Study On Industrial Production Technology Of KDF And α-Mangostin

This paper is divided into two parts which include the study on the industrial production of potassium diformate and the separation and extraction technology ofα-mangostin.The main results of first part are as follows:(1)The best process conditions for the synthesis of potassium diformate by using potassium carbonate and formic acid: the molar ratio of the reaction materials was 1:4.4,the reaction temperature was 70°C,the reaction time was 2.5h,and the yield of potassium diformate was 79%.(2)The mother liquor recycling process has been completed and validated,the product quality obtained by the mother liquor recycling process was reliable.(3)The pilot-scale study of the synthesis of potassium diformate and the mother liquor recycling process have been completed and validated in a one-cubic-meter reactor by using industrial grade raw materials.The product that meets the requirements can be produced through this process.The study showed that this process route was feasible.The main content of second pat are as fallows:(1)According to the results of single factor experiment,the optimum conditions for extraction and separation of α-mangostin are as follows: the extraction solvent was 90% ethanol,the ratio of solid to liquid was 1:10,the reflux extraction was 1 h,the extraction temperature was 70 °C,The number of extractions is twice.The final extraction rate was 1.93%.(2)After concentrating the extract solution and adding water into it,the product which consists of 55% α-mangostin and 10% γ-mangostin can be obtained by separating and drying the sediment which was from the extract solution.(3)Dichloromethane/petroleum ether were chosen as recrystallization solvent forα-mangostin after trying to use a variety of reagents.and the product which consists of70% α-mangostin and 5% γ-mangostin can be obtained by crystallizing once,The product of γ-mangostin has a recovery rate of 55%,after three crystallizations,the product contains 93% α-mangostin can be obtained.(4)The method of separating α-mangostin in mangosteen extract by column chromatography was explored,by using silica gel column,the mass ratio of sample to silica gel was 1:40,and the eluent was petroleum ether: ethyl acetate = 6: 1,the flow rate of the eluent was 2.5 m L/min.The product which contains 97% α-mangostin can be obtained with a yield of 81%.The standard material of α-mangostin andγ-mangostin can be obtained by preparative liquid chromatography technology.