CN211561924U - Simulated moving bed separation device with dilute solution of raffinate as supplementary eluent - Google Patents
Simulated moving bed separation device with dilute solution of raffinate as supplementary eluent Download PDFInfo
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- CN211561924U CN211561924U CN201922261355.7U CN201922261355U CN211561924U CN 211561924 U CN211561924 U CN 211561924U CN 201922261355 U CN201922261355 U CN 201922261355U CN 211561924 U CN211561924 U CN 211561924U
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Abstract
A simulated moving bed separator using the diluted raffinate solution as the additional eluent is composed of 6 chromatographic columns, 6 booster pumps, a circulation flowmeter, an extract regulating valve, a raffinate flowmeter, a raffinate regulating valve, a raffinate B tank, a C tank, a D tank, an E tank, a valve connected with the chromatographic columns, a feed and discharge pipeline and an additional eluent pipeline. After the device is operated, the mixture to be separated can be separated and subdivided into a plurality of extracting solution and raffinate components, and meanwhile, part of dilute raffinate is used as supplementary eluent to reduce the dosage of the eluent.
Description
Technical Field
The utility model relates to a separation refining technology field, concretely relates to simulation moving bed separator of weak solution as supplementary eluant of raffinate.
Background
Simulated moving bed chromatographic separations can be divided into continuous and procedural.
The chromatographic separation of a program simulated moving bed comprises three basic sections: a feed section, an elution section and a circulation section. In the feed section, the mixture to be separated enters the column and the raffinate is eluted. In the elution phase, the eluent is applied to a chromatographic column and the extract is eluted. In the circulation section, the material and eluent do not enter the chromatographic column, and no product is extracted, and only internal circulation is carried out. The flow of the simulated moving bed is not continuous.
CN203139686U, CN101940850B and CN203220780 describe separation devices for chromatographic separation in a simulated moving bed of the program type.
CN203139686U can only solve two-component separation of fast and slow components; CN203220780 provides a control method for a frequency-variable pressure-variable program-type simulated moving bed chromatographic separation device. These devices do not make full use of the dilute raffinate and do not finely divide the extract and raffinate.
Disclosure of Invention
To current procedure formula simulated moving bed chromatographic fractionation device can not subdivide extract and raffinate well, and can not make full use of not enough of more rare raffinate, the utility model provides a dilute solution of raffinate is as the simulated moving bed separator of supplementary eluant, in the disengaging process, directly returns partial more rare raffinate, utilizes as supplementary eluant, has reduced the quantity of eluant, has reduced the load of raffinate simultaneously, has correspondingly reduced the cost of the concentrated raffinate of subsequent handling.
The device comprises chromatographic columns C1-C6, booster pumps P1-P6, circulating flow meters FR 1-FR 6, an extract flow meter F1, an extract regulating valve T1, a raffinate flow meter F2, a raffinate regulating valve T2, a liquid B tank, a liquid C tank, a liquid D tank, a liquid E tank, a feeding and discharging valve, a circulating valve, a supplementary eluent valve and a pipeline.
Six circulating pipes, namely circulating pipes, booster pumps P1-P6, circulating flow meters FR 1-FR 6, circulating valves R11, R12-R61 and R62 are connected between the chromatographic columns C1-C6.
An eluent valve W1, a material valve F1 and a supplementary eluent valve RR1 are connected between the circulating valves R11 and R12; an eluent valve W2, a material valve F2 and a supplementary eluent valve RR2 are connected between the circulating valves R21 and R22; an eluent valve W3, a material valve F3 and a supplementary eluent valve RR3 are connected between the circulating valves R31 and R32; an eluent valve W4, a material valve F4 and a supplementary eluent valve RR4 are connected between the circulating valves R41 and R42; an eluent valve W5, a material valve F5 and a supplementary eluent valve RR5 are connected between the circulating valves R51 and R52; an eluent valve W6, a material valve F6 and a supplementary eluent valve RR6 are connected between the circulating valves R61 and R62. The other ends of the eluent valves W1-W6 are connected with eluent pipes, the other ends of the material valves F1-F6 are connected with feeding pipes, and the other ends of the supplementary eluent valves RR 1-RR 6 are connected with each other through supplementary eluent pipes.
