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采用溶剂热的方法合成纯手性金属有机骨架[Zn2(bdc)(L-lac)(dmf)].(DMF)(Zn-BLD)化合物。研究合成温度、合成时间和合成液浓度对生成Zn-BLD晶体的产量和晶相结构的影响。结果表明:110℃为最佳合成温度;溶剂热合成12 h,生成Zn-BLD晶体产量就已达到稳定与饱和;当合成温度为110℃,反应时间为12 h,4种反应物的摩尔比为n(Zn(NO3)2.6H2O)∶n(H2BDC)∶n(L-H2lac)∶n(DMF)=6.0∶1.5∶1.5∶387时,能够得到较高结晶度的纯相Zn-BLD晶体。优化条件下合成的Zn-BLD晶体对甲基苯基亚砜具有较高的对映体选择吸附性能,其对映体过量(e.e)值达到68.2%。通过热分析仪(TGA)对Zn-BLD晶体的热稳定性进行了表征,在不高于400℃时,Zn-BLD晶体具有很好的热稳定性。
The solvothermal method was used to synthesize a pure chiral metal organic framework [Zn2 (bdc) (L-lac) (dmf)]. (DMF) (Zn-BLD) The effects of synthesis temperature, synthesis time and concentration of synthetic solution on the yield and crystal structure of Zn-BLD crystals were studied. The results showed that 110 ℃ was the optimum synthesis temperature. The yield of Zn-BLD crystal was stable and saturated after solvothermal synthesis for 12 h. When the synthesis temperature was 110 ℃ and the reaction time was 12 h, the molar ratio of the four reactants (Zn (NO3) 2.6H2O): n (H2BDC): n (L-H2lac): n (DMF) = 6.0:1.5:1.5:387, pure crystalline Zn-BLD crystals with high crystallinity can be obtained . The synthesized Zn-BLD crystals under optimized conditions have higher enantioselective adsorption properties for methylphenyl sulfoxide, with an enantiomeric excess (e.e) of 68.2%. The thermal stability of Zn-BLD crystal was characterized by thermal analysis (TGA). The Zn-BLD crystal has good thermal stability up to 400 ℃.