WO2002081046A1 - A multi-functional apparatus for extracting and concentrating automatically in the dynamical-linear, non-supercritical or supercritical state with high efficiency - Google Patents

Abstract

The present invention relates to a multi-functional apparatus for extracting and concentrating automatically with high speed and high efficiency. Said apparatus can be operated in the dynamical-linear, non-supercritical or supercritical state, and during the operation of said apparatus menstruum used can be recovered automatically. This apparatus can be used in the Chinese traditional medicine, chemical engineering, food industry and the like. With said apparatus, automatic processes of extraction, concentration, separation, purification, and menstruum's recovery can be joined together into a closed circuit in order to fit the need of GMP production. Various menstruums alone or mixture of them can be used in the apparatus, and the menstruums can be recycled or auto-recovered through the system of the apparatus, among which concentration of menstruums can be auto-adjusted linearly. Extraction rate can be accelerated by using ultrasonic oscillation. Concentrating rate and menstruums' recovering rate can be increased by utilizing techniques of increasing temperature, microwave, decreasing pressure and so on, during which extracting temperature and pressure can be adjusted linearly.

Description

 Multifunctional and efficient dynamic linear double-critical automatic extraction and concentration equipment

 The invention relates to a device for quickly extracting effective components in industries such as Chinese medicine, chemical industry, food, and the like, specifically, a multifunctional high-efficiency dynamic linear double-critical automatic extraction, concentration, and automatic solvent recovery device. Background technique

 Extraction equipment is widely used in production fields such as Chinese medicine, but from the current domestic and foreign market surveys, most of the existing extraction equipment exists, with simple structure, complicated operation, high labor intensity, low extraction yield, and low degree of automation. , And poor sealing performance and other shortcomings. Because the existing equipment has a single function, extraction, concentration, and solvent recovery cannot be completed in one device. Therefore, its materials, especially solvents, cause a lot of waste and pollute the environment.

 According to Chinese patents and other relevant search data, there have been no reports of multifunctional related devices with dynamic linearity, which integrates dual-critical automatic extraction, concentration, and automatic solvent recovery.

Summary of the Invention

 The purpose of the present invention is to provide a rapid extraction of effective ingredients suitable for traditional Chinese medicine, chemical industry, food, etc., which not only realizes the integration of closed automatic extraction, concentration, separation and purification, and automatic solvent recovery to meet the requirements of GMP production, but also can be used. A variety of solvents are used for non-supercritical or supercritical extraction. The solvent can also be used in this equipment to achieve multi-functional dynamic linear double-critical automatic rapid and efficient extraction and concentration of solvents and automatic recovery.

 The purpose of the present invention is achieved as follows: an extraction tank, a fixed frame, a medium storage tank, a solvent storage tank, a supercritical condenser, an evaporator, a separator, a supercritical sedimentation separator, and a supercritical liquid storage tank , Non-supercritical solvent condensers, filters, storage tanks, ultrasonic generators, microwave generators, compressors, electric control boxes and pipes, valves, solenoid valves and other components connected between various equipment Double-critical automatic extraction and concentration device. The characteristics are: the extraction tank is fixed on the upper end of the fixed frame; the lower end of the extraction tank, the middle liquid storage tank is fixed in the middle of the fixed frame; the lower end of the middle liquid storage tank, the heat circulation pump is fixed in the middle of the other layer of the fixed frame: the fixed frame An evaporator, a microwave generator, and a supercritical gaseous filter are provided at the side end; a solvent storage tank is provided at the rear end of the fixed frame; a supercritical liquid storage tank, a supercritical condenser, and Compressor; a useful control box is set at the side of the entire equipment.