Outlets of the chromatographic columns C1-C6 are connected with extraction liquid valves M1-M6; the other ends of the extracting liquid valves M1-M6 are connected with an extracting liquid pipe; an extracting solution flowmeter F1 and an extracting solution regulating valve T1 are arranged on the extracting solution pipe, and then the extracting solution pipe is divided into 2 branches: the liquid tank B is connected to the liquid tank B after passing through a VB valve and a branch B; the liquid is connected to a liquid tank C after passing through a VC valve and a branch C.
The outlets of the chromatographic columns C1-C6 are also connected with raffinate valves N1-N6; the other ends of the raffinate valves N1-N6 are connected with a raffinate pipe; the raffinate pipe is provided with a raffinate flow meter F2 and a raffinate regulating valve T2, and then is divided into 2 branches: the liquid is connected to a liquid tank D after passing through a VD valve and a branch D; the liquid is connected to an E liquid tank after passing through a VE valve and an E branch.
The circulation flow meters FR 1-FR 6 are mounted on the first circulation pipe to the sixth circulation pipe.
The circulation flow meters FR 1-FR 6 are used for detecting the circulation flow during the circulation in the system; the booster pumps P1-P6 adjust the flow rate of the pumps by adjusting the power supply frequency of the pumps, so as to adjust the circulating flow rate; the extracting solution flowmeter F1 and the extracting solution regulating valve T1 are used for detecting and regulating the discharging flow of the extracting solution; and the raffinate liquid flowmeter F2 and the raffinate regulating valve T2 are used for detecting and regulating the raffinate discharge flow.
In a further improvement, the upper part and the lower part in the chromatographic column are provided with distributors.
In a further improvement, the chromatographic column is filled with an adsorbent media.
The utility model provides a liquid is carried in dilute solution of raffinate as the simulated moving bed separator of supplementary eluant selects suitable adsorbent and separation condition, with the material separation purification of difference, utilizes the liquid is carried in dilute solution of raffinate as supplementary eluant simultaneously, can save the quantity of eluant.
Drawings
FIG. 1 is an assembly drawing of a simulated moving bed separation unit using a dilute raffinate solution as the supplemental eluent.
The components in the drawings are as follows: chromatographic columns C1-C6, booster pumps P1-P6, circulating flow meters FR 1-FR 6, a first circulating pipe 5, a second circulating pipe 6, a third circulating pipe 7, a fourth circulating pipe 8, a fifth circulating pipe 9 and a sixth circulating pipe 10; eluent tube 1, feed tube 2; a supplemental eluent tube 11; an extract flow meter F1, an extract regulating valve T1, a raffinate flow meter F2 and a raffinate regulating valve T2; eluent valves W1-W6, material valves F1-F6, circulating valves R11, R12, R21, R22, R31, R32, R41, R42, R51, R52, R61 and R62, and supplemental eluent valves RR 1-RR 6; extraction liquid valves M1-M6, and extraction residue liquid valves N1-N6; liquid extracting pipe 3, branch B21, VB valve, liquid tank B, branch C22, VC valve, liquid tank C, liquid extracting pipe 4, branch D23, VD valve, liquid tank D, branch E24, VE valve, and liquid tank E.
Fig. 2 shows the first step in the operation of the apparatus. The black body in the column indicates that there is flow through.
Detailed Description
The device of the present invention will be described in further detail with reference to the accompanying drawings.
