Compound Preparation Of Ti-pillared Interlayed Montmorillonite And Interlayered Structure Research

Titanium pillared montmorillonite (Ti-PILCs) has particular macroporous structure, excellent physical and chemical performance such as large specific area surface, high thermal stability, good catalytic activity and photosensitivity, and so on. It attracts people's great attention in recent years, and shows wide application prospect in the fields of petroleum catalysis, environment protection, industry of fine chemicals and material science, etc.In this paper, a Ca-bentonite ore from Eastern Hubei province has been used as research object to prepare Ti-PILCs, which through dispersation purification, Ti pillaring agent, Ti-PILCs synthesis and interlayer structure study.Under appropriate technical conditions, the Ca-bentonite ore from Eastern Hubei province has been beneficiated by wet sedimentation separation process with sodium pyrophosphate as modification agent, producing an ultrapure Na-montmorillonite(value of d001 1.28 nm) with fine performance, then using it for matrix, a Ti-PILC has been synthesized.Ti-PILCs were obtained with pillaring agents were prepared from TiCl4 and HCl. Ti-PILCs were also obtained with pillaring agent prepared from Ti(n-C4H9O)4 and HCl, using purified Na-montmorillonite in Hubei as the starting clay. The results shows that titanium pillared montmorillonite with the largest pore structure (d001=3.74nm) can be gained using Ti(n-C4H9O)4 as titanium resource, when Ti/clay=20 mmol/g, H/Ti=2.0 mol/mol c(HCl)=5 mol/L and at the room temperature. The largest surface area is also up to 409.1m2/g. The material mostly contains mesopores within 2 nm to 4 nm, and possesses good thermal stability.The Ti-PILCs were calcined in the next step. The results showed that calcined temperature, calcined time, calcined speed and calcined ambience affected the physical and chemical properties of the calcined Ti-PILCs. The surface area of Ti-PILCs was reduced from S60℃= 409.1 m2/g to S600℃=374.3m2/g and S900℃= 358.2m2/g, respectively, and the basal spacing was reduced from d001=3.74 nm (60℃) to d600℃=3.67nm and d900℃=3.33 nm, respectively, after being calcined. It is clear that interbedded ordered degree was rised,and pore structure had tended towards regularity, and the thermal stability is over 900℃.In this paper, the basic structures and characteristic of Ti-PILCs have been studied by using XRD, BET method, FT-IR, TG-DSC, SEM, TEM and AFM, and the porous distribution by which Ti-PILCs were formed have been discussed, and make preliminary research on its formation mechanism.Using Ti-PILCs as solid acid catalyst in preparation of diphenylethane, a Friedel-Crafts probe reaction, the productivity of diphenylethane can reach 86.33% supremely, which shows that Ti-PILCs possesses good acid catalytic performance.Some indicators of the experimental products have taken the lead in the same field.