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研究了微波场中T型分子筛的结晶过程。考察了微波加热体系中合成参数如合成时间、溶胶组成、反应压力和模板剂用量对分子筛晶化的影响。微波加热的主要优点是减少合成时间,无模板剂的溶胶在普通加热条件下的晶化时间需要120h,而在微波场中则仅需要20～25h。另一方面,由于微波的快速加热特性促进了稳定相钙十字沸石的生成,从而减小了次稳定相T型分子筛的结晶区间。在未添加模板剂条件时,100℃下微波水热合成T型分子筛的结晶区间为:20≤nSiO2/nAl2O3≤22和0.31≤nM2O/nSiO2≤0.33(其中M2O=Na2O+K2O,nNa/nK=3和nSiO2/nH2O=11.70)。在普通加热和微波加热合成体系中,添加模板剂均能扩大结晶区间,同时还可以进一步减少合成时间。
The crystallization process of T zeolite in microwave field was studied. The effects of synthesis parameters such as synthesis time, sol composition, reaction pressure and the amount of template on the crystallization of molecular sieve were investigated. The main advantage of microwave heating is the reduction of the synthesis time, which requires 120 h for the crystallization without heating of the template and 20-25 h for the microwave field. On the other hand, due to the rapid heating characteristics of microwaves, the formation of stable-phase calcium-phophorite is promoted, which reduces the crystallization range of T-type zeolite. Under the condition of no templating agent added, the crystallization range of T zeolites synthesized by hydrothermal synthesis at 100 ℃ is 20≤nSiO2 / nAl2O3≤22 and 0.31≤nM2O / nSiO2≤0.33 (M2O = Na2O + K2O, nNa / nK = 3 and nSiO2 / nH2O = 11.70). In general heating and microwave heating synthesis system, adding a template agent can expand the crystallization interval, but also can further reduce the synthesis time.