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《CIESC Journal》 2019-01
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High-efficiency catalytic synthesis of polyoxymethoxy dimethylether from sulfolane-treated sulfonic acid resin

WANG Yan;SHI Lei;FAN Jiaqi;CHEN Fei;YAO Jie;XU Guangwen;Institute of Industrial Chemistry and Energy Technology, Shenyang University of Chemical Technology;College of Applied Chemistry,Shenyang University of Chemical Technology;  
Polymethoxy dimethylether(DMM3—7) as a diesel additive can improve diesel cetane number and fuel utilization rate, and has broad application prospects. For the synthesis of DMM3—7from dimethoxymethane(DMM) and trioxymethylene(TOX), this work systematically studied the effects of different conditional parameters on the conversions and products selectivity with the sulfolane-treated sulfonic acid as the catalyst and the reaction routes were proposed according to the results of products analysis by GC-MS. It was observed that trace amounts(mg/kglevel) of H_2O left in the reaction system significantly influenced the reactants conversions and products selectivity.With raising H_2O content, more white precipitation paraformaldehyde(PF) was gradually produced, while methanolwas substantially generated to lower the selectivity of DMM3—7. The sulfolane-treated method was first proposed and sulfolane solvent was acted as dehydration and pore-forming reagent, that resulted in the absorbed H_2O in thesurface/pores of NKC-9sulfolaneobvious decrease from 2154 mg/kg to 198 mg/kg. Meanwhile, 13 X molecular sieve wasapplied to significantly reduce H_2O content of DMM from 710 mg/kg to 54 mg/kg. When the reaction temperature is313 K(40℃), the reaction is 2 h, the pressure is 1.0 MPa, and the mass ratio of DMM to TOX is 2/1, the DMM andTOX conversion rates and the DMM3-7mass selectivity increase from 48.27%, 88.41% and 45.27% to 52.91%,93.34% and 61.58%, respectively. Comparing to literatures reports, the mass selectivity to DMM3-7 was higher than60% that makes it promising for industrial applications.
【Fund】: 国家重点研发计划项目(2018YFB0604500);; 国家自然科学基金项目(21303106);; 辽宁省高等学校创新人才项目(LR2016015);; 辽宁省自然科学基金项目(2015020243);; 沈阳市科技计划项目(17-231-1-68)
【CateGory Index】: TE624.81
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