CN214252159U - Continuous separation type supercritical fluid chromatographic system - Google Patents
Continuous separation type supercritical fluid chromatographic system Download PDFInfo
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- CN214252159U CN214252159U CN202023325525.2U CN202023325525U CN214252159U CN 214252159 U CN214252159 U CN 214252159U CN 202023325525 U CN202023325525 U CN 202023325525U CN 214252159 U CN214252159 U CN 214252159U
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- carbon dioxide
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- 238000000926 separation method Methods 0.000 title claims abstract description 27
- 239000012530 fluid Substances 0.000 title abstract description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 122
- 239000007788 liquid Substances 0.000 claims abstract description 89
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 61
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 61
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 11
- 239000010959 steel Substances 0.000 claims abstract description 11
- 238000004440 column chromatography Methods 0.000 claims abstract description 4
- 238000004808 supercritical fluid chromatography Methods 0.000 claims description 10
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000000746 purification Methods 0.000 abstract description 2
- 238000005057 refrigeration Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 4
- 238000013375 chromatographic separation Methods 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The utility model discloses a continuous separation type supercritical fluid chromatographic system, which comprises a mobile phase liquid inlet pipeline, a sample liquid inlet pipeline and a column temperature box; liquid carbon dioxide enters a heater after being mixed with an entrainer through a mobile phase liquid inlet pipeline, the heated carbon dioxide in a supercritical state enters a chromatographic column of a column incubator through a liquid inlet valve, meanwhile, a sample to be separated enters the corresponding chromatographic column through a sample inlet valve under the driving of a liquid inlet pump, an extracting solution of the sample to be separated after the chromatographic column chromatography separation enters a cyclone separator, required components after gas-liquid separation enter a collecting steel cylinder, carbon dioxide gas enters a carbon dioxide purifier through a back pressure valve B to be filtered, and the filtered and purified carbon dioxide enters the mobile phase liquid inlet pipeline again to be recycled. The system of the utility model can continuously sample, and can select the number of the chromatographic columns connected in series according to the type of the sample to be separated, thereby ensuring the separation quality and the separation efficiency of the sample; in addition, carbon dioxide used in the system can be recycled through purification, refrigeration and pressurization, and resources are effectively saved.
Description
Technical Field
The present invention relates to a supercritical fluid chromatography system, and more particularly to a continuous separation type supercritical fluid chromatography system.
Background
The supercritical fluid is characterized by low viscosity of gas, high density of liquid, higher diffusion coefficient between gas and liquid and the like when carbon dioxide is higher than critical pressure and critical temperature, the supercritical fluid chromatography is a supplement of liquid chromatography and gas chromatography, the supercritical fluid chromatography can solve the problems which cannot be solved by gas chromatography and liquid chromatography, can analyze nonvolatile samples which are difficult to vaporize by gas chromatography, and simultaneously has higher efficiency and shorter analysis time than the high performance liquid chromatography. A conventional preparative or semi-preparative supercritical fluid chromatography system (patent No. ZL2016206577411) uses a single column for separation, and since continuous sample injection cannot be performed, the separation efficiency is low, and the used carbon dioxide is directly discharged into the air, which causes waste.
SUMMERY OF THE UTILITY MODEL
Utility model purpose: aiming at the problems that the separation efficiency of a supercritical fluid chromatographic system in the prior art is low and carbon dioxide cannot be recycled, a continuous separation type supercritical fluid chromatographic system is provided.
The technical scheme is as follows: the utility model discloses a continuous separation type supercritical fluid chromatographic system, which comprises a mobile phase liquid inlet pipeline, a sample liquid inlet pipeline and a column incubator; liquid carbon dioxide enters a heater after being mixed with an entrainer through a mobile phase liquid inlet pipeline, the heated carbon dioxide in a supercritical state enters a chromatographic column of a column incubator through a liquid inlet valve, meanwhile, a sample to be separated enters the corresponding chromatographic column through a sample inlet valve under the driving of a liquid inlet pump, an extracting solution of the sample to be separated after the chromatographic column chromatography separation enters a cyclone separator, required components after gas-liquid separation enter a collecting steel cylinder, carbon dioxide gas enters a carbon dioxide purifier through a back pressure valve B to be filtered, and the filtered and purified carbon dioxide enters the mobile phase liquid inlet pipeline again to be recycled.
