Device for chromatographic separation of substances

FIELD: chemistry.

SUBSTANCE: device for chromatographic separation of substances contains three chromatographic columns connected to each other by crossover channels fitted with switching elements and extra channels fitted with switching elements which are connected to a source of the separated medium, eluent stream and system of receivers for collecting fractions. A controlled flow divider, one or more detectors and an analytical column are fitted at the output of the chromatographic separation system. Also in order to increase output and efficiency of the device for chromatographic separation of substances dissolved in supercritical fluids, the receivers for collecting fractions are fitted with level sensors and their outputs are further fitted with pilot-controlled valves which prevent diffusion of collected substances between receivers. The device also has a collector with a receiver and a flow regulator for the stream of fluids evaporated when pressure falls below the critical value. The device also has a high-pressure pump whose output is also connected to the flow regulator with pressure sensors at the input and output and a flow sensor, which guide part of the stream of formed fluids through the pilot-controlled valve into one or more spherical reactors which have an outer insulating layer and outer and inner heat chambers connected to heat or cold sources, temperature sensors, and the other part of the stream is directed to the analytical column and reactor. The reactor is connected through the pilot-controlled valve to the spherical collector of fluid solutions which is similar to the reactor whose output is connected to liquid batch collection device.

EFFECT: more accurate batching and increased output and efficiency of the disclosed device.

1 dwg

 

The invention relates to a device for the separation or purification of substances by methods of liquid chromatography.

Known preparative chromatograph, (1)containing three chromatographic column with direct, reverse and bypass option horizontal flow shared substance and solvent. The drawbacks are the low productivity due to work in discrete mode and use speakers with murine effect of blurring the chromatographic strip, negatively affecting the quality of secreted products, and the lack of effect of temperature on the sorption-desorption process.

A device (2), containing three chromatographic columns that implement the principles of radial flow chromatography in a continuous mode that allows you to use and the temperature factor reducing and murine effect due to the use of closed curves in space surfaces of the sorption layer.

The drawback of the device (2) can be considered as a lack of operational control of the quality of the chromatographic separation and the possibility to change settings directly in the process.

A device (3), containing three chromatographic columns that implement the principles of radial flow chromatography in a continuous mode of operation, is the quiet made in the form of closed space curves, symmetric surfaces, reducing murine effect. The device (3) has an adjustable flow divider, analytical column with detection devices, allowing you to control and adjust in real time the process of chromatographic separation.

The device (3) is the closest solution proposed. But (3) does not work with substances dissolved in supercritical fluids (SCF) at high pressure. GFR occupies an intermediate position between gas and liquid. He can, in contrast to normal fluid to be compressed when the pressure is above critical, and temperatures below the critical, and have a liquid state or to expand, turning into a source gas at a low pressure to a value less critical.

The purpose of the invention is improving the performance and efficiency of the chromatographic separation of substances dissolved in the SCF.

This objective is achieved in that the device for chromatographic separation of substances containing three chromatographic columns connected to each other transitional channels with installed switching elements that are connected to a source of partial mixture with a stream of eluent and receivers to collect fractions of the column, consisting of issaa insulation, the outer case, the outer porous wall, divided into sections intermediate porous partitions sorption layers, the inner porous wall of the inner casing, made in the form of closed-in space of such curves, surfaces, consistently covering each other, between the outer porous wall and an outer housing there is a gap in which, through multiple channels distributed introduces shared substance, and the channel output separable mixtures connected by one or more channels to the gap between the inner porous wall and the inner housing, and a chamber between the layer of thermal insulation and outer casing and the chamber formed by the inner housing, additional channels with installed managed switch elements connected with a source of coolant and the refrigerant at the outlet of the chromatographic separation system has an adjustable flow divider, one or more detectors and analytical column. Creates a closed system for continuous separation with the formation of the SCF, the dissolution of solid and liquid substances, and desireable fluid solutions in preparative chromatographic column, the separation and withdrawal of products in the receivers fractions where the fluid into gas, is collected and again the translation is carried out in GFR.

To ensure device operation chromatographic separation of substances dissolved in the SCF, the receivers collect fractions equipped with level sensors, and the output of them installed controlled valves, eliminating the diffusion of the collected substances between receivers, the collector receiver and regulator flow rate of evaporated by reducing the pressure of the fluid below the critical, high-pressure pump, the output of which is also connected flow regulators with pressure gauges on the inlet and outlet and a flow directing a portion of the flux produced fluids through a controlled valve in one or more spherical reactors for the partial dissolution of the substance, and the other part of the flow through a controlled valve on the analytical column.

The reactor via a controlled valve connected to the fluid collection solutions, the output of which is connected to the device selection of a dose of liquid, consisting of a switch threads, the intermediate measured capacities with concave walls for linearization of the scale of the magnitude of the doses and installed inside them turning tubes, having the drive and the ability to move in multiple degrees of freedom, while the inlet of the rotary tube can change its level relative to the upper liquid level in the intermediate volumetric capacity, the channels on which I feed propellant from the collection of fluid solutions and measuring tanks with flow regulators, contains pressure sensors at the inlet-outlet and a flow sensor connected via the high pressure reducer to the capacity of the propellant. To create and stabilize the pressure gradient in the system chromatographic separation to the receiver at the output of receivers separated into fractions or components of source materials, through the high pressure reducer connected capacitance turn in fluid gas. The temperature control fluid is supplied from the source of coolant and refrigerant channel managed valves.

