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利用一锅法制备了Dawson型钨磷酸和钼钒磷酸,并用红外光谱和X-射线衍射表征了其结构.采用沸腾法研究了合成的杂多酸对甲基丙烯酸甲酯(MMA)的催化阻聚性能,考察了杂多酸结构、杂多酸用量和反应温度等因素对MMA本体聚合反应的影响.结果表明:钒钼元素在杂多酸催化阻聚MMA的反应中具有明显的协同作用,而且,杂多酸对MMA的催化阻聚作用随钒原子数的增加而增强,杂多酸的用量和反应温度对MMA自聚反应的速率影响较大.在过氧化苯甲酰(BPO)为0.04 g,MMA为10 mL,H9P2Mo15V3O62质量为MMA的0.06%,反应温度为101.2℃或H9P2Mo15V3O62质量为MMA的0.03%,反应温度为89.4℃时,MMA自聚反应被抑制.与传统和常用酚阻聚剂相比,Dawson型钼钒磷酸具有阻聚效果好、后处理简单、无腐蚀和污染问题等优点,能够作为MMA的阻聚剂使用.
Dawson tungstophosphoric acid and molybdovanadophosphoric acid were prepared by one-pot method, and their structures were characterized by IR and X-ray diffraction. The catalytic resistance of the synthesized heteropolyacid to methyl methacrylate (MMA) Polymerization, the effects of heteropoly acid structure, heteropoly acid dosage and reaction temperature on the polymerization of MMA were investigated.The results showed that vanadium and molybdenum had synergistic effect in the reaction of heteropolyacid catalyzed polymerization of MMA, Moreover, the catalytic polymerization of MMA with heteropoly acid increased with the increase of the number of vanadium atoms, and the amount of heteropoly acid and the reaction temperature had a great effect on the rate of MMA self-polymerization.In the presence of benzoyl peroxide (BPO) 0.04 g, MMA is 10 mL, the mass of H9P2Mo15V3O62 is 0.06% of MMA, the reaction temperature is 101.2 ℃ or the mass of H9P2Mo15V3O62 is 0.03% of MMA, the polymerization reaction of MMA is inhibited when the reaction temperature is 89.4 ℃ .Compared with traditional and common phenolic Dawson type molybdovanadophosphoric acid has the advantages of good resistance to polymerization, simple aftertreatment, non-corrosive and pollution problems, and can be used as a polymerization inhibitor for MMA.