Design Of A Supercritical Fluid Extraction,rectification,chromatography Preparation Device And Its Application

There are many problems in the traditional method of the separation of compounds.For example,the consumption of chemical reagents is huge and produce a large amount of waste chemical reagents,leading to environment pollution;At the same time,the chemical reagents are toxic side effects,easy to produce harm to human body;The chemical reagents residue in the product is unavoidable;The high temperature operation conditions for heat-sensitive biological active substances has a strong destructive,leading to the target compounds were destructed;The period of separation is very long,leading to the large cost consumption of manpower and time and so on.As a result,the compounds separation fields needs automatic,high efficiency,energy saving device to solve these problems.The supercritical fluid as a kind of safe,efficient,environmental protection and energy saving technology,having a pivotal position in compounds separation fields.This paper based on these theory to design the supercritical fluid extraction,rectification,chromatography preparation device.The device adopts the programmable logic controller?PLC?to realize the automation control of the index and real-time monitoring in the process of separation.And with soybean oil deodorizer distillate as experimental materials,by using the device to separate the nature vitamin E to verify the feasibility of this device.The device consists of automation control system and liquid road system.The Schneider M238-PLC was used for automation control system.The input part of M238-PLC collect signal from the pressure transmitter,micro controller,inverter and touch screen.Then,through the logical operation output to the corresponding module,thus for automatic control and real-time monitoring of the device parameters.Liquid road system consists of the supercritical fluid extraction,supercritical fluid rectification and supercritical fluid chromatography.These three parts were controlled through adjusting the stop valve and reversing valve to change the liquid flow direction,realizing“Trinity”.The results of separating the natural vitamin E from the soybean oil deodorizer distillate by using this device shows that:The natural vitamin E content of 6.27%of methyl esterification soybean oil deodorizer distillate dealt by supercritical fluid extraction-rectification on condition that a column temperature gradient of 40-75?,the temperature of separator 1 and separator 2respectively were 85?and 50?,the feeding rate was 1mL/min,the flow rate of CO₂ was75mL/min,the initial pressure was 16MPa,2h,the final pressure was 20MPa,4h.The content of vitamin E increased from 6.27%to 40.45%;After that,the sample was dealt by supercritical fluid chromatography on condition that the temperature of chromatography column?300-400mesh silica gel?,separator 1 and separator 2 was 40?,the system pressure was 16MPa,the flow rate of CO₂ was 100mL/min,1h later,adding 1mL/min ethanol entrainer,2h.The content of vitamin E increased from 40.45%to 95%,and the recovery rate is 98.47%.The whole separation process takes only 10h.The device can solve the problems in the traditional separation method.And it belongs to environment friendly experimental device.To sum up,the design of the supercritical fluid extraction,rectification,chromatography preparation device has realized the intelligent,automatic,efficient and rapid separation of compounds.Because the operation of the device is very simple,fast and safe,and the separation effect is good,the development of the device for the compounds of automatic separation,extraction and purification has important value and significance.