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    • 8. 发明授权
    • Process for continuous preparation of diester of oxalic acid
    • 连续制备草酸二酯的方法
    • US4467109A
    • 1984-08-21
    • US495460
    • 1983-05-19
    • Susumu TaharaKozo FujiiKeigo NishihiraMasaoki MatsudaKatsuhiko Mizutare
    • Susumu TaharaKozo FujiiKeigo NishihiraMasaoki MatsudaKatsuhiko Mizutare
    • C07C69/36C07C69/34
    • C07C69/36
    • There is provided a process for the continuous preparation of a diester of oxalic acid, which comprises a first step of reacting carbon monoxide with an ester of nitrous acid in the gaseous phase; a second step of condensing the gaseous reaction mixture to separate a non-condensed gas from a condensed liquid containing the diester of oxalic acid; a third step of introducing the non-condensed gas of the second step to a regeneration column, thereby contacting it with a gas containing molecular oxygen and an alcohol, and recycling the resulting gas containing an ester of nitrous acid to the reactor of the first step; a fourth step of distilling out an alcohol containing a diester of carbonic acid formed as a by-product of the first step and obtaining a liquid diester of oxalic acid; and a fifth step of introducing the distillate of the fourth step to a hydrolysis column thereby hydrolyzing the diester of carbonic acid in the gas and recycling the alcohol as an alcohol source for the third step.
    • 提供了一种用于连续制备草酸二酯的方法,其包括使一氧化碳与亚硝酸酯在气相中反应的第一步骤; 冷凝气态反应混合物以从含有草酸二酯的冷凝液分离非冷凝气体的第二步骤; 将第二步骤的非冷凝气体引入再生塔的第三步骤,由此使其与含有分子氧和醇的气体接触,并将产生的含有亚硝酸酯的气体再循环到第一步骤的反应器 ; 第四步骤,蒸馏出含有作为第一步副产物的碳酸二酯的醇,得到草酸的液体二酯; 以及第五步骤,将第四步骤的馏出物引入水解塔,由此使气体中的碳酸二酯水解并再循环醇作为第三步的醇源。
    • 9. 发明授权
    • Process for continuously preparing a diester of oxalic acid
    • 连续制备草酸二酯的方法
    • US4461909A
    • 1984-07-24
    • US495459
    • 1983-05-19
    • Susumu TaharaKozo FujiiKeigo NishihiraMasaoki MatsudaKatsuhiko Mizutare
    • Susumu TaharaKozo FujiiKeigo NishihiraMasaoki MatsudaKatsuhiko Mizutare
    • B01J23/44C07C69/36C07C69/34
    • C07C69/36
    • There is provided a process for the continuous preparation of a diester of oxalic acid which comprises a first step of reacting carbon monoxide with an ester of nitrous acid in the gaseous phase; a second step of condensing the gaseous reaction mixture to separate a non-condensed gas from a condensed liquid containing the diester of oxalic acid; a third step of introducing the non-condensed gas of the second step to a regeneration column and thereby contacting it with a gas containing molecular oxygen and an alcohol to regenerate nitrogen monoxide in the non-condensed gas into an ester of nitrous acid so as to bring the concentration of nitrogen monoxide in the gas at the outlet of the column to a level of from 2 to 7% by volume; and a fourth step of recycling the gas of the third step containing the ester of nitrous acid and from 2 to 7% by volume of nitrogen monoxide to the reactor of the first step.
    • 提供了一种用于连续制备草酸二酯的方法,该方法包括使一氧化碳与亚硝酸酯在气相中反应的第一步骤; 冷凝气态反应混合物以从含有草酸二酯的冷凝液分离非冷凝气体的第二步骤; 将第二步骤的非冷凝气体引入再生塔的第三步骤,由此使其与含有分子氧和醇的气体接触,以将非冷凝气体中的一氧化氮再生成亚硝酸酯,以便 使塔的出口处的气体中的一氧化氮浓度达到2〜7体积%的水平; 以及将含有亚硝酸酯和2〜7体积%一氧化氮的第三步骤的气体再循环到第一步骤的反应器的第四步骤。