Process for extracting diosgenine from turmeric by catalytic hydrolysis method
A technology that catalyzes hydrolysis and diosgenin, applied in organic chemistry, steroidal compounds, etc., can solve the problems of environmental pollution, acid wastewater generation, environmental pollution, etc., and achieve the effects of easy process conditions, environmental protection, and avoidance of acid wastewater
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Embodiment 1
[0018] Fresh turmeric rhizomes are washed and crushed, decellulose and starch are processed, then the remaining solids are dried, cooled and crushed to a refined raw material with a particle size of 0.5mm, and the content of dioscin in the raw material is increased to 15-20 %. Get refined raw material 10.0g, add the Fe(NO 3 ) 3 9H 2 150ml of aqueous solution of O (concentration: 0.02M) was placed in an autoclave, and the temperature was raised to 100°C to catalyze the hydrolysis. Using water vapor as the pressurization medium, control the pressure inside the kettle to 0.5MPa, keep it for 30 minutes, then cool to room temperature, filter the reacted product, and dry the filter residue in an oven at 110°C overnight. Put the dried material with a water content of 6% into a 500ml round bottom flask, add petroleum ether (60ml×3), reflux and extract at 85°C for 240 minutes, recover petroleum ether, cool and crystallize at room temperature, filter, and cool the precipitated crysta...
Embodiment 2
[0020] Fresh turmeric rhizomes are cleaned and crushed, decellulose and starch treated, then the remaining solids are dried, cooled and crushed to a particle size of 2.0mm, and the content of dioscin in the raw material is increased to 15-20%. Take 10.0g of refined raw material, add 3.00gCuSO 4 ·5H 2 150ml of aqueous solution of O (concentration: 0.08M) was placed in an autoclave, and the temperature was raised to 150°C to catalyze the hydrolysis. Using water vapor as the pressurization medium, control the pressure inside the kettle to 0.8MPa, keep it for 60 minutes, then cool to room temperature, filter the reacted product, and dry the filter residue in an oven at 60°C overnight. Put the dried material with a water content of 9% into a 500ml round bottom flask, add petroleum ether (60ml×3), reflux and extract at 85°C for 240 minutes, recover petroleum ether, cool and crystallize at room temperature, filter, and cool the precipitated crystals Dry to obtain diosgenin 0.172g. ...
Embodiment 3
[0022] Fresh turmeric rhizomes are cleaned and crushed, decellulose and starch treated, then the remaining solids are dried, cooled and crushed to a refined raw material with a particle size of 1.0mm, and the content of dioscin in the raw material is increased to 15-20 %. Take 10.0 g of refined raw materials, add 1.75 g of bipyridine and copper chloride complex [(bpy)CuCl 2 ] of 150ml aqueous solution (concentration is 0.04M), placed in the autoclave, heated to 190 ° C to catalyze the hydrolysis. Using water vapor as the pressurization medium, control the pressure inside the kettle to 1.2MPa, keep it for 90 minutes, then cool to room temperature, filter the reacted product, and dry the filter residue in an oven at 120°C overnight. Put the dried material with a water content of 3% into a 500ml round bottom flask, add petroleum ether (60ml×3), reflux and extract at 85°C for 240 minutes, recover petroleum ether, cool and crystallize at room temperature, filter, and cool the prec...
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