Example one
As shown in figure 1, the utility model provides a simulated moving bed separation device using dilute solution of raffinate as supplementary eluent. The device comprises chromatographic columns C1-C6, booster pumps P1-P6, circulating flow meters FR 1-FR 6, circulating flow meters FR 1-FR 6, an extract flow meter F1, an extract regulating valve T1, a raffinate flow meter F2, a raffinate regulating valve T2, a liquid tank B, a liquid tank C, a liquid tank D and a liquid tank E, a feeding and discharging valve, a circulating valve, a supplementary eluent valve and a pipeline.
Circulation pipes I5 to VI 10, booster pumps P1 to P6, circulation flow meters FR1 to FR6, circulation valves R11, R12 to R61 and R62 are connected between the chromatographic columns C1 to C6;
an eluent valve W1, a material valve F1 and a supplementary eluent valve RR1 are connected between the circulating valves R11 and R12; an eluent valve W2, a material valve F2 and a supplementary eluent valve RR2 are connected between the circulating valves R21 and R22; an eluent valve W3, a material valve F3 and a supplementary eluent valve RR3 are connected between the circulating valves R31 and R32; an eluent valve W4, a material valve F4 and a supplementary eluent valve RR4 are connected between the circulating valves R41 and R42; an eluent valve W5, a material valve F5 and a supplementary eluent valve RR5 are connected between the circulating valves R51 and R52; an eluent valve W6, a material valve F6 and a supplementary eluent valve RR6 are connected between the circulating valves R61 and R62. The other ends of the eluent valves W1-W6 are connected with the eluent tube 1, the other ends of the material valves F1-F6 are connected with the feeding tube 2, and the other ends of the supplementary eluent valves RR 1-RR 6 are connected with each other through a supplementary eluent tube 11.
Outlets of the chromatographic columns C1-C6 are connected with extraction liquid valves M1-M6; the other ends of the extracting liquid valves M1-M6 are connected with an extracting liquid pipe 3; an extracting solution flowmeter F1 and an extracting solution regulating valve T1 are arranged on the extracting solution pipe 3, and then the extracting solution pipe is divided into 2 branches: the liquid is connected to a liquid tank B after passing through a VB valve and a branch B21; the liquid C passes through a VC valve and a C branch 22 and then is connected to a C liquid tank.
The outlets of the chromatographic columns C1-C6 are also connected with raffinate valves N1-N6; the other ends of the raffinate valves N1-N6 are connected with a raffinate pipe 4; the raffinate pipe 4 is provided with a raffinate flow meter F2 and a raffinate regulating valve T2, and then is divided into 2 branches: the D liquid tank is connected with the VD valve and the D branch 23; the E liquid tank is connected after passing through a VE valve and an E branch 24.
The circulation flow meters FR 1-FR 6 are mounted on the first circulation pipe to the sixth circulation pipe. When the system is used for internal circulation and 6 chromatographic columns C1-C6 are connected in series to form a group, the flow values of the circulating flow meters FR 1-FR 6 are consistent, and only one of the circulating flow meters is taken as the measurement of the circulating flow.
The circulation flow meters FR 1-FR 6 are used for detecting the circulation flow rate during the circulation in the system. The booster pumps P1-P6 adjust the flow rate of the pumps by adjusting the frequency of power supplied to the pumps, thereby adjusting the circulation flow rate. An extract flowmeter F1 and an extract regulating valve T1 for detecting and regulating the discharge flow of the extract. The raffinate flowmeter F2 and the raffinate regulating valve T2 are used for detecting and regulating the raffinate discharge flow.
The upper part and the lower part in the chromatographic column are provided with distributors to ensure that the feed liquid is uniformly distributed and forms columnar flow.
The chromatographic column is filled with an adsorption medium compatible with the material to be separated.
Example two
The first step in the operation of the apparatus is shown in figure 2. This example details the operation thereof.
Dividing 6 chromatographic columns C1-C6 into 4 intervals of Z1, Z2, Z3 and Z4; z1 consists of 1 column, Z2 consists of 2 columns, Z3 consists of 2 columns, and Z4 consists of 1 column. Each section moves forward as the device is operated.
