Method for preparing levulinic acid from hexabasic sugar catalyzed and hydrolyzed by fire resistant and highly acidic resin
A strong acid resin, catalytic hydrolysis technology, applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve the problems of corrosion, large pollution, poor water resistance, etc., and achieve mild reaction conditions and high yields , to avoid the effect of difficult recycling
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Embodiment 1
[0018] In the 500mL batch type autoclave, adding concentration is 10g / L glucose aqueous solution 300mL and 35w resin 0.3g (the water content of 35w resin is 50%, the mass ratio of glucose and high temperature resistant strong acid resin (dry basis) is 20: 1), after airtight, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 2 minutes; continue to heat up to 120°C for hydrolysis for 16 hours; the hydrolyzate is cooled to obtain a hydrolyzate, and the hydrolyzate is sampled, and the sample is passed through a 0.45um microporous membrane After filtration, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The conversion rate of glucose in the hydrolyzate was 62.2%, and the molar yield of levulinic acid was 12.6%.
Embodiment 2
[0020] In the 500mL batch type autoclave, adding concentration is 20g / L glucose aqueous solution 300mL and 35w resin 0.8g (the water content of 35w resin is 50%, the mass ratio of glucose and high temperature resistant strong acid resin (dry basis) is 15: 1), after airtight, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 2 minutes; continue to heat up to 130°C for 16 hours of hydrolysis; the hydrolyzate is cooled to obtain a hydrolyzate, and the hydrolyzate is sampled, and the sample is passed through a 0.45um microporous membrane After filtration, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The conversion rate of glucose in the hydrolyzate was 65.6%, and the molar yield of levulinic acid was 15.4%.
Embodiment 3
[0022] In the 500mL intermittent autoclave, adding concentration is 40g / L glucose aqueous solution 300mL and 35w resin 2.4g (the water content of 35w resin is 50%, the mass ratio of glucose and high temperature resistant strong acid resin (dry basis) is 10: 1), after airtight, start stirring, heat up to boiling under normal pressure, open the exhaust valve for 3 minutes; continue to heat up to 140°C for hydrolysis for 16 hours; the hydrolyzate is cooled to obtain a hydrolyzate, and the hydrolyzate is sampled, and the sample is passed through a 0.45um microporous membrane After filtration, it was quantitatively analyzed by high performance liquid chromatography (HPLC). The conversion rate of glucose in the hydrolyzate was 70.2%, and the molar yield of levulinic acid was 20.2%.
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