Supplementary information

Catalysis effect and conversion process of transition metal chloride in the synthesis of diethyl carbonate from ethyl carbamate and ethanol

Wenbo Zhao*, Jiejing Nong,Guobiao Cao, Xiangting Liu, Zhuang Tang, Yuan Chen

Faculty of Chemical Engineering, Kunming University of Science and Technology, Kunming, 650500, China

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Fig. S1. XRD patterns of ammine TMC prepared by reaction of TMC and ammonia and their standard patterns from ISCD

Fig. S2 DSC spectra of diammine TMC from the reaction of TMC in ethanol with ammonia

Fig. S3 XRD patterns of intermediate Cd(NH3)Cl2

a: from decomposition of Cd(NH3)2Cl2 at 160 °C for 2 h, vacuum; b: from reaction of EC and ethanol at 180 °C for 6 h

Fig. S4 Conversion of ZnCl2 under the different reaction condition

A: ZnCl2 ethanol solution with NH3; B: 180 °C, 6 h; C: 190 °C, 12 h; D: 210 °C, 12 h

Figure S5. FTIR spectrum of intermediate in the conversion process of NiCl2.

Fig. S6. XRD patterns of intermediate in the reaction with NiCl2 as catalyst

A: Ni(NH3) Cl2 from ISCD; B: from reaction at 180 °C for 6 h

Fig. S7. XRD patterns of thermal decomposition product of Ni(NH3)2Cl2.

A: at 220 °C for 2 h; B: at 250 °C for 2 h

Fig. S8. TG curve of thermal decomposition product of Ni(NH3)2Cl2

A: at 220 °C for 2 h; B: at 250 °C for 2 h


Table S1 Weight loss of precipitate from the reaction of TMC ethanol solution and ammonia

Entry / Name / Theory lost (%) / Experiment lost (%) / Completely decomposition temperature (°C)
1 / Mn(NH3)2Cl2 / 21.3 / 22.8 / 285
2 / Co(NH3)2Cl2 / 20.7 / 22.3 / 280
3 / Ni(NH3)2Cl2 / 20.7 / 20.9 / 300
4 / Zn(NH3)2Cl2 / 20.0 / uncertain / uncertain
5 / Cd(NH3)2Cl2 / 15.7 / 15.3 / 250