The extraction tank is a place where the soluble components in the material are dissolved after the material comes into contact with the solvent, and it is fixed on the upper end of the fixed frame; the sieve hole of the extraction tank (the material dissolved body) and the inner wall of the tank body (li Liquid layer) with ultrasonic Oscillator (to speed up the dissolution rate), heating, temperature control and liquid level counting device, the outer wall of the tank is provided with a thermal insulation layer, the top of the extraction tank is provided with a solvent channel, one end of which is directly inserted into the center of the inner liner, and the other end is a quarter tube It plays the role of spraying the solvent into the leaching and quenching material or recovering the solvent in the material residue into the storage tank at the end of the extraction; one end of the solvent channel quarter tube passes a single-pass high-sealed magnetic valve and supercritical storage liquid The output tube at the bottom of the tank is connected. The two ends are connected to the three-way electromagnetic ceramic (T3) connected to the supercritical gas filter through a single-way sealed magnetic valve. The three ends are connected to the three-way through a single-way sealed magnetic valve. The output end of the non-supercritical solvent liquid pump is connected, and the four-end end is connected to the three-way solenoid valve (T1) at the lower end of the non-supercritical condenser. The one-end end is connected to the three-way solenoid valve (T1). The solvent storage tank is connected; the other end of the three-way solenoid valve (T3) is connected to the compressor inlet; the top end of the extraction tank is provided with a material inlet hole laterally, and its hole cover is designed to withstand high pressure and airtight; the extraction tank Liquid outlet pipe at the bottom of the lower end The middle liquid storage tank fixed in the middle of the fixing frame is connected, and the pancreatic-shaped thermal circulation tube in the inner layer (ie, the drip layer) of the extraction liquid of the extraction tank is arranged at the upper end of the tank and the outlet pipe is set at the lower end of the tank. It is connected to the water (oil) heating layer of the steamer through a heat circulation pump. If necessary, a temperature-controlled heat exchange cycle can be purchased. There is no slag checking hole with a sealable switch on the lower side of the tank.

 The medium storage tank is mainly used for temporarily storing and filtering impurities for non-supercritical material leachate. The color is fixed below the extraction tank, and the upper end is connected with the three-way solenoid valve (T2) of the extraction tank liquid outlet pipe. It is connected with the three-way solenoid valve (T2). The other branched capillaries receive the supercritical material leachate from the top of the evaporator through the spray head, and the liquid outlet under the medium storage tank can regulate the non-supercritical material leachate from the evaporator through the liquid inlet pump. Inject into the middle and lower liquid inlets.

 The evaporator is used as a place for evaporating and concentrating material leaching solution, and for solvent recovery and heat exchange. The water (oil) heat exchange interlayer is installed inside. The heater is installed at the bottom of the interlayer, and the evaporator is coated with a thermal insulation layer. Holes and spray nozzles for leachate of supercritical materials; the top of the steam hole pipe is connected with a separator; the upper end of the interlayer is provided with a thermal circulation tube connected to the pancreas-shaped thermal circulation tube in the extraction tank, and the lower end of the interlayer is connected to the thermal circulation pump To form a complete thermal cycle system.

 The splitter is used as the main place for automatically adjusting the concentration ratio of non-supercritical solvent. The lower end of the splitter is connected to the steam channel of the evaporator, and the other end is connected to the non-supercritical condenser. There is a temperature control system to ensure the separation of Zizi; the Zizi device also has a Zizi liquid discharge channel.

The non-supercritical condenser is a place where non-supercritical extraction solvent vapor condenses. It is composed of a spiral-shaped water-proof high-efficiency condensing tube group. Water cooling is recycled by a cooling tower. The upper inlet channel of the condenser is connected to a three-way solenoid valve. (T1) The other end of the pipe is connected to the extraction tank; the central micro-piercing bridge is connected to the microwave generator; the middle and lower ends are provided with wide pipes to connect to the supercritical sedimentation separator, and the conical bottom is provided with a valve for extraction Material extraction holes; thermal water circulation (oil) pipes at the upper end of the water-proof (oil) heat exchange interlayer of the steamer, and return water at the lower end (Oil) pipeline.

 The supercritical sedimentation separator is used for sedimentation and separation of the extraction dust carried during the recovery of the supercritical extraction solvent gas. It is fixed outside the evaporator, and one end of the supercritical sedimentation separator is connected to the lower end of the evaporator. The upper end is provided with a lateral pipe connected to the supercritical gaseous filter.

 The supercritical gaseous filter is used as a place for filtering solvent gas during supercritical extraction. One end is connected to the supercritical settlement separator, and the other end is connected to a three-way solenoid valve (T3)-the other end. The end of the three-way solenoid valve (T3) is connected to the inlet of the compressor.

