节点文献
催化加氢法提高煤制乙二醇UV值的工艺研究
Industrial Study on the UV Increase of Coal-prepared EG with Catalytic Hydrogenation
【作者】 陈波;
【导师】 张光旭;
【作者基本信息】 武汉理工大学 , 化学工程, 2014, 硕士
【摘要】 乙二醇(EG)属于一种特别重要的化工原料,主要用于制聚酯、合成纤维等。煤制乙二醇是一条具有较大潜力和较佳的生产技术路线,但在新工艺路线中受设备和原料等的影响,生产的乙二醇中引入了原石油路线所没有的杂质,这些杂质对下游产品的制备合成有很大的影响,体现产品的着色、强度和颜色等。本论文主要采用催化加氢的方法还原煤基乙二醇中的不饱和杂质,并在加氢还原后采用改性活性炭液相吸附其中的微量杂质以提高乙二醇的紫外透过率(UV)达到国家标准。研究的主要内容有:(1)通过采用不同的活性组分、不同的载体、运用不同的制备方法制备出不同的加氢催化剂,对其结构进行表征;(2)对催化剂进行活性评价,筛选出具有较高活性的加氢催化剂并优化催化剂合成条件;(3)优化催化加氢反应条件,提高煤基乙二醇的UV值;(4)由于煤基乙二醇中有部分杂质并未被还原,因此采用物理方法即活性炭吸附,对活性炭进行改性并优化吸附条件使煤基乙二醇达到国家要求。结果表明:(1)采用等体积多步浸渍法制备的NiO-γ-Al2O3,尿素调节pH值为7,Ni(NO3)2·6H2O和γ-Al2O3摩尔比为1:1,焙烧温度为600℃,焙烧6h时催化剂活性最好;(2)在催化加氢时,反应温度为90℃,反应时间为8h,氢气压力为0.3MPa,催化剂用量为乙二醇的1%,经过减压蒸馏,乙二醇在220nm、275nm、350nm处的UV值分别能达到67.5%、90.7%、99.9%;(3)在催化加氢后,对采用硝酸氧化活性炭后再对其进行在氮气保护高温密闭改性后的吸附效果最好,并在吸附温度为60℃,吸附时间70min,乙二醇与活性炭的质量比为180:1的条件下煤制乙二醇的UV值在220nm、275nm、350nm处最终能达到78.2%、94.7%、99.9%,达到生产聚酯纤维的要求。
【Abstract】 EG is an important industrial material, which can be used for the synthesis ofpolyester and synthetic fiber. However, due to the equipment and resources, the EGproduced through the new method shows a poor quality with new defects.Theproperties of EG decides the product to a large extent, like the product’s color andintensity.In the paper, the catalytic hydrogenation was used to reduce the unsaturateddefects in coal-prepared EG. After the reduction, the purification using the modifiedactivated carbon to remove the impurities was adopted to increase the UV value tomeet the national criterion.The main contents are:(1) Using different active constituent, carrier and methodto fabricate different hydrogenation catalysts and characterizing them;(2) Evaluatingthe activity of the catalysts, selecting the most active one and optimizing thepreparation conditions;(3) Optimizing the catalysis reaction to improve the UV ofEG and (4) Physically absorbing the unreduced defects using the activated carbon andoptimizing it to meet the national criterion.The results show:(1) NiO-γ-Al2O3prepared using the multi-stepimpregnation method obtained the best catalytic activity at pH of7, Ni(NO3)2·6H2Oand γ-Al2O3molar ratio of1:1, calcination temperature of600℃and calcinationtime of6h;(2) During the catalytic hydrogenation, the UV of EG under220nm,275nm and350nm reached67.5%,90.7%and99.9%, respectively at the reactiontemperature of90℃, reaction time of8h, hydrogen pressure of0.3MPa and thecatalytic dose of1%;(3) After the catalytic hydrogenation, the adsorption workedbest in sealed N2under high temperatures using nitric acid-oxidized activated carbonand the UV of EG under220nm,275nm and350nm reached78.2%,94.7%and99.9%, respectively at the adsorption temperature of60℃, adsorption time of70min and the EG and activated carbon mass ratio of180:1.
【Key words】 Making ethylene glycol from coal; UV transmittance; catalytichydrogenation; activated carbon adsorption;