煤矸石制备A型分子筛工艺条件优化研究.doc

煤矸石制备A型分子筛工艺条件优化研究.doc

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煤矸石制备A型分子筛工艺条件优化研究

煤矸石制备A型分子筛工艺条件优化研究 Optimization of Process Conditions on A Type Zeolite Preparation Using Coal Gangue as Raw Material 摘要 随着我国新的大型、特大型煤矿不断发现,煤炭能源的重要作用也受到人们越来越多的关注。但是煤炭开采过程中的主要固体废弃物,煤矸石的环境污染问题和资源利用问题也日益成为制约煤炭工业大力发展的瓶颈。利用煤矸石富含硅、铝元素,将其制备成高附加值的分子筛,代替传统低附加值产品是煤矸石研究领域中的一个重要课题。 本研究以煤矸石为原料,采用酸浸-碱熔,并通过水热合成的方法制备高结晶度A型分子筛。重点考察了煤矸石预处理阶段和分子筛制备过程中的主要工艺参数对产物的影响。考察了煤矸石制备分子筛适宜的工艺参数:煤矸石经破碎至104μm,于100℃下烘干至恒重后与33%盐酸按V固:V液=1:8比例混合均匀,于70℃下加热至干。处理后的煤矸石与2.5 mol/L氢氧化钠混合,在马弗炉中于850℃下焙烧6h,产物在水溶液中浸渍,过滤除渣,滤液中添加10g/L-15g/L硅酸钠,待形成初凝胶后,取溶胶于水热合成反应釜110℃下晶化4h,晶化产物水洗至中性后过滤干燥,即得产品A型分子筛。 对得到的分子筛产品,利用IR和TG-DSC对产物的性能进行了分析,结果表明:利用煤矸石可以获得A型分子筛特征明显的产物,该产物热稳定性良好,达到工业分子筛热稳定性要求。 关键词:煤矸石;分子筛;工艺优化;制备 Abstract For large and super large coal mine had been found constantly, the important role of coal energy had been paid more attention. But the environmental pollution and resource utilization of coal gangue, which was the main solid waste along with the coal mining, is more and more restricting the development of coal industry. For coal gangue is rich in silicon and aluminum, it was becoming an important issue on used coal gangue as raw to prepare high additional value product zeolite to replace the lowly added products. The coal gangue had been used as raw material, prepared high crystallinity A type zeolite by acid leaching, alkali fusion and hydro-thermal method. The effect of main process parameters had been researched on coal gangue pretreatment stage and zeolite synthesize stage. The process parameters of zeolite preparing had been optimized and obtained the suitable prepare conditions:coal was grind to the particle size reach 104μm, and then after was dry at 100 ℃, mix with 33% HCl in the ratio VS:VL was 1:8, heated at 70℃, after the pretreated, coal gangue was mixed with 2.5mol/L NaOH, calcinate it at 850℃ for 6h, the product was dissolve by water and filtrated to remove solid, filter liquor was added by 10g/L-15g/L Na2SiO3, after the gel had been formed, put it into Hydrothermal synthesis reactor, crystalli

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