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sapo56分子筛的合成研究-synthesis of sapo 56 molecular sieve
摘要明,加入晶种之后,分子筛的合成时间可以进一步缩短,粒径明显变小,分子筛的形貌也发生了很大的变化。在此基础上 SAPO-56 的合成可以稳定放大至 1 L。选取典型样品进行 SEM、FT-IR、TG-DTA、NH3-TPD 表征。SEM 结果表明, 采用 TMHD 作为单一模板剂时,分子筛呈正六边形的片状结构,平均粒径为 20 μm;正丙胺部分替代模板剂之后,分子筛呈切顶六方双锥,平均粒径为 20 μm;向合成体系中加入晶种,分子筛的形貌变成了典型的六方双锥,平均粒径为 3 μm。TG-DTA 结果表明,SAPO-56 分子筛具有良好的热稳定性。NH3-TPD 结果 表明,硅铝比对分子筛的酸性影响不大,原始配比合成的分子筛酸性位主要集 中在中强酸性位,使用复合模板剂以及加晶种之后,合成的分子筛在弱酸性位 和中强酸性位都有脱附峰,这说明,复合模板剂以及加晶种合成的分子筛酸性 明显增强。关键词:SAPO-56 分子筛;水热合成;老化;复合模板剂;晶种;粒径IIAbstractIn the circumstances of our countrys shortage of oil resources, the process of methanol to olefins is the most likely one to replace the traditional oil olefin reaction route. The key issue of methanol to olefins is the selection of the catalysts. Currently, the industrialized catalysts have a poor ablity to resist coke formation, short life time and poor selectivity, so studies on catalysts are still a hot issue at home and abroad. This article selects SAPO-56 as the research object, mainly to study the synthetic rules, morphology and particle size.SAPO-56 molecular sieve was synthesized hydrothermally using N,N,N’, N’,-tetramehtyl-hexane-1, 6-diamine (TMHD) as template agent, phosphoric acid as phosphorus source, pseudo-boehmite as aluminium source, and white carbon black as silicon source. First of all, the influence of synthetic conditions on the molecular sieves was studied. By changing the amount of Si, Al, P, pure phase region of SAPO-56 appeared in the range of 0.14 n (SiO2) /n (M) 0.31, 0.32 n (Al2O3) /n(M) 0.53 and 0.26 n (P2O5) /n (M) 0.48 (M=SiO2+Al2O3+P2O5),in this area purephase of SAPO-56 can be synthesized at the condition of 200 ℃and 72 h. Then other compositions (Si, Al, P) was fixed, the effect of water and template amount on the synthesis of SAPO-56 was also investigated. The results showed that pure SAPO-56 crystal could not be synthesized when n (TMHD) /n (P2O5) 1.4.To control the crystal size of SAPO-56, we took an aging process beforehydrothermal crystalllization and studied the influence of a
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