The mobile phase liquid inlet pipeline comprises a refrigerator, a booster pump, a booster tank, a pressure reducing valve, a flowmeter and a flow regulating valve, carbon dioxide after being purified is filtered and liquid carbon dioxide coming out of a steel cylinder enter the refrigerator together for cooling, and the carbon dioxide is pumped into the booster tank through the booster pump after being cooled by the refrigerator.
Wherein, the liquid carbon dioxide that the pressure boost jar came out falls into two branch roads, one of them branch road is feed liquor branch road I, liquid carbon dioxide in the feed liquor branch road I flows through relief pressure valve I, flowmeter I and flow control valve I, get into heater I after mixing with the entrainer and heat, then get into in the feed liquor valve, another branch road is feed liquor branch road II, feed liquor branch road II is arranged in bringing the sample into the chromatographic column, be equipped with relief pressure valve II on the feed liquor branch road II, flowmeter II and flow control valve II, liquid carbon dioxide in the feed liquor branch road II flows through relief pressure valve II, flowmeter II and flow control valve II, get into heater II after mixing with the sample and heat, then get into in the introduction valve.
The system comprises a valve, a flowmeter, a pump and a back pressure device, wherein the valve, the flowmeter, the pump and the back pressure device are connected with the control system through signal lines respectively.
Has the advantages that: the system of the utility model can continuously sample, and can select the number of the chromatographic columns connected in series according to the type of the sample to be separated, thereby ensuring the separation quality and the separation efficiency of the sample; in addition, carbon dioxide used in the system can be recycled through purification, refrigeration and pressurization, and resources are effectively saved.
Drawings
FIG. 1 is a system schematic diagram of a supercritical fluid chromatography system of the present invention;
FIG. 2 is a schematic diagram of a structure in which polychromatic spectra columns are connected in series in a column incubator.
Detailed Description
The technical solution of the present invention will be further explained with reference to the accompanying drawings.
As shown in fig. 1-2, the utility model discloses during the specific application, A is the compressed air import, and B is the import of liquid carbon dioxide, and compressed air passes through A mouth and gets into air supply main valve 27, gets into regulator cubicle 2 through air supply main valve 27, provides the air supply for pneumatic valve (11, 45), backpressure ware (12,44) and flow control valve (23, 38) respectively to the system can not normally work when air supply main valve 27 does not detect pressure.
The utility model discloses a continuous separation type supercritical fluid chromatographic system, which comprises a mobile phase liquid inlet pipeline, a sample liquid inlet pipeline and a column incubator 13; the mobile phase liquid inlet pipeline comprises a refrigerator 22, a booster pump 17, a booster tank 7, a pressure reducing valve, a flow meter and a flow regulating valve, liquid carbon dioxide enters a heater after being mixed with entrainer through the mobile phase liquid inlet pipeline, the heated carbon dioxide in a supercritical state enters a chromatographic column of a column oven 13 through a liquid inlet valve 41, a sample to be separated enters a corresponding chromatographic column through a sample injection valve 14 under the drive of a liquid inlet pump 15, an extracting solution of the sample to be separated after chromatographic column chromatography separation enters a cyclone separator, required components after gas-liquid separation enter a collecting steel cylinder, carbon dioxide gas enters a carbon dioxide purifier 8 through a back pressure valve B10 for filtration, the filtered pure carbon dioxide (at the moment, the carbon dioxide is in a gas-liquid mixed state) and the liquid carbon dioxide coming out of the steel cylinder enter a refrigerator together for cooling, and the carbon dioxide is pumped into the booster tank through the booster pump after being cooled by the refrigerator (the liquid carbon dioxide is obtained after being cooled by the refrigerator) for cooling) to be pumped into the booster tank for cooling Can be recycled.
