SO_4~(2-)改性的镧-锆双组分交联累托土固体酸催化剂的制备和表征

用镧-锆双组分交联剂交换Na基累托土中的水合钠离子,再引入SO42-作促进剂进行改性,制备了SO42-改性的镧-锆双组分交联累托土固体酸催化剂(SO42-/La-Zr-CLR)。采用XRD、TGA、DTA和IR等分析手段对催化剂进行了表征,考察了催化剂的制备条件对其催化活性的影响。实验结果表明,将La引入到Zr交联剂中,交联后得到的交联粘土热稳定性明显提高。以乙酸和正丁醇酯化反应作探针,催化剂的最佳制备条件为:交联剂中n(La)/n(Zr)=0.15,n(Zr)/m(Na-R)=3.5 mmol/g,焙烧温度600℃。在此条件下制得催化剂的乙酸转化率达到96.74％,反复再生4次后,乙酸转化率仅下降4.68％。

Preparation and Characterization of Sulfated La- Zr Pillared Rectorite Solid Acids

Sulfated La- Zr pillared rectorite solid acids,SO42- /La - Zr- CLR,were prepared by exchanging the Na + hydrate in Na - rectorite with La - Zr pillaring agent and successive introduction of SO42- as accelerator. XRD, IR, TGA and DTA techniques were used for characterization. Effects of preparation conditions on catalytic activity were investigated taking esterification of HAc with n - BuOH as probing reaction. Thermal stability of the resulted pillared clay during calcination were much improved by adding La to Zr pillaring agent. Preferable preparation conditions were: n ( La)/n (Zr) - 0.15 in pillaring agent; n (Zr)/m (Na-R) = 3.5 mmol/g; m (SO42- )/w(clay) =30% ; calcination temperature 600 ℃ , under which the conversion rate of HAc was high as 96.74% and decreased only 4.68% after 4 regeneration cycles.