水热合成纳微尺度Co_(3)O_(4)及其催化解聚木质素磺酸钙性能研究  

Synthesis of sub-micron Co_(3)O_(4) and its catalytic performance in depolymerization of calcium lignosulfonate

作　　者：陈彦广[1,2] 关金双 邓冀童 韩洪晶 王海英[1,2] 张梅 CHEN Yan-guang;GUAN Jin-shuang;DENG Ji-tong;HAN Hong-jing;WANG Hai-ying;ZHANG Mei(School of Chemistry and Chemical Engineering,Northeast Petroleum University,Daqing 163318,China;Heilongjiang Provincial Key Laboratory of Oil and Gas Chemical Technology,Daqing 163318,China)

机构地区：[1]东北石油大学化学化工学院,黑龙江大庆163318 [2]黑龙江省石油与天然气化工省重点实验室,黑龙江大庆163318

出　　处：《现代化工》2022年第1期145-150,156,共7页Modern Chemical Industry

基　　金：国家自然科学基金(21908021);黑龙江省杰出青年基金(JC2018002)。

摘　　要：通过水热合成法制备了一系列Co_(3)O_(4)晶体,利用X射线衍射、扫描电子显微镜以及N;物理吸附仪等对合成Co_(3)O_(4)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(NO_(3))_(2)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Co_(3)O_(4)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 cm^(3)/g。当催化解聚反应温度为260℃、反应时间为5 h、m(CLS)∶m(Co_(3)O_(4))=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%)。A series of Co_(3)O_(4) 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, N_(2) physical adsorption instrument and so on.The catalytic performance of Co_(3)O_(4) 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 Co_(3)O_(4)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 cm^(3)·g^(-1).The liquid phase yield reaches 58.44% when the reaction temperature for the hydrothermal depolymerization of calcium lignosulfonate by Co_(3)O_(4)is at 260℃,the reaction lasts for 5 h, m(CLS)/m(Co_(3)O_(4))=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 木质素磺酸钙 催化解聚 酚类化合物 

分 类 号：TK6[动力工程及工程热物理—生物能]