Figure 1 shows the schematic diagram of the proposed device. The device comprises a chromatographic column 1, 2, 3 with the radial flow of the partial substances and eluent. They can take the form of, for example, sphere, ellipsoid, and other closed distributed in space, surfaces, covering each other. The columns are interconnected transitional channels 11-24 with installed switching elements 26-43 in the form of, for example, diaphragm valves with pneumatic booster driven by means of compressed air. Transitional channels connected to the reservoir 4, 5, 6, 7, 8. Heating or cooling of each column individually, through the reservoir 9, 10, and switches 44-51. Supply flows on the sorption, desorption and regeneration in chromatographic columns, the production is carried out through the channels 53, 54, 55. The channel 52 and pH meter 68 is installed on the output sorbed flow, and channel 56 - deformiruemogo and regeneration. At the output of the channel 56 has a flow divider 57, forming in addition to the main flow bypass line 58. The bypass line is connected to the detector 59, pH meter 60, analytical column 61, the dispenser 62 and additional eluent channel 63. Switchable valves 64, 65, 66 and 67 by the signal detector 59 distributed for the hooks 66A and 67a useful components or fractions. The level control collect fractions or components are determined by the sensors 69 and 70, for example ultrasound.

The proposed device belongs to the category of radial-flow chromatographs, convenient for ion exchange, affinity, hydrophobic, obrashennih and other sorption-desorption divisions.

Initially, the column 1 is set to the mode of sorption. Through the channel 53, the collector 4, the channel 25, the valve 43, the channel 16 sorbed flow with the shared substance passes through the layer of sorbent column 1. The valves 40, 41, 42; 27, 29 are closed. The release of sorbed flow through the channel 11 and the valve 26 into the reservoir 6 through the channel 52, the locking readings of the pH-meter 68 - team capacity.

Simultaneously, the column 2 is in the desorption mode. Eluent flows into it through the channel 54, the collector 7, the channel 18, the open valve 28, the channel 12. The valves 30, 31 are closed. The origin of the result of the displacement of the sorption layer detainees components. The flow of eluent together with replaced components through the channel 13, the open valve 33, the collector 4, the channel 56 is supplied to the flow divider 57. The valve 32 sacristy flow via the bypass line 58 is fed to the detector 59, pH meter 60. The main part of the flow passes through the valves 64, 66 or 65, 67, controlled by the signal detector, traps 66A or 67a.

Column 3 is in the regeneration mode, i.e. cleaning of traces of eluent, and works simultaneously with columns 1 and 2. The liquid stream, purifying column 3, flows through the channel 55, the collector 8, the channel 22, the valve 36, the channel 14. The valves 34, 35, 37 are closed. The output stream from the column 3 is carried out via channels 15 and 23 through the valve 39, the collector 5, the channel 56, the flow divider 57, the bypass line 58, the detector 59, pH meter 60, the valve 65 vent trap 67a and the valve 67 to the reservoir 71.

The time column is determined by their sorption capacity. Each cycle of the column operates in the mode of sorption, desorption and regeneration program flow switching. After the first switching column 1 mode "sorption" goes into "desorption", column 2 is in mode "regeneration", column 3 - mode "sorption". Then column 1 goes into "regeneration", column 2 is in mode "sorption", column 3 - mode "desorption", etc. Thus, by switching the flow is continuous chromatographic partition is of substances with control and adjustment of the quality and efficiency of separation in real time.

The original form of the analytical column similar to the form of preparative column, made in the form of closed space curves distributed surfaces, covering each other. It allows you to simulate large-scale processes in the preparative columns.

Through the dispenser 62 in manual or automatic mode is entered in column 61 the estimated value of the sample. The signal detector 59 determined the optimal parameters of temperature, flow rate, eluent buffer fluid, consistently implemented the process of adsorption, desorption and regeneration.

For the formation of SCF in the manifold 71 is installed receiver 72, which is connected through a high pressure reducer cylinder 104 103 filled with fluid forming gas such as xenon (Xe), which has a critical pressure of 5.8 MPa and the critical temperature of +16,6C. At the outlet of the receiver 71 through the flow regulator 7 with pressure sensors at the inlet and outlet and a flow 73a and b connected to the high pressure pump 74 through the flow regulator 73 and managed the valve 75 through the channels 80 and 63 directs the flow Heh pressure above the critical temperature and below the critical in the reactor 78 on the partial dissolution substances or dispenser 62 analytical column for analysis of substances to the chromatographic column and after chromatographic separation. The reactor 78 having the t shape of the closed space curves, surfaces, covering each other, for example spherical. He is isolated from the environment of the insulating layer 87 has a few cameras: external temperature chamber 88, the reaction chamber 78, the inner temperature of the chamber 83. Chambers 88 and 89 connected to the heat source 10 and cold 9 through controlled valve 75, the channel 82, using temperature sensors 105 maintain the temperature GFR below critical. The reactor is equipped with an adjustable blow-off valve 106. After dissolution in GFR shared substances from the reactor 78 the mixture through a controlled valve 81 is sent to the spherical supply tank 79, having an insulating layer 86, the external thermal chamber 85, the internal thermal chamber 84, the level sensor a, temperature sensors 105 to maintain the temperature GFR below critical.

