CN114733524B - 一种利用废弃变色硅胶的甲烷干重整催化剂及其制备方法 - Google Patents
一种利用废弃变色硅胶的甲烷干重整催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 38
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Abstract
本发明公开了一种利用废弃变色硅胶的甲烷干重整催化剂及其制备方法。利用废弃硅胶为载体制成的催化剂，将固废资源化的同时能有效催化甲烷干重整反应，且变色硅胶中含有的氯化钴指示剂有助于提高催化剂的热稳定性，延长了催化剂的使用寿命，降低了催化剂的制造成本，具有较高的应用价值。
Description
技术领域
本发明涉及镍基非均相催化剂制备领域，主要集中于以硅胶颗粒为载体的催化剂及其制备方法。
背景技术
天然气是一种以甲烷为主的烃类混合物，其中甲烷的含量为83％～99％。作为当今社会最重要的一次能源之一，其具有优质、清洁、高效、低碳的特点，因此在世界能源消费结构中占据重要地位。由于甲烷也是全球气候变暖的诱因之一，直接利用对环境不利，因此如何平衡工业应用和环境保护是全人类都面对的难题。目前化学工业中对甲烷的综合利用主要包括甲烷的直接转化和间接转化为主，前者由于反应过程控制难度大，使用受到了一定程度的限制，而间接转化工艺已较为成熟，且目前仍是学术界研究的重点课题。作为间接转化工艺之一的干重整反应，可将甲烷转化为合成气(CO+H2)，同时利用了甲烷和二氧化碳两种温室气体，有效缓解了环境问题；且合成气是重要的平台化合物，是费托合成及制取工业甲醇的原料。
在甲烷干重整反应中，催化剂起着至关重要的作用。Pt等贵金属催化剂具有活性高、稳定性强、抗积碳等优点，但由于贵金属催化剂价格昂贵，使用成本过高，因此，其大规模应用受到限制。由于镍基催化剂具有与贵金属相当的活性，且价格相对便宜，适合大规模使用，因而目前相关研究主要集中在镍基催化剂上。
催化剂的载体起到支撑和分散活性组分的作用，直接影响到催化剂本身的效果。传统的甲烷干重整催化剂载体主要有氧化铝、氧化钙、氧化镁、陶瓷、二氧化硅等高熔点的物质。本发明所用的变色硅胶的主要成分即是二氧化硅。由于工业上的变色硅胶多次重复使用后只能废弃，易造成环境污染且大量浪费其中的二氧化硅资源。因此，本发明利用废弃变色硅胶作为催化剂载体，在保证催化效果的基础上，将固废重新资源化，拓宽了催化剂载体来源，在保护环境和节约成本两方面都产生积极作用。
发明内容
本发明所要解决的技术问题是：本发明旨在提供一种利用变色废弃硅胶的甲烷干重整催化剂及其制备方法，该催化剂在保持甲烷较高转化率的前提下，具有制作工艺简单，原料获取方便，实现固废利用和节约资源的特点。
为解决上述技术问题，本发明提供一种利用废弃变色硅胶的甲烷干重整催化剂，包括活性成分和载体；所述活性成分为镍，以金属质量计，占催化剂的质量百分比为1-3％；所属载体为废弃变色硅胶颗粒；镍具有催化甲烷二氧化碳重整反应的作用。
上述利用变色废弃硅胶的甲烷干重整催化剂及其制备方法，包括以下步骤：
(1)将废弃变色硅胶浸渍于镍的可溶性盐溶液中，烘干得催化剂前驱体；
(2)将催化剂前驱体焙烧得成品。
步骤(1)中，所述镍的可溶性盐为镍的醋酸盐。
步骤(1)中，所述浸渍温度为40-60℃；所述浸渍时间为2-4h。
步骤(2)中，所述焙烧温度为400-500℃；所述焙烧时间为4-6h。
本发明的催化剂经过还原后用于催化甲烷干重整反应，催化剂还原步骤具体为：在氮气氛围下以3-5℃/min的升温速率将催化剂床层缓慢升至450-500℃，切换气体为氮气和氢气混合的还原性气氛，氢气占气体总体积浓度为15-25％，恒温还原2-4h。
本发明的催化剂运行条件为：压力0.1MPa，温度600-900℃，气体体积空速750-1250h-1，CH4/CO2比值0.5-1.5，其中CH4/CO2表示CH4与CO2的体积比。
与现有技术相比，本发明的有益效果在于：本发明采用废弃变色硅胶作为催化剂载体，拓宽了催化剂载体来源，实现了废弃物资源化，且制备过程简单低廉，易实现催化剂批量生产；本发明催化剂使用的变色硅胶中含有的氯化钴指示剂有助于提高催化剂的热稳定性，延长了催化剂的使用寿命，具有较高的应用价值。