 The compressor is used as a power source for the supercritical extraction cycle and double-critical solvent recovery. The inlet end of the camel press is connected to the three-way solenoid valve (T3), and the outlet end is connected to the three-way by the magnetic wide (T4). One end of the three-way solenoid valve (T4) is connected to the pipeline, and the other end is connected to the three-way solenoid valve (T5). The three-way solenoid valve (T5) is connected to the upper end of the non-supercritical condenser. Solenoid valve (T5) The other split (super) pipe is connected to the supercritical condenser. The other end of the supercritical condenser pipe is connected to the top of the supercritical liquid storage tank through a one-way high-sealed solenoid valve. Supercritical ti! Liquid tank The lower end of the pipeline is connected to the upper end of the extraction tank via a one-way high-sealed solenoid valve.

 In the supercritical spray head, the supercritical extract liquid is atomized through its rapid decompression production, and the leachate can be deposited on the bottom of the evaporator, and the solvent production is vaporized, and the exhaust gas is arranged in the middle and lower part of the steamer. The hole enters the gas filter, and after filtering, it is returned to the compressor for repeated use.

 The non-supercritical zirconia separator has a built-in temperature control system to adjust the temperature to achieve non-supercritical extraction of the mixed solvent vapor zirconia, which can dynamically and continuously change the concentration of the quenched solvent. The condensate from the zirconia goes into the liquid storage tank through the discharge channel, and the solvent vapor (the concentration will change linearly) enters the condenser after the zirconia is separated.

 The non-supercritical condenser is composed of a double-layer water-cooled pancreas-shaped tube, which can quickly condense the solvent vapor into the solvent liquid, and regularly control the return to the extraction tank for continuous linear gradient cycle extraction or solvent recovery through the pipeline and the solenoid valve. Storage tank; compressor, during supercritical extraction, it is the driving force of the extraction cycle, while continuously compressing the solvent gas into the condenser, condensing into a supercritical liquid phase solvent, supplying it to the extraction tank, and also absorbing evaporation from the evaporator to restore the gaseous phase. Solvent; At the end of any critical extraction, it can help to efficiently recover the solvent from the leachate or material residue. There are also cooling towers for condensers, water storage (oil) tanks for evaporators, and electrical control boxes.

When using the device of the present invention, firstly, the raw materials to be extracted should preferably be packed in cloth bags, and loaded into the tank from the upper entrance of the extraction tank. When operating non-supercritical extraction, the non-critical solvent storage tank can be used in the electrical control facility. A certain proportion of the solvent (water, alcohol, acetone, etc.) is added to the eluent from the top of the extraction tank through the third end of the solvent channel under the action of the non-supercritical solvent liquid pump for extraction. If needed to enhance the solubility of the extract throughout the extraction process The solution rate and extraction yield can be processed by ultrasonic vibration to heating, etc. As long as the ultrasonic generator is started through electrical control, the contents of the tank can be extracted by vibration. If a linear change in the concentration of the mixed solvent is required, it can be achieved by electrically controlling the operation of the separator; if the concentration efficiency of the leachate and the solvent recovery rate are to be improved, the microwave generator and compressor can be turned on (T4 is not open), so that the microwave can pass through The bridge will radiate the leaching liquid in the evaporator, and promote the rapid evaporation of the solvent inside the leaching liquid, or start the compressor to evacuate the evaporator, which can also promote the rapid evaporation of the leaching liquid solvent. The evaporated solvent vapor is condensed by the non-supercritical condenser and then recovered into the storage tank. . When the non-supercritical extraction is over, if you need to recover the material residue and the solvent in the extraction extract, turn on the non-supercritical automatic solvent recovery switch, and start the compressor to quickly extract the evaporation solvent from the evaporation tank and the extraction tank, respectively. After the condenser is cooled, it enters the non-supercritical liquid storage tank for recovery. If the extraction method needs to be changed to a supercritical state, the solvent circulation of the non-supercritical system can be closed through the electronically controlled conversion system (if it has been opened, the non-supercritical solvent must be recovered and then closed), and the supercritical solvent (C0 ₂ Etc.) The solvent in the storage tank is added to the extraction tank for extraction, and the compressor shifts to the supercritical extraction cycle. The pressure and temperature can be achieved by electronic control. At the end of extraction, the supercritical automatic solvent recovery switch should be turned on to recover the solvent into the storage tank. After closing the supercritical storage tank, restore the normal pressure of the system, and then open the discharge orifice door at the lower end of the evaporation tank to collect the extract concentrate.

