水热合成纳微尺度Co3O4及其催化解聚木质素磺酸钙性能研究

陈彦广, 关金双, 邓冀童, 韩洪晶, 王海英, 张梅

现代化工 ›› 2022, Vol. 42 ›› Issue (1) : 145 -150,156.

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现代化工 ›› 2022, Vol. 42 ›› Issue (1) : 145-150,156. DOI: 10.16606/j.cnki.issn0253-4320.2022.01.030
科研与开发

水热合成纳微尺度Co3O4及其催化解聚木质素磺酸钙性能研究

    陈彦广, 关金双, 邓冀童, 韩洪晶, 王海英, 张梅
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Synthesis of sub-micron Co3O4 and its catalytic performance in depolymerization of calcium lignosulfonate

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摘要

通过水热合成法制备了一系列Co3O4晶体,利用X射线衍射、扫描电子显微镜以及N2物理吸附仪等对合成Co3O4产物的晶相、形貌以及孔结构参数进行表征,并对其解聚木质素磺酸钙的催化性能进行评价。结果表明,当Co(NO32为钴源、Co(Ⅱ)初始浓度为0.4 mol/L、NaOH为沉淀剂、反应体系pH为9、晶化温度为220℃、时间为12 h时,合成的Co3O4产率为82.3%,结晶度为98.47%,且晶粒呈规则的立方体结构,粒径约为80~90 nm,孔容为0.059 cm3/g。当催化解聚反应温度为260℃、反应时间为5 h、m(CLS):m(Co3O4)=2:1、体系中乙醇体积分数为40%时,液相收率高达58.44%;其中酚类化合物选择性高达55.81%(紫丁香酚类为32.37%,愈创木酚类为7.9%,苯酚类为15.54%)。

Abstract

A series of Co3O4 crystal is prepared via the hydrothermal synthesis method,and its crystal phase,morphology and pore structure are investigated via X-ray diffraction,scanning electron microscopy,N2 physical adsorption instrument and so on.The catalytic performance of Co3O4 crystal in depolymerization of calcium lignosulfonate is also studied.The optimal synthesis conditions are obtained as follows:cobalt nitrate is used as cobalt source,the initial concentration of Co(Ⅱ) is 0.4 mol·L-1,pH value of the system is regulated to 9 by NaOH,the crystallization temperature remains at 220℃ and the crystallization spends 12 h.Under these conditions,the yield of Co3O4 reaches 82.3%,and the crystallinity is 98.47%.The crystal shows regular cubic structure with a particle size of 800-900 nm.The pore volume of the obtained product is 0.059 cm3·g-1.The liquid phase yield reaches 58.44% when the reaction temperature for the hydrothermal depolymerization of calcium lignosulfonate by Co3O4 is at 260℃,the reaction lasts for 5 h,m(CLS)/m(Co3O4)=2:1,and the volume fraction of ethanol is 40%.The selectivity of phenolics reaches as high as 55.81% (32.37% for syringols,7.9% for guaiacols,and 15.54% for phenols).

关键词

四氧化三钴 / 酚类化合物 / 催化解聚 / 木质素磺酸钙

Key words

tricobalt tetroxide / phenolic compounds / catalytic depolymerization / calcium lignosulfonate

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水热合成纳微尺度Co3O4及其催化解聚木质素磺酸钙性能研究[J]. 现代化工, 2022, 42(1): 145-150,156 DOI:10.16606/j.cnki.issn0253-4320.2022.01.030

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