Fixed bed hydrolysis method for glycoside type soy bean isoflavone materials
A technology based on soybean isoflavones and glycosides, applied in organic chemistry and other fields, can solve problems such as acid wastewater environmental pollution, equipment corrosion, and application restrictions, and achieve the effects of easy industrialization, equipment corrosion, and simple process
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Embodiment 1
[0016] 1) Take 800 g of soybean germs that are pulverized and passed through a 30-mesh sieve. The total isoflavone content is 1.5%, add 600 ml of 60% ethanol aqueous solution, stir and extract, and the extraction temperature is controlled at 40° C. The first extraction time was 60 minutes, the second and third extraction times were 10 minutes respectively, and a total of three extractions were performed. Suction filtration at 40°C after each extraction is completed, combine the filtrates extracted three times, and concentrate to obtain 145.3 g of glycoside-type soybean isoflavone crude extract, the total isoflavone content of the crude extract is 7.6%, and the total isoflavone extraction rate is 92.0% .
[0017] 2) The crude extract was dissolved in 11 times the volume of 30% aqueous methanol solution to prepare a reaction solution. The size of the fixed-bed hydrolysis reactor is φ15×1030mm, and 182ml of macroporous strongly acidic cation exchange resin is filled inside. The...
Embodiment 2
[0019] 1) same as embodiment 1 step 1);
[0020] 2) The crude extract of glycosidic soybean isoflavones (total isoflavone content is 8.1%) was dissolved in 16 times the volume of 50% aqueous ethanol to prepare a reaction solution. The size of the fixed-bed hydrolysis reactor is φ30×1030mm, and 728 ml of macroporous strongly acidic cation exchange resin is filled inside. Pass the reaction solution into a fixed-bed reactor at a flow rate of 0.5ml / min for hydrolysis reaction, the temperature is controlled at 50°C, the contact time of the hydrolysis reaction is 524min, and the hydrolyzate is obtained by concentration after the reaction is completed. The hydrolysis conversion rate of total isoflavones is 90.3%, and the yield of free soybean isoflavones is 89.1%.
Embodiment 3
[0022] 1) same as embodiment 1 step 1);
[0023] 2) The crude extract of glycosidic soybean isoflavones (total isoflavone content is 8.1%) was dissolved in 16 times the volume of 50% aqueous ethanol to prepare a reaction solution. The size of the fixed-bed hydrolysis reactor is φ30×1030mm, and 728ml of dry hydrogen catalytic resin is filled inside. The reaction solution was passed into a fixed bed reactor at a flow rate of 0.5ml / min to carry out hydrolysis reaction, the temperature was controlled at 70°C, and the contact time of the hydrolysis reaction was 524min. After the reaction was completed, the product was concentrated to obtain the product. The hydrolysis conversion rate of total isoflavones is 94.2%, and the yield of free soybean isoflavones is 92.3%.
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