 The present invention is designed and developed because it improves the current existing Chinese medicine extraction equipment that does not meet the requirements of GMP production. It can realize the rapid and automatic extraction of two critical liquid solvents in a set of equipment and concentrate the effective ingredients such as traditional Chinese medicine. Linear change in solvent concentration, automatic recycling and recovery functions, stable production and operation, no solvent leakage, high efficiency, and extraction spectrum bandwidth. The effective component selective separation and extraction can be accomplished by changing the temperature and pressure of the solvent and the extraction process to achieve a large The purpose of large-scale preparation and processing is very simple.

BRIEF DESCRIPTION OF THE DRAWINGS

 The specific structure of the present invention is given by the following embodiments and the accompanying drawings.

 FIG. 1 is a structural view of the present invention.

detailed description

Example 1 _:

An extraction tank (1), the extraction tank (1) is fixed on the upper end of the fixed frame (2), and the middle of the liquid storage tank (5), the middle liquid storage tank is fixed in the middle of the lower fixed frame (2) of the extraction tank (1). (5) The lower end of the fixed frame (2) is fixed with a heat circulation pump (11) in the middle of the other layer; the side of the fixed frame (2) is provided with an evaporator (6), a microwave generator (9) and a supercritical gaseous filter. (12); a non-supercritical solvent storage tank (3) is provided at the rear end of the fixed frame (2); a supercritical liquid storage tank (15) and supercritical condensation are provided at the other end of the fixed frame (2) (14) and compressor (13): An electric control box (8) is provided at the side of the entire device. The extraction tank (1) is provided with a material entry hole at the top, and the bottom of the lower end The liquid pipeline is provided with a medium storage tank (5) between the three-way solenoid valve (T2) and the fixing frame (2), and a supercritical evaporation spray head connected to the upper end of the evaporator (6) through a supercritical infusion capillary tube, and an extraction tank ( 1) The upper end thermal circulation water (oil) pipe is connected to the evaporator (6) upper return water (oil) pipe and the water storage (oil) tank through a three-way pipe, and the lower end of the extraction tank (1) is thermally circulated into the water (oil) pipe. It is connected to the heat circulation water outlet (oil) pipe of the lower end of the heat circulation pump (11) and the evaporator (5), and the bottom of the extraction tank (1) is provided with a slag checking hole; the pipeline under the middle liquid storage tank (5) and the evaporator (6) The liquid inlet hole below the liquid level gauge is connected, and the upper pipe is connected to the three-way solenoid valve (T2)-the split end; one of the three ends of the three-way solenoid valve (T2) is connected to the spray at the top of the evaporator (6) through a capillary tube. Head; the middle of the top of the evaporator (6) is provided with a steam channel to connect the Zizi (18), the Zizi (18) is equipped with a thermostat and a Zizi drainage pipe connected to the Zizi liquid storage tank (4); The top of the evaporator (6) is also provided with a supercritical evaporation spray head, the upper end is provided with a heat circulation return water (oil) pipe, and the lower and middle parts are provided with a supercritical evaporation spray head. The boundary return pipe is connected to a settling separator (7) fixed in the middle of the exterior. A liquid level gauge is also installed on the outside, a temperature controller and a thermal water outlet (oil) pipe are installed on the lower end, and a microwave guide bridge (10) and a microwave generator are connected on the lower end. (9), the bottom is provided with extract holes, the upper end of the evaporator (6) is connected to the upper end of the non-supercritical condenser (18); the upper end of the supercritical sedimentation separator (7) is provided with a pipe and a supercritical side The gas filter (12) is connected, and the other end of the pipe of the supercritical gas filter (12) is connected to the compressor (13) and the extraction tank (1) through a three-way solenoid valve (T3); the outlet of the compressor (13) The pipe is connected to the supercritical condenser (14) and the non-supercritical condenser (18) through the three-way solenoid valve (T4), and the other end of the pipe is switched on and off The valve is connected to the top of the supercritical liquid storage tank (15), and the lower end pipe of the supercritical liquid storage tank (15) is connected to the upper end of the extraction tank (1) through the on-off valve; all electrical control channels are implemented through the control box (8).

