【作者】 史家伟；

【导师】 张秋民；

【作者基本信息】 大连理工大学 ， 能源化工， 2011， 硕士

【摘要】 油页岩残渣是油页岩在工业制油、燃烧以及发电等化工过程中产生的废料,如果直接抛弃不仅会对环境造成不必要的污染和破坏,而且是对资源的浪费。本文旨在利用油页岩残渣制备氧化铝和白炭黑,探索一种适合油页岩残渣回收利用的实验方案。实验以抚顺油页岩制油残渣为原料,先以酸溶法提取原料中的Al2O3,再通过碱溶反应将残渣中的SiO2化为Na2SiO3。考察了原料粒度、煅烧温度、煅烧时间、酸碱溶液浓度、液固比、反应温度及反应时间对油页岩残渣中Al2O3和SiO2浸出率的影响规律。结果表明,抚顺油页岩残渣最佳煅烧温度为850℃,煅烧时间为1.0h,原料粒度为0.074mm；酸溶反应最佳盐酸浓度为12%,液固比为5：1,反应温度为100℃,反应时间为1.5h；碱溶反应最佳NaOH浓度为6mol/L,液固比为5：1,反应温度为90℃,反应时间为3.0h。在上述所得最佳工艺条件下,原料中Al2O3和SiO2的浸出率分别为81.75%和80.01%。采用均相化学沉淀法由酸溶反应得到的氯化铝滤液制备氧化铝,通过单因素考察法确定最佳工艺条件如下：反应温度为55℃,铝酸钠浓度为0.4mol/L,乙酸乙酯加入与铝离子物质的量比为1.7：1,反应时间为1.5h,活性剂的剂量为总体系质量的0.3%。各项工艺指标在最佳工艺条件下时,得到中位径(d50)为0.216μm的氧化铝白色粉末。经表征研究证实所得产品是γ-Al2O3。经醋酸分离提纯后纯度可达98.7%。采用二氧化碳为潜伏酸化剂代替强酸,结合醋酸的高选择性分离方法,研究以油页岩制油残渣提取氧化铝后的滤渣为原料,低腐蚀低能耗条件下制备高品质白炭黑的工艺方法,并研究工艺条件对白炭黑产品的粒径分布影响规律。研究表明,采用碳化反应法,由残渣碱提取液硅酸钠溶液制备白炭黑的最佳工艺条件为：反应温度为50℃,硅酸钠溶液浓度为0.0274g/ml,CO2流量为20ml/min,表面活性剂聚乙二醇6000的用量为0.007g/ml,此工艺条件下得到的白炭黑粒径最小,为20-30nm,经醋酸分离提纯后的白炭黑纯度为98.4%。更多还原

【Abstract】 In the processes of oil refining industry, burning system and power generation process using oil shale will produce residue of oil shale, it will not only bring unnecessary pollution and destruction to environment, but also waste of resources if directly throw away. This paper intends to preparation alumina and silica to explor a suitable way to make good use and recycle of residue.The work take residue of Fushun oil shale as raw material, Al2O3 in material converts into AICl3 by means of acid leaching reaction at first, and then SiO2 converts into Na2SiO3 through alkali leaching reaction. Using single-factor method research influence of activation temperature, activation time, granularity of raw material, concentration of HCl and NaOH solution, liquid-solid ratio, reaction temperature and reaction period on leaching rates of Al2O3 and SiO2 were obtained. The optimum technological conditions of Al2O3 and SiO2 leaching process are as follows:the activation temperature is 850℃, the activation time is 1.0h, the granularity of raw material is 0.074mm; The optimum acid leaching conditions are listed as follows:the concentration of acid is 12%, the liquid-solid ratio is 5:1, reaction temperature is 100℃, the reaction period is 1.5h; The optimum alkaline leaching conditions are as follows:the concentration of NaOH solution is 6mol/L, the liquid-solid ratio is 5:1, the reaction temperature is 90℃, the reaction time for 3.Oh. The leaching rates of Al2O3 and SiO2 are 81.75% and 80.01% respectively.Homogeneous chemical precipitation method was used in the alumina preparation. Optimum technological conditions of alumina preparation are determined by single-factor research method. The result is as follows:the reaction goes at 55℃for 1.5h, the concentration of sodium meta aluminate is 0.4 mol/L, the dose of surfactant is 0.3% of total system quality. the purity can be effectively improved by acetic acid solution(25%) wash,γ-Al2O3 is 0.216μm(d5o), and the degree of purity is 98.7%.Using CO2 replacing strong acid as latent acidifier and combining highly selective separation method of acetic acid study, the silica was prepared from filter cake that gets from acid leaching process and the influence of preparation process on particle size of silica. The results show that optimum technological conditions of modification preparation silica are as follows:the reaction temperature is 50℃, the concentration of sodium silicate 0.027g/L, CO2 flow is 20ml/min, the dose of surfactant is 0.007g/ml of volume of total system. The white powder silica was spherical approximately, and the average particle size(d50) was 20-30nm. the product could be comparable with the relevant national standards, degree of purity is 98.4%. It provides a new way for the development and utilization of residue of oil shale,.更多还原