Ce-β/MCM-41催化苯甲醚乙酰化反应

Catalytic Acetylation of Anisole with Ce-β/MCM-41

通过β沸石的碱溶解得到沸石结构碎片和结构单元,然后将这些结构碎片和单元在模板剂CTAB的作用下自组装形成β/MCM-41复合分子筛,并考察了NaOH浓度、CTAB质量分数对β/MCM-41的影响。当NaOH浓度1.5mol/L、CTAB质量分数10%时,能够制备出长程有序性较好的β/MCM-41复合分子筛。随后制备了稀土金属Ce骨架掺杂的Ce-β/MCM-41复合分子筛,并考察Ce掺杂量(m(Ce)/m(β)=0.03、0.08)对Ce-β/MCM-41的影响,当m(Ce)/m(β)=0.03时,所制备0.03-Ce-β/MCM-41的长程有序性较好。以0.03-Ce-β/MCM-41为催化剂,在固定床上考察乙酰化反应工艺条件对p-MOAP收率的影响。正交试验结果表明,当反应物流量65 mL/h、体积空速6.5h^(-1)、反应温度140℃和n(AA)/n(AN)=6.0时,p-MOAP的4.0h收率可达58.6%。

With CTAB as template,theβ/MCM-41 micro-mesoporous composite molecular sieve has been synthesized by selfassembly of the zeolite structure fragments and the structural units obtained by alkali-treatedβzeolite,and the effects of the alkali solution concentration,CTAB dosage in the synthesis process ofβ/MCM-41 was investigated.The β/MCM-41 composite molecular sieve with well long-range order can be synthesized under the optimum conditions：The solution concentration of NaOH is 1.5 mol/L and the mass fraction of CTAB is 10%.Then the Ce-β/MCM-41 composite molecular sieve doped skeleton with rare earth metal Ce was synthesized and the effect of Ce doping amount（Ce/β=0.03,0.08）on Ce-β/MCM-41 was investigated.The result shows that the 0.03-Ce-β/MCM-41 had a well long-range order.The effect of acetylation reaction conditions on the yield of p-MOAP was investigated by using 0.03-Ce-β/MCM-41 as a catalyst in a fixed bed.The single-factor experiments showes that the 4.0 hp-MOAP yield is 58.6% under the conditions：The velocity of the reactants flow is 65 mL/h,the LHSV is 6.5 h^（-1）,reaction temperature is 140 ℃ and n（AN）/n（AA）=6.0.