Claims

Rights request 1. An extraction tank, a fixed frame, a medium storage tank, a solvent storage tank, a supercritical condenser, an evaporator, a separator, a supercritical sedimentation separator, a supercritical liquid storage tank, and a non-supercritical solvent condenser , Filter, water storage (oil) tank, ultra-microwave generator, microwave generator, compressor, electric control box and pipeline solenoid valve connected between various devices, etc. It is characterized by: an extraction tank, the extraction tank is fixed on the upper end of the fixed frame, the middle of the lower end of the extraction tank is fixed with a medium storage tank, and the lower end of the middle storage tank is fixed with a heat circulation pump in the middle Evaporator and micro generator are set on the side of the fixed frame; solvent storage tank is set on the rear side of the fixed frame; supercritical liquid storage tank, supercritical condenser and compressor are set on the other side of the fixed frame ; An electric control box is set at the side of the entire device.  2. The multifunctional high-efficiency dynamic linear double-critical automatic extraction and concentration device according to claim 1, characterized in that the extraction tank is fixed at the upper end of the fixed frame; the inner tank of the extraction tank is inside the sieve hole and the wall of the tank body. Equipped with an ultrasonic oscillator, heater, temperature controller and liquid level gauge, a thermal insulation layer is laid on the tank wall; a solvent channel is provided in the center of the top of the extraction tank; There are materials entering the hole, and the hole cover is designed to withstand high pressure and sealed without leaking air; a liquid outlet pipe at the bottom of the lower end of the extraction tank is connected to the middle liquid storage hoop fixed in the middle of the fixed frame; a pancreatic heat circulation tube in the inner layer of the extraction tank extract The inlet and outlet pipes are set at the lower end of the tank and connected to the water-proof (oil) heating layer of the evaporator through an effective circulation pump. A slag checking hole on the lower end of the tank is provided to seal the switch.  3. The multifunctional high-efficiency dynamic linear double-critical automatic extraction and concentration equipment according to claim 1, characterized in that the medium storage tank is fixed below the extraction tank, and the upper end is selected from the extraction pipe of the extraction tank, and the bottom outlet The liquid channel is divided into two by a three-way valve. One is for non-supercritical extraction, which is entered from the liquid inlet hole under the evaporator through a liquid inlet pump; and the other for supercritical extraction, which is entered from the top of the evaporator through a capillary through a spray head. 4. The multifunctional high-efficiency dynamic linear double-critical automatic extraction and concentration equipment according to claim 1, characterized in that the evaporator is provided with a water-proof (oil) heat exchange interlayer, and the upper center of the evaporator is provided with steam. Hole and supercritical material leaching liquid spray head, the top of the steam hole is connected with a separator: the upper end of the separator is connected to the upper inlet of the non-supercritical condenser, and the upper end of the non-supercritical condenser is also connected to the three-way solenoid valve (T5). The lower end of the non-supercritical condenser is connected to a three-way solenoid valve (T1); the upper end of the evaporator is also fixed with another pipe, which is internally connected with a water (oil) heat exchange sandwich, and the externally connected extraction tank heat circulation pipe and Water storage (oil) tank; The microwave guide bridge connected to the upper end of the evaporator is connected to the microwave generator; there is no non-supercritical extractable pressure level gauge at the middle side of the evaporator and the non-supercritical fluid is connected to the bottom of the non-supercritical medium storage tank. The critical leachate input pipe is provided with a supercritical air return pipe in the middle and lower part which is connected with the air inlet hole at the lower end side of the supercritical sedimentation separator, and an extract extracting hole is provided at the bottom. 5. The multifunctional high-efficiency dynamic linear double-critical automatic extraction and concentration equipment according to claim 1, wherein a supercritical sedimentation separator is fixed in the middle of the outer surface of the evaporator, and the upper end of the supercritical sedimentation separator is laterally disposed. The gas outlet pipe is connected to the supercritical gas filter. The other pipe of the supercritical gas filter is connected to the compressor through a three-way solenoid valve (T3)-the split end is connected to the compressor, and the other pipe of the compressor is connected to the three-way solenoid valve (T4, Τ5). ) Connected to the supercritical condenser. The other end of the supercritical condenser is connected to the top of the supercritical liquid storage tank through a one-way sealed solenoid valve. The lower end of the supercritical liquid storage tank is connected to the upper end of the extraction tank through a one-way sealed solenoid valve. One end of the solvent channel is connected.  6. The multifunctional high-efficiency dynamic linear double-critical automatic extraction and concentrating device according to claim 1, characterized in that the transmission control system is arranged in the separating device, and a pipeline is connected to the storage tank of the separating liquid, and A pipe is connected to the upper end of the non-supercritical condenser.  7. The multifunctional high-efficiency dynamic linear double-critical automatic extraction and concentration device according to claim 1, characterized in that said condensers are all composed of a double-layer water-cooled pancreatic tube.