And the supplementary eluent pipe 11 connects the supplementary eluent valves RR 1-RR 6, and when the system runs, the liquid in any chromatographic column flows to other chromatographic columns by opening and closing the corresponding valves.
The 6 columns were filled with adsorption media compatible with the substances to be separated.
The device operation is divided into 3 periods: a circulation period StepA; elution periods StepB1, StepB2, StepB 3; feeding periods StepC1, StepC 2; these 3 periods constitute 1 step and 6 steps constitute 1 cycle. And (5) continuously circulating.
During the circulation period StepA, 6 chromatographic columns are connected in series to form a group, no material enters or exits the system at the moment, and the system performs internal circulation. At the moment, booster pumps P1-P6 are started, and circulating valves R11, R12-R61 and R62 are opened; the other valves are closed. The circulating flow is taken from one of FR 1-FR 6, accumulated, and after reaching a set value, the operation is switched to StepB1, and StepA is stopped.
During the elution period StepB1, the dilute solution was drained from the bottom of the 2 nd column of Z3, and flowed to the top of the 1 st column of Z3, and the 2 columns of Z3 self-circulated. At the moment, the booster pumps P4 and P5 are started, circulating valves R42, R51, R52 and R61 are opened, a supplementary eluent valve RR6 and a supplementary eluent valve RR4 are opened, and other pumps and valves are closed. StepB1 is advanced by a volume, that is, by setting a volume of outflow, and after the flow rate is measured and accumulated through FR5 and reaches a set value, StepB2 is executed and StepB1 is stopped. The dilute solution discharged from the lower part of the 2 nd column of Z3 is dilute in concentration and contains a small amount of substances having a weak adsorption force. If the solution discharged from the lower part of the 2 nd column of Z3 has a high concentration and contains many substances having a weak adsorption ability, it is not preferable to return the solution.
During the elution period StepB2, eluent enters from the upper part of Z1, and impurities are discharged from the lower part of the 2 nd chromatographic column of Z3 and enter an E liquid groove. The driving method of StepB2 is a volume, that is, a volume of discharged impurities is set, the volume of discharged impurities is measured and accumulated by a raffinate flowmeter F2, and after the set value is reached, the operation is shifted to StepB3, and StepB2 is stopped.
During the elution period StepB3, eluent enters from the upper part of Z1, and raffinate is discharged from the lower part of the 2 nd chromatographic column of Z3 and enters a D liquid groove. StepB3 is advanced by setting a volume flow rate, and the volume flow rate of the raffinate is measured and accumulated by a raffinate flow meter F2, and after reaching the set value, StepC1 is executed and StepB3 is stopped.
At the time of the feed period StepC1, there were 2 steps: step (1): eluent enters from the upper part of Z1, and extracting solution 1 is discharged from the lower part of Z1 and enters into a C liquid groove. The stepwise advancement is a volumetric amount, i.e. a volumetric amount of outflow is set, and the volumetric amount of outflow of the extracting solution 1 is metered and accumulated by the extracting solution flow meter F1, and after reaching the set value, the stepwise advancement is stopped and the step is shifted to StepC2 (if the stepwise advancement (2) is completed). Step (2): the mixture to be separated enters from the upper part of the 1 st chromatographic column of Z3, and the raffinate is discharged from the lower part of the 2 nd chromatographic column of Z3 and enters a D liquid groove. The stepwise advancement is a volumetric amount, i.e., a volumetric amount of effluent is set, and the volumetric amount of effluent raffinate is metered and accumulated by raffinate flow meter F2, and after reaching the set value, the stepwise advancement is stopped and the step is shifted to StepC2 (if step (1) is also completed).
