Method for preparing 5-hydroxymethylfurfural by catalyzing through loaded type ferric phosphate
A technology of hydroxymethyl furfural and iron phosphate, applied in chemical instruments and methods, physical/chemical process catalysts, chemical recycling and other directions, can solve problems such as large environmental pollution, difficult separation, and cannot be recycled and reused, and achieves process operation steps The effect of less, easy separation and good industrial application prospects
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Embodiment 1
[0019] 2g of silica gel was placed in 10% phosphoric acid solution, under normal temperature and air atmosphere, stirred at 2000 rpm, soaked for 2 hours, added with PO 4 3- Equimolar FeCl 3 to the solution, and slowly add it to the previous solution under the condition of stirring at 1500~2500 rpm. Add an appropriate amount of sodium hydroxide solution to adjust the pH value of the solution to 7, continue to stir the solution at 2000 rpm for 3 hours, then filter the solution, collect the solids, dry them in a vacuum oven at 60°C, weigh them, and store them for later use;
Embodiment 2
[0021] Add 5ml of aqueous solution containing 5% glucose to the pressure bottle, add 0.2 g of the prepared supported iron phosphate catalyst, add 1 ml of acetone, tighten the pressure bottle, heat to 120 ° C in an oil bath, at 2000 rpm Under the condition of stirring for 1 minute, react for 60 minutes. After the reaction, the sample was naturally cooled, diluted with ultrapure water, and analyzed by high performance liquid chromatography for the content of glucose and 5-hydroxymethylfurfural. The conversion rate of glucose was calculated to be 94.02%, and the yield of 5-hydroxymethylfurfural was 43.39%.
[0022] Table 1 Glucose Conversion Preparation 5-Hydroxymethylfurfural Results
[0023] time Cellulose conversion rate 5-Hydroxymethylfurfural Yield 30 39.76% 19.83% 40 61.89% 34.48% 50 88.76% 46.77% 60 99.02% 55.39% 70 99.32% 52.31%
Embodiment 3
[0025] 2g of silica gel was placed in 10% phosphoric acid solution, under normal temperature and air atmosphere, stirred at 2000 rpm, soaked for 2 hours, added with PO 4 3- Equimolar FeCl 3 to the solution, and slowly add it to the previous solution under the condition of stirring at 1500~2500 rpm. Add an appropriate amount of sodium hydroxide solution to adjust the pH value of the solution to 7, continue to stir the solution at 2000 rpm for 3 hours, then filter the solution, collect the solids, dry them in a vacuum oven at 60°C, weigh them, and store them for later use; Add 5ml of cellulose aqueous solution to the pressure bottle, add 0.2 g of the prepared supported iron phosphate catalyst, add 1 ml of acetone, tighten the pressure bottle, heat to 120 ° C in an oil bath, and stir at 2000 rpm Under the conditions, the reaction time was 60 min. After the reaction, cool the sample naturally, dilute it with ultrapure water and analyze the content of glucose and 5-hydroxymethyl...
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