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Synthesis of methyl glycolate by Hydrogenation of Dimethyl Oxalate over Cu-Ag/SiO_2 Catalyst

Journal of Natural Gas Chemistry 2007年第1期16卷 78-80页

作者： Baowei Wang Qian Xu Hua Song Genhui Xu School of Chemical Engineering and Technology Key Lab for Green Chemical Technology Tianjin University Tianjin 300072 China

methyl glycolate is a good solvent and can be used as feedstock for the synthesis of some important organic chemicals. Catalytic hydrogenation of dimethyl oxalate （DMO） over copper-silver catalyst supported on silica was studied. The Cu-Ag/SiO2 catalyst supported on silica sol was prepared by homogeneous deposition-precipitation of the mixture of aqueous euprammonia complex and silica sol. The proper active temperature of Cu-Ag/SiO2 catalyst for hydrogenation of DMO was 523-623 K. The most preferable reaction conditions for methyl glycolate （MG） were optimized： temperature at 468-478 K, 40-60 mesh catalyst diameter, H2/DMO ratio 40, and 1.0 h^-1 of LHSV.

关键词： dimethyl oxalate methyl glycolate ethylene glycol hydrogenation Cu-Ag/SiO2 catalyst

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Catalytic Systems Containing p-Toluenesulfonic Acid for the Coupling Reaction of Formaldehyde and methyl Formate

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Journal of Natural Gas Chemistry 2007年第3期16卷 286-292页

作者： Kebing Wang Jie Yao Yue Wang Gongying Wang Chengdu Institute of Organic Chemistry Chinese Academy of Sciences Chengdu 610041 Sichuan China Graduate School of Chinese Academy of Sciences Beijing 100039 China

The coupling reaction of formaldehyde （FA） and methyl formate （MF） to form methyl glycolate （MG） and methyl methoxy acetate （MMAc）, catalyzed by p-toluenesulfonic acid （p-TsOH） as well as assisted by different kinds of solvents or Ni-containing compounds, had been investigated. The results showed that when the reaction was carried out at 140 ℃, with a molar ratio of FA to MF of 0.65 ： 1, molar fraction of p-TsOH to total feedstock of 11.0%, and reaction time of 3 h, the yield of MG and MMAc was 31.1% and 17.1%, respectively, p-TsOH catalyzed the coupling reaction by means of the synergistic catalysis of protonic acidity and soft basicity. Adding extra solvents to the reaction system was unfavorable for the reaction. The composite catalytic system consisting of p-TsOH and NiX2 （X=Cl, Br, I） exhibited a high catalytic performance for the coupling reaction, and NiX2 acted as a promoter in the reaction, whose promotion for the catalysis increased in the following order： NiCl2〈NiBr2〈NiI2. The present system is less corrosive when compared with the previous system, in which strong inorganic liquid acids were used as catalysts.

关键词： formaldehyde methyl formate methyl glycolate methyl methoxy acetate p-toluenesulfonicacid

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Condensation reaction of formaldehyde and methyl formate catalyzed by a composite catalyst system

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Chinese Chemical Letters 2007年第7期18卷 811-813页

作者： Ke Bing Wang Gong Ying Wang Chengdu Institute of Organic Chemistry Chinese Academy of Sciences Chengdu 610041 China Graduate School of Chinese Academy of Sciences Beijing 100039 China

The condensation reaction of formaldehyde and methyl formate to form methyl glycolate and methyl methoxy acetate catalyzed by p-toluenesulfonic acid and different Lewis acid compounds has been investigated. The composite catalytic system consisting of p-toluenesulfonic acid and NiX2 （X = Cl, Br, I）, especially NiI2, exhibited a high catalytic performance for the condensation reaction, the total yield of MG and MMAc was up to 72.37%.

关键词： p-Toluenesulfonic acid Formaldehyde methyl formate methyl glycolate methyl methoxy acetate

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