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小木虫: 金币+0.5, 给个红包，谢谢回帖
tangjy: 金币+5, C-EPI+1, 感谢应助！欢迎常来催化版！ 2012-03-19 12:07:49
8.9K2O:Al2O3:90SiO2:3K2SO4:27.3 H2N(CH2)8NH2:3588H2O
（1）0.176 g Al2(SO4)3 •18H2O 溶解于2 g H2O；
（2）0.40 g KOH 溶解于 2 g H2O；
（3）1.04 g 1,8-辛二胺溶解于 7.3 g H2O；
（4）3.57 g Ludox AS-40 与2.5 g 水混合，搅拌均匀；
（5）（1）与（2）混合，搅拌均匀；
（6）将（5）滴加于（3）中；
（7）将（4）缓慢滴加于（6）中，搅拌均匀，然后静置老化24 小时。
（8）转入特氟龙内胆的压力溶弹，在搅拌状态下加热至160 °C，保持72小时。反应结束后，冷却，离心分离，再用水洗涤，此过程循环5 次。将得到的白色固体在100 °C 干燥，然后转入马弗炉600 °C 灼烧10 小时除去模板剂。
(P.S: ZSM-5和Cristobalite是ZSM-22合成过程中易出现的杂晶，这是由于TON型结晶是亚稳定相，其骨架结构能量比较高，而MFI型结晶是稳定相，所以当晶化时间延长，产品会转化为MFI相)
In a Teflon beaker, 1.0 g of KOH (Kanto Chemicals) was dissolved in 4.55 g of deionized water, to which an aqueous solution of 0.44 g Al2(SO4)3 •18H2O (Wako) prepared in 4.55 g of deionized water was added, resulting in a clear solution upon thorough mixing. Among the various structure-directing agents (SDAs) that have been used for the synthesis of TON-type zeolites, 1,8-diaminooctane (Wako) was used as the SDA in the present study. Separately, 2.6 g of 1,8- diaminooctane was dissolved in 18.2 g of deionized water and added into the Teflon beaker under constant stirring using a motor-driven stirrer. The mixture was then stirred for a further 30 min to obtain a clear solution. Colloidal silica (30 wt% SiO2; Sigma-Aldrich) was used as a silica source. 11.9 g of the colloidal silica mixed with 6.74 g of deionized water was also added under stirring. The final reaction mixture was stirred for 90 min to yield the synthesis gel.
Ref: Masih, D.; Kobayashi, T.; Baba, T. Chem. Comm. 2007, 3303.
我按照这两篇文献都做出了晶相很纯的H-ZSM-22分子筛，KOH就是普通的国药集团的，一定要用Ludox AS-40 或者Ludox AS-30，在所有的滴加过程中，我一般习惯用较大的搅拌速度。老化24h后，高温水热72h的过程中，一定要保持充分的搅拌，负责很容易生成杂项。一般我得到的原粉都是粉末，没有结块。除模板剂时，时间可以适当延长，一维孔道分子筛不太容易除模板剂的，你得到黑色或者灰色可能是除模板剂不干净。 |
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