具体实施方式
以下通过实施例对本发明进一步说明。
(1)原料来源：本发明所用变色硅胶颗粒为多次重复利用后失去使用价值的废弃物；本发明所用的其余原料均由市场购得。
(2)样品制备：
实施例1
称取5g Ni(CH3COO)2·4H2O与60ml去离子水配置成溶液，另称取116g粒度为3-5mm的废弃变色硅胶颗粒浸渍于溶液中，40℃恒温浸渍4h，浸渍完成后放入烘箱中于100℃干燥12h，再转移到马弗炉中于450℃下焙烧4小时，得到含镍为1.0wt％的甲烷干重整催化剂。
实施例2
称取10g Ni(CH3COO)2·4H2O与70ml去离子水配置成溶液，另称取76.7g粒度为3-5mm的废弃变色硅胶颗粒浸渍于溶液中，50℃恒温浸渍4h，浸渍完成后放入烘箱中于100℃干燥10h，再转移到马弗炉中于400℃下焙烧5小时，得到含镍为3.0wt％的甲烷干重整催化剂。
实施例3
称取20g Ni(CH3COO)2·4H2O与80ml去离子水配置成溶液，另称取88g粒度为3-5mm的废弃变色硅胶颗粒浸渍于溶液中，55℃恒温浸渍4h，浸渍完成后放入烘箱中于100℃干燥10h，再转移到马弗炉中于500℃下焙烧4小时，得到含镍为5.0wt％的甲烷干重整催化剂。
对比实施例4
称取10g Ni(CH3COO)2·4H2O与70ml去离子水配置成溶液，另称取76.7g粒度为3-5mm的无色纯硅胶颗粒浸渍于溶液中，50℃恒温浸渍4h，浸渍完成后放入烘箱中于100℃干燥10h，再转移到马弗炉中于400℃下焙烧5小时，得到含镍为3.0wt％的甲烷干重整催化剂。
将实施例1-3制备获得的含镍甲烷干重整催化剂分别在氮气氛围下以3-5℃/min的升温速率将催化剂床层温度缓慢升至450℃，切换气体为氮气和氢气混合的还原性气氛，氢气占气体总体积浓度为15-25％，恒温还原2-4h。将还原后的催化剂继续应用于甲烷干重整反应，催化剂装填体积为50ml，反应条件为压力0.1MPa，温度900℃，气体体积空速1000h-1，CH4/CO2比值1.0，进料气组成为CH4占总体积的45％，CO2占总体积的45％，N2占总体积的10％，结果见表1。
实施例2与对比实施例4进行稳定性比较评价，还原步骤同上。将还原后的催化剂继续应用于甲烷干重整连续反应30h，催化剂装填体积为50ml，反应条件为压力0.1MPa，温度750℃，气体体积空速1000h-1，CH4/CO2比值1.0，进料气组成为CH4占总体积的45％，CO2占总体积的45％，N2占总体积的10％，结果见表2。
由实施例1、实施例2和实施例3比较可以看出，采用相同的制备步骤制备的不同镍含量的催化剂催化效果不同，实施例2的甲烷和二氧化碳转化率最高；从实施例2与对比实施例4可以看出，实施例2采用废弃变色硅胶作为载体，其中的氯化钴可有效增强催化剂的热稳定性，连续30h的甲烷干重整反应中实施例2所述方法制备出的催化剂未出现明显的失活现象。
表1样品对甲烷干重整催化效果
表2样品催化甲烷干重整稳定性效果
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (4)
1.一种利用废弃变色硅胶为载体的甲烷干重整催化剂，其特征在于，所述甲烷干重整催化剂通过将废弃变色硅胶浸渍于镍的可溶性盐溶液中，烘干得催化剂前驱体，然后将催化剂前驱体焙烧400-500℃得到甲烷干重整催化剂；所述甲烷干重整催化剂包括活性成分和载体；所述活性成分为镍，以金属质量计，占催化剂质量的百分比为1-3％；所述载体为含有氯化钴指示剂的废弃变色硅胶颗粒，所述硅胶颗粒粒径为3-5mm。
2.根据权利要求1所述的废弃变色硅胶为载体的甲烷干重整催化剂，其特征在于所述镍的可溶性盐为镍的醋酸盐。
3.根据权利要求1所述的废弃变色硅胶为载体的甲烷干重整催化剂，其特征在于，将废弃变色硅胶浸渍于镍的可溶性盐溶液的过程中浸渍温度为40-60℃；浸渍时间为2-4h。
4.根据权利要求1所述的废弃变色硅胶为载体的甲烷干重整催化剂，其特征在于，将催化剂前驱体焙烧400-500℃的过程中，焙烧时间为4-6h。
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