Process for the preparation of glycols
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example 1
[0041]0.3 g of glucose (portion 1) was dissolved in 30 ml of deionised water and charged into a 60 ml autoclave equipped with a gas stirrer and hydrogen supply along with 0.5 g of a W(10.88)-Ni(3.63)-Pt(0.05) / ZrO2 catalyst and 0.5 g of a Ru(1.0) / SiO2 catalyst. The autoclave was closed, the gas phase was replaced by nitrogen, then by hydrogen and the autoclave was pressurised to 3000 kPa (absolute). The autoclave was stirred at 1450 rpm, heated to 195° C. in 12-15 minutes and kept at 195° C. and 8500 kPa (absolute) for 5 minutes. The reactor was then cooled to room temperature over 15 minutes, depressurised and opened. A liquid sample of 0.3 ml was taken for analysis. 1.0 g glucose was added (portion 2), and the procedure was repeated, with a 10 minute reaction time at 195° C. Three more lots of glucose (portions 3, 4 and 5) were added following the same procedure. Finally, portion 6, comprising 1.7 g of glucose was added and the reaction was continued for 30 minutes. The total amoun...
example 2
[0042]The procedure of Example 1 was repeated, with the difference that 0.25 g of a W(10.88)-Ni(3.63)-Pt(0.05) / ZrO2 catalyst and 0.25 g of a Ru(1.0) / SiO2 catalyst were used and portions 2 to 5 each contained 0.5 g of glucose. The total amount of glucose (portions 1 to 6) added to 30 ml water was 3 g, corresponding to a total concentration of 10 wt % glucose.
example 3
[0043]15 ml of deionised water, 0.5 g of a W(10.88)-Ni(3.63)-Pt(0.05) / ZrO2 catalyst and 0.5 g of a Ru(1.0) / SiO2 catalyst were charged into a 60 ml autoclave, equipped with a gas stirrer and hydrogen supply. The autoclave was closed, the gas phase replaced by nitrogen, then by hydrogen and the autoclave was pressurised to 3000 kPa (absolute). The autoclave was stirred at 1450 rpm, heated to 195° C. in 12-15 minutes and the pressure increased to 8500 kPa (absolute). 1.5 ml of a 40 wt % glucose solution in water was pumped into the autoclave every nine minutes at a rate of 5 ml per minute until 10 portions had been added. After the addition of the tenth portion, the autoclave was maintained for an additional 10 minutes at 195° C. The total amount of glucose added was 6 g, corresponding to a total concentration of 20 wt % glucose. The total reaction time was 100 minutes at 195° C.
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