法及应用，属于生物质高压液化催化剂技术领域。
背景技术
生物质能源利用转化技术主要集中在经不同转化途径的生物质固化、生物质气化和液化技术的研究开发，其中生物质液化制备生物柴油、乙醇和二甲醚等，可以替代石油能源产品，有望成为车用替代燃料。生物质直接液化技术包超临界液化、常压催化液化和高温高压液化三种，而高压液化取决于温度、压力、溶剂、催化剂等因素，特别是催化剂直接影响液化产物的分布。生物质液化催化剂主要有均相催化剂和多相催化剂，均相催化剂有酸和碱催化剂。均相催化剂由于难以回收和腐蚀性强，对设备要求高而受到限制，多相催化剂有金属催化剂和分子筛等，该类催化剂易回收，但在生物质裂解过程中形成的烯烃或小分子进入催化剂内部而形成结焦而失活。钙钛矿复合氧化物具有高的结构稳定性，催化活性主要取决于B位阳离子，同时其表面的吸附氧也是催化反应中的活性物质。B位离子经过不同金属离子掺杂后，其晶格氧含量会有所增加，催化剂性能提高，对消除催化剂表面结焦具有重要意义。
发明内容
本发明一种生物质高压液化催化剂的制法和应用，本发明制备的催化剂用于生物乙醇重整制氢反应，其收率高。
本发明具体采用的技术方案是：
一种生物质高压液化催化剂的制法，其特征是，采用共沉淀法制备介孔La0.6Pr0.4FeO3钙钛矿型催化剂，包括如下步骤：
将硝酸镧、硝酸镨和硝酸铁按物质的量为(0.5-0.6):(0.4-0.5):1的摩尔比配制混合溶液，缓慢滴加氨水溶液至pH＝8-9，共沉淀开始加入CTAB，抽滤，沉淀物干燥后，在550-600℃下预烧6-8h以除去有机模板剂，然后750-800℃煅烧3-5h，得催化剂，其中，CTAB用量按照硝酸镧与CTAB物质的量之比为(8-9):1。
其中，所述的干燥温度为80-120℃。
其中，本发明所添加的有机模板剂的材质和添加量采用现有技术。
其中，本发明制备的催化剂La0.6Pr0.4FeO3的比表面积为22.64-26.13m2/g；平均孔径为21.36-30.23nm。
一种一种生物质高压液化催化剂的应用，其特征是，包括如下步骤，
1)称量10.00g经粉碎的生物质原料和1-1.5g所述La0.6Pr0.4FeO3催化剂加入到250mL不锈钢圆柱形高压反应釜内，并加入150mL蒸馏水作为液化反应介质；
2)用N2置换(连续操作2-4次)余留在高压反应釜内的空气，置换结束后，在N2气氛下将反应体系密闭，开启机械搅拌器以300-340r·min-1恒速搅拌，加热至300-350℃恒温反应时间20-30min后，冷至室温，分离油相。
其中，步骤1)的生物质原料粒径不大于0.28μm。
其中，步骤2)高压反应釜内N2气压力为0.1Mpa。
其中，液化率为59.68-64.76％，残渣率为11.62-13.41％，酯类物质收率50.65-56.94％。
与现有技术相比，本发明的有益效果在于：液化率比同类催化剂提高；产物的选择性提高，酯类物质总收率达56.94％。
具体实施方式
一、介孔La0.6Pr0.4Fe O3双钙钛矿催化剂的制备：
采用共沉淀法制备介孔La0.6Pr0.4FeO3钙钛矿型催化剂。将硝酸镧、硝酸镨和硝酸铁按物质的量为0.6:0.4:1的摩尔比配制混合溶液，缓慢滴加氨水溶液至pH＝8～9，共沉淀开始就加入定量的CTAB(硝酸镧：CTAB＝9:1)，抽滤，沉淀物在80℃下干燥，550℃预烧6h以除去有机模板剂，然后750℃煅烧3h。
二、催化剂的应用
称量10.00g经粉碎的生物质原料(粒径不大于0.28μm)和1g权利要求1所述的La0.6Pr0.4FeO3催化剂加入到250mL不锈钢圆柱形高压反应釜内，并加入150mL蒸馏水作为液化反应介质。用N2置换(连续操作3次)余留在高压反应釜内的空气，置换结束后，在N2(0.1Mpa)气氛下将反应体系密闭。开启机械搅拌器以300r·min-1恒速搅拌，加热至350℃恒温反应时间30min后，冷至室温，分离油相。
Claims (6)
1.一种生物质高压液化催化剂的制法，其特征是，采用共沉淀法制备介孔La0.6Pr0.4FeO3钙钛矿型催化剂，包括如下步骤：
将硝酸镧、硝酸镨和硝酸铁按物质的量为(0.5-0.6):(0.4-0.5):1的摩尔比配制混合溶液，缓慢滴加氨水溶液至pH＝8-9，共沉淀开始就加入CTAB，抽滤，沉淀物干燥后，在550-600℃下预烧6-8h以除去有机模板剂，然后750-800℃煅烧3-5h，得催化剂，其中，CTAB用量按照硝酸镧与CTAB物质的量之比为(8-9):1。
2.根据权利要求1所述的生物质高压液化催化剂的制法，其特征是，所述的干燥温度为80-120℃。
3.根据权利要求1所述的生物质高压液化催化剂的制法，其特征是，所述La0.6Pr0.4FeO3催化剂的比表面积为22.64-26.13m2/g；平均孔径为21.36-30.23nm。
4.一种生物质高压液化催化剂的应用，其特征是，包括如下步骤，
1)称量10.00g经粉碎的生物质原料和1-1.5g所述La0.6Pr0.4FeO3催化剂加入到250mL不锈钢圆柱形高压反应釜内，并加入150mL蒸馏水作为液化反应介质；
2)用N2置换(连续操作2-4次)余留在高压反应釜内的空气，置换结束后，在N2气氛下将反应体系密闭，开启机械搅拌器以300-340r·min-1恒速搅拌，加热至300-350℃恒温反应时间20-30min后，冷至室温，分离油相。
5.根据权利要求4所述的生物质高压液化催化剂的应用，其特征是，步骤1)的生物质原料粒径不大于0.28μm；步骤2)高压反应釜内N2气压力为0.1Mpa。
6.根据权利要求4所述的生物质高压液化催化剂的应用，其特征是，液化率为59.68-64.76％，残渣率为11.62-13.41％，酯类物质收率50.65-56.94％。
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| CN105126901A (zh) * | 2015-09-14 | 2015-12-09 | 青岛大学 | 一种应用在海藻液化反应的分子筛催化剂及其制备方法 |
| CN105797736A (zh) * | 2015-10-14 | 2016-07-27 | 北京林业大学 | 一种新型介孔钙钛矿型氧化物/二氧化硅的制备方法及其在水处理中的应用方法 |
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| CN105032437A (zh) * | 2015-06-05 | 2015-11-11 | 广东石油化工学院 | 钙钛矿型复合氧化物催化剂及其制备方法和应用 |
| CN105126901A (zh) * | 2015-09-14 | 2015-12-09 | 青岛大学 | 一种应用在海藻液化反应的分子筛催化剂及其制备方法 |
| CN105797736A (zh) * | 2015-10-14 | 2016-07-27 | 北京林业大学 | 一种新型介孔钙钛矿型氧化物/二氧化硅的制备方法及其在水处理中的应用方法 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114904507A (zh) * | 2022-06-15 | 2022-08-16 | 济南大学 | 一种用于柴油车尾气催化净化的多功能型镨氧化物纳米棒催化剂 |
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