A kind of solid acid catalyst for catalyzing esterification to synthesize gallate
A solid acid catalyst, gallic acid ester technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, preparation of organic compounds, etc., to achieve high catalytic activity and selectivity, mild reaction conditions , the effect of easy operation
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Embodiment 1
[0047] Add 5g vinylimidazole and 0.02g AIBN to 50mL acetone solvent, mix and stir at 60°C for 12h, solid powder appears, add 8g 1,3-propane sultone, continue stirring for 24h, the solid product is filtered and washed with acetone for 3 and drying at 50 °C for 8 h to obtain the sulfonic acid-functionalized polyionic liquid precursor PIL-SO. 3 , the 3g PIL-SO 3 Disperse in an aqueous solution, add 17 g of 70% phytic acid (PhA) aqueous solution, stir at room temperature for 12 h, filter, wash with water three times, and dry at 60 °C for 10 h to obtain a solid acid catalyst [PIL-SO 3 ][PhA].
[0048] For the solid acid catalyst prepared in this example [PIL-SO 3 ][PhA] was characterized by TG and FT-IR,figure 1 for [PIL-SO 3 ][PhA], it can be seen that the thermal stability of the solid acid catalyst is as high as 350 °C. From the FT-IR plot ( figure 2 ), it can be seen that in the wavenumber range of 1000-1200 cm -1 There is a strong characteristic absorption peak of the s...
Embodiment 2
[0050] Add 5g vinylpyridine and 0.02g AIBN to 50mL acetone solvent, mix and stir at 60°C for 12h, solid powder appears, add 8g 1,3-propane sultone, continue stirring for 24h, the solid product is filtered and washed with acetone for 3 and drying at 50 °C for 8 h to obtain the sulfonic acid-functionalized polyionic liquid precursor PIL-SO. 3 , the 3g PIL-SO 3 Disperse in an aqueous solution, add 17 g of 70% phytic acid (PhA) aqueous solution, stir at room temperature for 12 h, filter, wash with water three times, and dry at 60° C. for 10 h to obtain a pyridyl solid acid catalyst.
Embodiment 3
[0052] 30 mL of cyclohexane, 0.05 mmol of gallic acid, 0.1 mmol of propanol, 50 mg of the catalyst prepared in Example 1 [PIL-SO 3 ][PhA] was added to a round-bottomed flask, and the reaction was stirred at 60 °C for 4 h to obtain a mixture containing propyl gallate.
[0053] The calculation of the yield and selectivity of the product is based on the gas chromatographic detection chart and calculated by the area normalization method. Through gas chromatography analysis, the yield of propyl gallate in this example was 95%, and the selectivity was 100%.
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