ISSN 1008-5548

CN 37-1316/TU

2020年26卷  第3期
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微反应器制备镁铝尖晶石介孔材料及其性能评价

Preparation of magnesium-alumina spinel mesoporous materials in micro-reactor and evaluation of it’s properties

Doi:10.13732/j.issn.1008-5548.2020.03.001
作者:王玉军,张建辉,李孟华,王东军,贾云刚,姜伟,赵仲阳,金书含,辛颖

摘要:采用膜分散微反应器,利用共沉淀法研究镁铝尖晶石介孔材料的制备条件,考察合成条件对镁铝尖晶石纯度、晶粒尺寸、晶体相态和孔结构的影响,并成型得到Ni-Mo-MgAl2O4-γ-Al2O3催化剂;以质量分数为20%的小桐籽油为反应原料,在高温、高压加氢脱氧装置中对催化剂的加氢脱氧性能进行评价。结果表明:原料金属盐溶液浓度总和为0. 5 mol/L(其中镁、铝金属的物质的量比为1∶2)、反应pH为11、表面活性剂CTAB浓度为0. 001 mol/L、焙烧温度为1 000℃时,制备得到的镁铝尖晶石介孔材料具有较大的介孔面积和介孔体积;Ni-Mo-MgAl2O4-γ-Al2O3催化剂具有较大的比表面积和良好的机械稳定性、水热稳定性;在温度为360~390℃、压力为4. 0 MPa、空速为5. 0 h-1、氢油质量比为200的工艺条件下,加氢脱氧油的收率大于79%。

关键词:膜分散微反应器;共沉淀法;镁铝尖晶石;加氢脱氧

Abstract: The preparation conditions of magnesium-alumina spinel mesoporous materials were studied by co-precipitation method in a membrane dispersion micro-reactor.The effects of preparation conditions on purity,grain size,crystal phase and pore structure of magnesium-alumina spinel were investigated,and Ni-Mo /MgAl2O4 -γ-Al2O3 catalyst was formed; The hydrodeoxidized performance of the catalyst was evaluated in a high temperature and high pressure hydrogenation plant with 20% tung seed oil as feed.The results show that the magnesium-alumina spinel mesoporous materials with high mesoporous area and mesoporous volume are obtained under the concentration of raw material concentration 0.5 mol /L ( the ratio of Magnesium and aluminum was 1∶2) ,solution pH of 11,the concentration of CTAB 0.001 mol /L,and the calcination temperature 1 000 ℃.Ni-Mo /MgAl2O4-γ-Al2O3 catalyst has high specific surface area and good mechanical and hydrothermal stability.Under the conditions of temperature from 360 to 390 ℃,pressure 4.0 MPa,airspeed 5.0 h - 1 ,hydrogen-oil ratio 200,the yield of hydrodeoxidized oil is over 79% . 

Keywords: membrane dispersion microreactor; co-precipitation method; magnesium-alumina spinel; hydrogenation deoxidization