Or additionally arranging a liquid inlet pipeline for quickly bringing the sample into the chromatographic column, namely dividing the liquid carbon dioxide from the pressurizing tank 7 into two branches, one branch is a liquid inlet branch I20, liquid carbon dioxide in the liquid inlet branch I20 flows through a pressure reducing valve I26, a flow meter I24 and a flow regulating valve I23, after being mixed with entrainer (the entrainer enters a liquid inlet branch I20 under the driving of an entrainer pump 25), the mixed entrainer enters a heater I21 for heating, and then enters a liquid inlet valve 41, the other branch is a liquid inlet branch II30, the liquid inlet branch II30 is used for rapidly bringing a sample into the chromatographic column, the liquid inlet branch II30 is provided with a pressure reducing valve II16, a flow meter II37 and a flow regulating valve II38, the liquid carbon dioxide in the liquid inlet branch II30 flows through the pressure reducing valve II16, the flow meter II37 and the flow regulating valve II38, after mixing with the sample, the mixture enters a heater II39 to be heated, and then enters an injection valve 14.
When the system works, liquid carbon dioxide enters the system from a steel cylinder through a liquid carbon dioxide inlet-B port, the liquid carbon dioxide firstly enters a refrigerator 22 for cooling, pure liquid carbon dioxide is pumped into a pressure increasing tank 7 through a booster pump 17, the pressure in the pressure increasing tank 7 is controlled by adjusting a back pressure valve A9, the liquid carbon dioxide sequentially flows through a pressure reducing valve I26, a flow meter I24 and a flow regulating valve I23, the output flow of the carbon dioxide is controlled through the flow meter I24 and a flow regulating valve I23, meanwhile, an entrainer is pumped into a liquid inlet branch I through an entrainer pump I25 to be mixed with the liquid carbon dioxide, a mixed mobile phase enters a heater I21, the liquid carbon dioxide is heated to a supercritical state by the heater 21, then the carbon dioxide in the supercritical state enters a chromatographic column of a column temperature box 13 through a liquid inlet valve 41, simultaneously a sample to be separated enters the chromatographic column corresponding to the column temperature box 13 through a sample inlet valve 14 under the driving of a liquid inlet pump 15 to be mixed with the mobile phase for chromatographic separation, the number of chromatographic columns connected in series is determined in advance according to the type of a corresponding sample, a control system drives a one-way stop valve 35 between the chromatographic columns with the corresponding number to be opened, simultaneously drives an outlet 1 of a sample inlet valve 14 and a liquid inlet valve 41 to be opened and drives inlets 42 and 43 to be opened correspondingly, each outlet of the sample inlet valve 14 is correspondingly connected with a liquid inlet of one chromatographic column, the chromatographic columns connected with the corresponding outlets of the sample inlet valve 41 and the sample inlet valve 14 are the same, for example, the outlet 1 of the sample inlet valve 14 is correspondingly connected with a liquid inlet of the chromatographic column 1a, the outlet 1 of the liquid inlet valve 41 is correspondingly connected with a liquid inlet of the chromatographic column 1a, each inlet of the switching valves (42 and 43) is correspondingly connected with a liquid outlet of one chromatographic column, when the outlets 1 of the sample inlet valve 14 and the sample inlet valve 41 are opened, a sample liquid and a mobile phase enter the chromatographic column 1a, the inlet 3 of the switching valves (42 and 43) is opened, the No. 3 inlet of the switching valves (42,43) is correspondingly connected with the liquid outlet of the No. 3 chromatographic column 3a, which indicates that the sample liquid adopts 3 chromatographic columns connected in series for chromatographic separation; when the sample liquid is still in the chromatographic separation process, the liquid outlets of the sample valve 14 and the liquid inlet valve 41 are switched, liquid is fed and separated from the liquid inlet of the No. 4 chromatographic column 4a, and the liquid outlets of the sample valve 14 and the liquid inlet valve 41 are switched back and forth at the first port and the fourth port, so that the continuous sample feeding of the system is realized; the separated materials enter the corresponding cyclone separator 18 or 46 through the pneumatic valve 11 or the pneumatic valve 45 (different pneumatic valves are switched under the control of the control system, which is judged to be extracting solution based on the required components, which is raffinate, and then correspondingly enter different collecting steel cylinders), the required components after gas-liquid separation enter the collecting steel cylinder 19 or 47, carbon dioxide gas enters the backpressure valve B10, then enters the carbon dioxide purifier 8 for filtering, the carbon dioxide after pure filtration and liquid carbon dioxide coming out from the steel cylinder enter the refrigerator 22 for cooling, and the carbon dioxide and the liquid carbon dioxide are pumped into the pressure increasing tank 7 by the pressure increasing pump 17 for recycling. A back pressure regulator (12,44) is used to ensure that the carbon dioxide in the system is at a pressure in the supercritical state.
