以机械混合的Zn(OAc)2和Hβ为催化剂,碳酸二甲酯(DMC)、苯胺和甲醛溶液为原料,采用“一步”法合成了二苯甲烷二氨基甲酸甲酯(MDC)。实验结果表明,优化的反应条件是:n(DMC)/n(AN)/n(HCHO):31/1/0.15、n(Zn(OAc)2)/n(AN)=0.15、m(H8)/m(AN)=0.8,在120℃反应6h,苯胺转化率为79.8%,MDC收率为18.6%。Zn(OAc)2+Hp催化剂使用一次即失活,通过对失活催化剂表征发现其失活的原因是由于ZnO的生成所致。
Using dimethyl carbonate (DMC), aniline and formaldehyde as raw material, Zn(OAc)2+ Hβ was selected as the catalyst for the one-step synthesis of MDC. The effect of reaction conditions on catalytic performance of Zn(OAc)2 +Hβ was studied. Optimal reaction conditions were as follows: n (DMC)/n(AN)/n(HCHO)=31/1/0. 15, n(Zn(OAc)2)/n(AN)=0. 15, m(Hβ)/m(AN)=0. 8, reaction temperature was 120 ℃, reaction time was 6 h. Under these conditions, aniline conversion was 79.8 % and MDC yield was 18.6 %. Zn(OAc)2+Hβ Catalyst was deactivated after being used for only once. The cause for its deactivation was the formation of ZnO by the characterization of the deactivated Zn(OAe)2+Hβ catalyst.