The supply tank 79 channel 90 is connected to the flow switch 92 device for selection of doses of fluid, which includes the high-pressure bladder 77 with high pressure reducer 76. In the cylinder 77 is an inert gas propellant, such as argon (Ar), a critical temperature is 122C and critical pressure of 4.8 MPa, at temperatures Heh around 0C does not allow you to go Ar in the SCF phase, remaining in the gas phase.

The gearbox output channel 76 89 through the flow regulator 73 with pressure sensors 73a and flow V is connected with a metering container of the STU 79, and channel 91 through the flow regulator 73 with pressure sensors 73a and flow V - switch threads 92 of the device for selecting a dose of the liquid.

Device for selection of a dose of liquid in addition to switch threads 92 has an intermediate volumetric capacity 98, 102 with concave walls for linearization of scales of values doses 96, 100 and installed inside them swivel tube 97, 101, with actuators 95, 99 and the ability to move in multiple degrees of freedom. The input hole of the rotary tubes 97, 101 can change its level relative to the upper liquid level in the intermediate measuring containers 98, 102. Control flow switch 92 by using detectors of the gas phase 93, 94 mounted at the exit of the rotary tube.

In the proposed device created a closed loop continuous chromatographic separation of solid and liquid substances dissolved in formed from the gas GFR engaged in the transition back into a gaseous state at a pressure below the critical at the time of collection products chromatographic separation followed by the formation of SCF, dissolved substances and dispensing them into a chromatographic column filled with an inert gas to a pressure above the critical value.

The presence in the chromatographic column of a significant pressure gradient allows you to work in conditions of high the effective liquid chromatography (HPLC), that improves the performance and efficiency of the chromatographic separation, the proposed device.

It should be noted and the universality of the scheme proposed device that enables operation in the combined mode chromatographic separation, including proyavitelem version with serial connection of columns.

Sources of information

1. The prospectus of the company Sepragen Corporation USA on preparative chromatograph Quanta Sep 1000, 1996

2. Patent for invention No. 2152611 on application No. 98119812 from 02.11.1998,

3. Patent for invention No. 2334227 on application No. 2007112214 from 02.04.2007, prototype.

Device for chromatographic separation of substances containing three chromatographic columns connected to each other transitional channels with installed switching elements and additional channels with installed switching elements that are connected to a source of partial mixture with a stream of eluent and receivers to collect fractions of the column, consisting of a layer of insulation, the outer case, the outer porous wall, divided into sections intermediate porous partitions sorption layers, the inner porous wall, an inner case made in the form of closed-in space of such curves, surfaces, sequentially, Katya is related to each other, between the outer porous wall and an outer housing there is a gap in which, through multiple channels distributed shared substance, and the channel output separable mixtures connected by one or more channels to the gap between the inner porous wall and the inner housing, and a chamber between the layer of thermal insulation and outer casing and the chamber formed by the inner housing, additional channels with installed managed switching elements, connected with a source of coolant or refrigerant at the outlet of the chromatographic separation system installed an adjustable flow divider, one or more detectors and analytical column, characterized in that, to improve performance and the efficiency of the device for chromatographic separation of substances dissolved in supercritical fluids receivers to collect fractions equipped with level sensors, and the output of them installed controlled valves, eliminating the diffusion of the collected substances between receivers, the collector receiver and regulator flow rate of evaporated by reducing the pressure of the fluid below the critical, high-pressure pump, the output of which is also connected flow regulators with pressure gauges on the inlet and outlet and a flow sensor, the direction is the following part of the flow produced fluids through a controlled valve in one or more spherical reactors, with external insulation layer and the external and internal thermal cameras, which are connected to sources of heat or cold, temperature sensors, and the other part of the flow on the analytical column, reactor, connected through a controlled valve with a spherical collection of fluid solutions, similar to the reactor, the output of which is connected to the device for selection of doses of fluid, consisting of a switch threads, the intermediate measured capacities with concave walls for linearization of the scale of the magnitude of the doses and installed inside them turning tubes, having the drive and the ability to move in multiple degrees of freedom, while the inlet of the rotary tube can change its level to the upper liquid level in the intermediate measuring containers, and control of the flow switch by using detectors of the gas phase, mounted at the exit of the rotary tube, the channels for supplying the propellant from the collection of fluid solutions and measuring tanks with flow regulators containing pressure sensors and flow connected through a high pressure reducer to the capacity of the propellant to create a supercritical fluid and stabilize the pressure gradient in the system chromatographic separation, to the receiver at the output of receivers fractions and components shared in the substances through the high pressure reducer connected capacity into the supercritical fluid of gas.



 

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