At the time of the feed period StepC2, there were 2 steps: step (1): eluent enters from the upper part of Z1, and extracting solution 2 is discharged from the lower part of Z1 and enters into a liquid B tank. The stepwise advancement is a volumetric amount, i.e. a volume of extracted liquid is set, and the volumetric amount of extracted liquid 2 is measured and accumulated by the extracted liquid flow meter F1, and after reaching the set value, the stepwise advancement is stopped and the step is performed StepA (if the stepwise advancement (2) is completed). Step (2): this step corresponds to step (2) of StepC1, which, if step (2) of StepC1 is completed, is not performed and is transferred to StepA (if step (1) is also completed).
While moving from StepC2 to StepA in the next cycle, the compartments and the feed and discharge positions moved to the next column. After six operating cycles, each state of the device returns to the initial state, and the device continues to operate and continuously circulates.
The embodiment of the utility model provides a is not right the utility model discloses a restriction. The person skilled in the art can carry out many variants of the method according to the invention.
Claims (4)
1. A simulated moving bed separation device using dilute solution of raffinate as a supplementary eluent comprises chromatographic columns C1-C6, booster pumps P1-P6, circulating flow meters FR 1-FR 6, an extract flow meter F1, an extract regulating valve T1, a raffinate flow meter F2, a raffinate regulating valve T2, a feed and discharge valve, a circulating valve, a supplementary eluent valve and a pipeline, and is characterized in that,
circulating pipes I (5) to six (10) are connected between the chromatographic columns C1 to C6, booster pumps P1 to P6, circulating flow meters FR1 to FR6, circulating valves R11, R12 to R61 and R62; eluent valves W1-W6, material valves F1-F6 and supplementary eluent valves RR 1-RR 6 are connected among the circulating valves R11, R12-R61 and R62; the other ends of the eluent valves W1-W6 are connected with an eluent tube (1), the other ends of the material valves F1-F6 are connected with a feeding tube (2), and the other ends of the supplementary eluent valves RR 1-RR 6 are connected with each other through a supplementary eluent tube (11);
outlets of the chromatographic columns C1-C6 are connected with extraction liquid valves M1-M6; the other ends of the extracting liquid valves M1-M6 are connected with an extracting liquid pipe (3); an extracting solution flowmeter F1 and an extracting solution regulating valve T1 are arranged on the extracting solution pipe (3), and then the extracting solution pipe is divided into 2 branches: the liquid is connected to a liquid tank B after passing through a VB valve and a branch B (21); the liquid is connected to a liquid tank C after passing through a VC valve and a branch C (22);
the outlets of the chromatographic columns C1-C6 are also connected with raffinate valves N1-N6; the other ends of the residual liquid extracting valves N1-N6 are connected with a residual liquid extracting pipe (4); the raffinate pipe (4) is provided with a raffinate liquid flowmeter F2 and a raffinate regulating valve T2, and then is divided into 2 branches: the D liquid tank is connected with the vacuum pump through a VD valve and a D branch (23); is connected to an E liquid tank after passing through a VE valve and an E branch (24).
2. The device according to claim 1, wherein the circulation flow meters FR 1-FR 6 are used for detecting the circulation flow rate when circulating in the system; the booster pumps P1-P6 adjust the flow rate of the pumps by adjusting the power supply frequency of the pumps, so as to adjust the circulating flow rate; the extracting solution flowmeter F1 and the extracting solution regulating valve T1 are used for detecting and regulating the discharging flow of the extracting solution; and the raffinate liquid flowmeter F2 and the raffinate regulating valve T2 are used for detecting and regulating the raffinate discharge flow.
3. The apparatus of claim 1, wherein the upper and lower portions of the column have distributors.
4. The apparatus of claim 1, wherein the chromatography column is packed with an adsorbent media.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112979418A (en) * | 2019-12-17 | 2021-06-18 | 南京凯通粮食生化研究设计有限公司 | Method for separating ethylene glycol and butanediol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112979418A (en) * | 2019-12-17 | 2021-06-18 | 南京凯通粮食生化研究设计有限公司 | Method for separating ethylene glycol and butanediol |
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