Manual shut-off valves (28,36,29,40) in the system facilitate manual shut-off of mobile phase into the column for servicing.
Claims (4)
1. A continuous separation type supercritical fluid chromatography system characterized in that: comprises a mobile phase liquid inlet pipeline, a sample liquid inlet pipeline and a column incubator; liquid carbon dioxide enters a heater after being mixed with an entrainer through a mobile phase liquid inlet pipeline, the heated carbon dioxide in a supercritical state enters a chromatographic column of a column incubator through a liquid inlet valve, meanwhile, a sample to be separated enters the corresponding chromatographic column through a sample inlet valve under the driving of a liquid inlet pump, an extracting solution of the sample to be separated after the chromatographic column chromatography separation enters a cyclone separator, required components after gas-liquid separation enter a collecting steel cylinder, carbon dioxide gas enters a carbon dioxide purifier through a back pressure valve B to be filtered, and the filtered and purified carbon dioxide enters the mobile phase liquid inlet pipeline again to be recycled.
2. The continuous separation type supercritical fluid chromatography system according to claim 1, characterized in that: the mobile phase liquid inlet pipeline comprises a refrigerator, a booster pump, a booster tank, a pressure reducing valve, a flowmeter and a flow regulating valve, carbon dioxide after being purified by filtration and liquid carbon dioxide coming out of a steel cylinder enter the refrigerator together for cooling, and the carbon dioxide is pumped into the booster tank through the booster pump after being cooled by the refrigerator.
3. The continuous separation type supercritical fluid chromatography system according to claim 1, characterized in that: liquid carbon dioxide that the pressure boost jar came out falls into two branch roads, one of them branch road is feed liquor branch road I, liquid carbon dioxide in the feed liquor branch road I flows through relief pressure valve I, flowmeter I and flow control valve I, mix back entering heater I with the entrainer and heat, then in the entering feed liquor valve, another branch road is feed liquor branch road II, feed liquor branch road II is used for bringing the sample into the chromatographic column, be equipped with relief pressure valve II on the feed liquor branch road II, flowmeter II and flow control valve II, liquid carbon dioxide in the feed liquor branch road II flows through relief pressure valve II, flowmeter II and flow control valve II, mix back entering heater II with the sample and heat, then in the admission valve.
4. The continuous separation type supercritical fluid chromatography system according to claim 1, characterized in that: the system also comprises a control system, and all valves, flow meters, pumps and back-pressure devices in the system are respectively connected with the control system through signal lines.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202023325525.2U CN214252159U (en) | 2020-12-31 | 2020-12-31 | Continuous separation type supercritical fluid chromatographic system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202023325525.2U CN214252159U (en) | 2020-12-31 | 2020-12-31 | Continuous separation type supercritical fluid chromatographic system |
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| CN214252159U true CN214252159U (en) | 2021-09-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112782315A (en) * | 2020-12-31 | 2021-05-11 | 江苏汉邦科技有限公司 | Continuous separation type supercritical fluid chromatographic system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112782315A (en) * | 2020-12-31 | 2021-05-11 | 江苏汉邦科技有限公司 | Continuous separation type supercritical fluid chromatographic system |
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| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 223005 no.1-9 Jixian Road, Huai'an Economic and Technological Development Zone, Huai'an City, Jiangsu Province Patentee after: Jiangsu Hanbang Technology Co.,Ltd. Address before: 223005 no.1-9 Jixian Road, Huai'an Economic and Technological Development Zone, Huai'an City, Jiangsu Province Patentee before: JIANGSU HANBON SCIENCE & TECHNOLOGY Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder |