CN102218225B - Column chromatography separating unit - Google Patents
Column chromatography separating unit Download PDFInfo
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- CN102218225B CN102218225B CN 201110077072 CN201110077072A CN102218225B CN 102218225 B CN102218225 B CN 102218225B CN 201110077072 CN201110077072 CN 201110077072 CN 201110077072 A CN201110077072 A CN 201110077072A CN 102218225 B CN102218225 B CN 102218225B
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- serpentine condenser
- grinding port
- outer grinding
- chromatographic column
- column chromatography
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Abstract
The invention discloses a column chromatography separating unit, which comprises a spherical condensing pipe, a coiled condensing pipe, a chromatography column, a reaction container and a heater, wherein an outer grinding port at the lower part of the spherical condensing pipe is connected with an inner grinding port of the coiled condensing pipe; an outer grinding port of the coiled condensing pipe is connected with an inner grinding port of the chromatography column; an outer grinding port of the chromatography column is connected with the reaction container; and a communicated side pipe is arranged between the upper end of a chromatography column body and the upper edge of the outer grinding port of the chromatography column. The column chromatography separating unit integrates the separation and condensation of mixtures. As the connecting parts are connected by the grinding ports, the separation and condensation of the mixtures can be realized in a relatively closed pipeline; easily oxidized and decomposed substances are reduced from being contacted with the air; and environmental pollution is prevented simultaneously when solvent loss is reduced.
Description
Technical field
The present invention relates to a kind of column chromatography separating unit, particularly a kind of integrated, capable of circulation and eco-friendly column chromatography separating unit can be applicable to the fields such as chemical engineering, pharmaceutical engineering and food engineering.
Background technology
Chromatographic technique be a kind of according to different material in different medium physics, chemistry or biological property difference and migration velocity is different, thereby realize the technology of the separation and purification of material now has been widely used in the industries such as chemical industry, food, medicine.Column chromatography is one of a kind of separation means the most frequently used in chromatography process.Column chromatography method commonly used can be divided into non-pressure process, negative pressure method and pressurization according to the separating pressure difference.The normal pressure column chromatography is most widely used in practice, normally adopts as required different adsorbents, eluant, eluent to come the separation and purification of realize target material.
A kind of column chromatography device is disclosed among the CN200920166640, device is realized the separation of mixture and is concentrated in the pipeline of relatively sealing, be connected for ground between chromatographic column and the receiving flask, be provided with pipette in the receiving flask, pipette is connected with a Rotary Evaporators again, the solution that chromatography is collected is concentrated, be a kind of column chromatography device of realizing mixture separation and simmer down to one.But this device for the sample that is difficult to separate, can need a large amount of solvents in actual mechanical process, but also needs the artificial eluant, eluent that adds, and on the top of chromatographic column, has solvent evaporates and the loss that causes.
A kind of chromatographic column device for separating of chemical mixture and natural products is disclosed among the CN200720201107.This device is fairly simple, and the chromatographic column upper end is designed for ground, can install liquid feeding ball and pressue device additional; The minim pipette of cylinder lower end adopts teflon piston, good airproof performance.But this device can not be avoided a large amount of volatilizations of solvent in specific implementation process, do not prevent the concrete measure of solvent evaporates.
A kind of device for pressurized column chromatography is disclosed among the CN200820188701.The upper end of chromatographic column is connected with pressurizer.The chromatographic column cylinder upper end is provided with two with the arm of piston, is used for connecting sample injector, and the sample injector lower end is provided with two with the arm of piston, and is connected with the chromatographic column upper end, can control the interpolation of eluant, eluent, when piston is opened, consists of the container of a connection; The sample injector outside is provided with scale, can observe intuitively the consumption of eluant, eluent, convenient record and calculating consumption, and there is a ground lid its upper end.But this device need to manually add eluant, eluent, lacks the volatilization prevention protection to eluent and eluant, eluent, can not the continuous circulation operation.
In sum, common column chromatography device has the following disadvantages at present: separation and concentration and recovery carry out step by step usually, need continually supplementing solvent in the chromatographic column, receiving flask also needs to reclaim solvent by means such as rotary evaporations continually, cause easily so on the one hand dried post, for the material of unstable, the easy decomposition of character, easy oxidation, owing to the long period ingress of air or when environment temperature is higher, occur to decompose or oxidation in addition.In addition, separation solvent commonly used has certain toxicity, volatilizees for a long time in air, causes volatilization loss on the one hand, on the other hand, the healthy of operator is threatened.
Summary of the invention
The purpose of this invention is to provide a kind of solvent can circulate voluntarily, and can prevent substance oxidation, eco-friendly column chromatography device, to overcome the deficiencies in the prior art.
To achieve these goals, the technical solution used in the present invention is such:
A kind of column chromatography separating unit, comprise spherical condensation tube (1), serpentine condenser (2), chromatographic column (3), reaction vessel (4) and heater (5), wherein the outer grinding port of spherical condensation tube (1) bottom is connected with ground (11) in the serpentine condenser, serpentine condenser outer grinding port (14) is connected with ground (16) in the chromatographic column, and chromatographic column outer grinding port (23) is connected with reaction vessel (4); Chromatographic column cylinder (17) upper end upward is provided with the side pipe (7) that is communicated with between the edge with chromatographic column outer grinding port (23), and side pipe (7) middle part is provided with side pipe piston (18).
Described serpentine condenser (2) is embedded serpentine condenser, comprise ground (11), water inlet (13), delivery port (12), sleeve pipe (10), coiled pipe (15) and serpentine condenser outer grinding port (14) in the serpentine condenser, its middle sleeve (10) top closely is connected with the interior ground (11) of serpentine condenser, sleeve pipe (10) bottom is connected with the serpentine condenser outer grinding port (14) of water inlet (13) lower end, and the coiled pipe (15) that is connected with water inlet (13), delivery port (12) stretches outside serpentine condenser outer grinding port (14) is introversive.
Spherical condensation tube of the present invention (1), serpentine condenser (2), chromatographic column (3) and reaction vessel (4) cooperatively interact by ground and form the separation facility of chromatography of a cover relative closure, its operation principle is as follows: at first, eluant, eluent in the chromatographic column (3) flows into reaction vessel (4) with the portioned product that elutes, under heater (5) heating, eluant, eluent steam enters side pipe (7), eluant, eluent steam by side pipe (7) enters chromatographic column cylinder (17) upper end, steam and serpentine condenser (2) heat exchange condensation, part is spherical condensation tube (1) the further condensation of eluant, eluent by serpentine condenser (2) top of in time condensation not, so that the eluant, eluent droplets fall of condensation to condenser pipe when bottom temperature near room temperature, spherical condensation tube (1) topmost available absorbent cotton clogs, and prevents that airborne steam and dust granule from entering tomographic system.By regulating heating-up temperature, can guarantee the eluant, eluent submergence filler (19) in the chromatographic column (3), prevent dried post and avoided frequently replenishing eluant, eluent.Reaction vessel (4) also can be by the automatic suction loss of negative pressure of vacuum eluant, eluent or change another eluant, eluent.
Different from conventional column chromatography device, major advantage of the present invention is: the present invention collects mixture separation, simmer down to one.Because each junction adopts ground to connect, can in the pipeline of a relative closure, realize the separation of mixture and concentrated, reduce easy oxidation, easy contacting of decomposed substance and air, prevent the pollution of the environment in the time of the minimizing solvent loss.Realize in addition the cycling of eluant, eluent, avoided manually replenishing continually eluant, eluent, effectively prevented the generation of dried post.Whole system can be realized continuous operation, is beneficial to environmental protection, and is simple and practical.
Description of drawings
Fig. 1 is the component drawings of column chromatography separating unit of the present invention;
Fig. 2 is the assembling schematic diagram of column chromatography separating unit of the present invention;
Fig. 3 is the inner cased type serpentine condenser schematic diagram of column chromatography separating unit of the present invention;
Fig. 4 is conventional serpentine condenser schematic diagram;
Fig. 5 is the chromatographic column schematic diagram of column chromatography separating unit of the present invention;
Fig. 6 is conventional chromatographic column schematic diagram;
Fig. 7 is the TIC of eluate.
Among the upper figure, 1-spherical condensation tube, 2-serpentine condenser, 3-chromatographic column, 4-reaction vessel, 5-heater, 6-vavuum pump, 7-side pipe, 8-charging aperture, 9-vacuum orifice, ground in the 10-sleeve pipe, 11-serpentine condenser, 12-delivery port, 13-water inlet, 14-serpentine condenser outer grinding port, 15-coiled pipe, ground in 16-chromatographic column, 17-cylinder, 18-side pipe piston, 19-filler, 20-core baffle plate, 21-dropping liquid piston, 22-minim pipette, 23-chromatographic column outer grinding port.
The specific embodiment
The invention will be further described below in conjunction with accompanying drawing.
As shown in Figure 1, 2, column chromatography separating unit of the present invention comprises spherical condensation tube (1), serpentine condenser (2), chromatographic column (3), reaction vessel (4) and heater (5), but each several part complements each other to form the relatively column chromatography system of the continued operation of sealing of a cover by ground, wherein the outer grinding port of spherical condensation tube (1) bottom is connected with ground (11) in the serpentine condenser, serpentine condenser outer grinding port (14) is connected with ground (16) in the chromatographic column, and chromatographic column outer grinding port (23) is connected with reaction vessel (4); Reaction vessel (4) can be there-necked flask, and it comprises charging aperture (8) and vacuum orifice (9) and evaporation mouth middle and that chromatographic column cooperatively interacts, and heater (5) is thermostat water bath or electric heating cover.
Shown in Fig. 5,6, the present invention is different from conventional column chromatography device to a great extent, and conventional column chromatography device is mainly a cylindric uncovered chromatographic column, and the chromatographic column of all size is arranged on the market.Pillar is long, and the corresponding number of plates is just high, separates all rightly, and its blade diameter length ratio is generally in 1:5～10.Core baffle plate (20) and dropping liquid piston (21) are arranged at the chromatographic column bottom.Core baffle plate (20) filters the solid particle in the eluant, eluent in order to support filler (19).Dropping liquid piston (21) has glass material and polytetrafluoroethylene (PTFE) material.Conventional column chromatography device can be transformed into pressurization and chromatography device with negative pressure as required, but no matter normal pressure, pressurization or negative pressure, exist all that eluant, eluent volatilization loss is serious, easily oxidation, easily decomposed substance and air Long contact time generation oxidation, need frequent replenish eluant, eluent, easy dried post and separate rear product need the further shortcoming such as concentrated.
The present invention is provided with the side pipe (7) that is communicated with in chromatographic column cylinder (17) upper end with between the upper edge of outer grinding port (23), and side pipe (7) middle part is provided with side pipe piston (18), and this design can form cover column chromatography system relatively sealing, continued operation.
Such as Fig. 3, shown in 4, serpentine condenser of the present invention (2) is embedded serpentine condenser, comprise ground (11) in the serpentine condenser, water inlet (13), delivery port (12), sleeve pipe (10), coiled pipe (15) and serpentine condenser outer grinding port (14), its middle sleeve (10) top closely is connected with the interior ground (11) of serpentine condenser, sleeve pipe (10) bottom is connected with the serpentine condenser outer grinding port (14) of water inlet (13) lower end, with water inlet (13), the coiled pipe (15) that delivery port (12) connects stretches outside serpentine condenser outer grinding port (14) is introversive.
During use, eluant, eluent in the chromatographic column (3) enters there-necked flask with the product that elutes on a small quantity by minim pipette (22), product is concentrated in there-necked flask, eluant, eluent then enters side pipe (7) by water-bath or the continuous heating evaporation of electric heating cover, the upper port that enters chromatographic column (3) by side pipe (7) eluant, eluent steam, with serpentine condenser (2) heat exchange condensation, the eluant, eluent of in time condensation is not by further condensation of spherical condensation tube (1).Like this, as long as by regulating the water-bath heating-up temperature, the eluant, eluent liquid level in the chromatographic column (3) can keep the submergence filler always, prevents dried post, avoids the artificial frequent eluant, eluent that replenishes.Close side pipe piston (18) and dropping liquid piston (21), can discharge eluate with vavuum pump (6) pressurization, when vacuumizing, vacuum causes the interior negative pressure of there-necked flask from the eluant, eluent of the automatic suction loss of charging aperture or changes another eluant, eluent.
Adopt the method for column chromatography, the selection n-hexane is eluant, eluent, and silica gel separates the neutral organic compound in the coal tar as adsorbent.For effect of the present invention is described, example adopts respectively column chromatography separating unit of the present invention (Fig. 2) and conventional post separation facility of chromatography (Fig. 6) to carry out separation test, for can accurate analysis the separated product of two covering devices relatively, adopt gas chromatograph-mass spectrometer (GC-MS) that separated product is formed and content is measured.
Experimental raw is to take from the coal tar of Fugu County, northern Shensi blue charcoal factory, and the fundamental property that heavy oil (tar depositing reservoir subsurface layer oil) is measured by GB sees Table 1.
As shown in Figure 2, take by weighing respectively 100g silica gel (column chromatography silica gel special, 60-100 order, activation 2h), in the chromatographic column of packing into (wet method dress post, solvent uses 200mL); Take by weighing respectively heavy oil 2.5g and silica gel 5g, add and be equipped with in the beaker of 10ml n-hexane, ultrasonic radiation 20min, the slip that mixes insert and steam in the Rotary Evaporators to silica gel not till the wall built-up, and the silica gel that absorption is had heavy oil slowly uniformly adding has been filled in the chromatographic column Silica Surface of post; With the 100ml n-hexane there-necked flask of packing into, add a small amount of zeolite, then as shown in Figure 2, the erection column chromatographic apparatus, open condensed water, with water-bath or electric heating cover heating there-necked flask, be the temperature of being a bit larger tham the n-hexane boiling point with adjustment, at this moment, dropping liquid piston (21) is in closed condition, side pipe piston (18) is in open mode, treat that chromatographic column has liquid with return line flow lower time, open dropping liquid piston (21), regulate wash-out required drip speed (this experiment 1 second 3), at this moment, the liquid level of chromatographic column is kept certain height.
For shown in Figure 6, dropping liquid piston (21) regulate to drip speed, collects eluant, eluent, along with the decline of liquid level in the post need to replenish eluant, eluent in certain time interval.
This test elution time is 12h, end to be tested, close side pipe piston (18) and dropping liquid piston (21), open vavuum pump, in there-necked flask, blast gas, the there-necked flask internal pressure raises, and can the mixed liquor of eluant, eluent and product be discharged the about 100mL of eluant, eluent and product by charging aperture (8); The eluant, eluent and the about 8L of product that are eluted by Fig. 6 device.To place Rotary Evaporators from the mixture that stream oriented device obtains respectively, concentrate, use again the acetone solution of 5mL, and then carry out GC-MS and analyze.
Can be found by Fig. 7 analysis result, adopt column chromatography separating unit of the present invention and conventional post chromatographic apparatus, can obtain identical experimental result, but adopt the present invention can greatly reduce the consumption of eluant, eluent, conventional amount is 8L, and the present invention only needs 300mL(to comprise the used solvent of wet method dress post) solvent, simultaneously, this invention effectively prevents the volatilization of organic solvent, thereby reduces in the experimentation health hazard to the operator.
Claims (2)
1. column chromatography separating unit, it is characterized in that comprising spherical condensation tube (1), serpentine condenser (2), chromatographic column (3), reaction vessel (4) and heater (5), wherein the outer grinding port of spherical condensation tube (1) bottom is connected with ground (11) in the serpentine condenser, serpentine condenser outer grinding port (14) is connected with ground (16) in the chromatographic column, and chromatographic column outer grinding port (23) is connected with reaction vessel (4); Chromatographic column cylinder (17) upper end upward is provided with the side pipe (7) that is communicated with between the edge with chromatographic column outer grinding port (23); Described serpentine condenser (2) is embedded serpentine condenser, comprise ground (11), water inlet (13), delivery port (12), sleeve pipe (10), coiled pipe (15) and serpentine condenser outer grinding port (14) in the serpentine condenser, its middle sleeve (10) top closely is connected with the interior ground (11) of serpentine condenser, sleeve pipe (10) bottom is connected with the serpentine condenser outer grinding port (14) of water inlet (13) lower end, and the coiled pipe (15) that is connected with water inlet (13), delivery port (12) stretches outside serpentine condenser outer grinding port (14) is introversive.
2. column chromatography separating unit according to claim 1 is characterized in that: be provided with side pipe piston (18) in the middle part of the side pipe (7).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110077072 CN102218225B (en) | 2011-03-30 | 2011-03-30 | Column chromatography separating unit |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110077072 CN102218225B (en) | 2011-03-30 | 2011-03-30 | Column chromatography separating unit |
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| CN102218225A CN102218225A (en) | 2011-10-19 |
| CN102218225B true CN102218225B (en) | 2013-01-30 |
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| CN 201110077072 Expired - Fee Related CN102218225B (en) | 2011-03-30 | 2011-03-30 | Column chromatography separating unit |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104845651A (en) * | 2015-06-10 | 2015-08-19 | 神华集团有限责任公司 | Method of separating components of coal tar |
| CN105368473A (en) * | 2015-11-03 | 2016-03-02 | 西北大学 | Device and process for separating coal tar components |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201115795Y (en) * | 2007-09-30 | 2008-09-17 | 贵州省中国科学院天然产物化学重点实验室 | Novel chromatographic column |
| CN201346409Y (en) * | 2008-08-15 | 2009-11-18 | 华南师范大学 | Controllable pressurizing chromatographic separation column |
| CN201470151U (en) * | 2009-07-08 | 2010-05-19 | 胡彦涛 | Novel chromatographic device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2584372A1 (en) * | 2004-11-04 | 2006-05-11 | Bio-Rad Pasteur | Stackable chromatography module and chromatography column comprising a stack of such modules |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201115795Y (en) * | 2007-09-30 | 2008-09-17 | 贵州省中国科学院天然产物化学重点实验室 | Novel chromatographic column |
| CN201346409Y (en) * | 2008-08-15 | 2009-11-18 | 华南师范大学 | Controllable pressurizing chromatographic separation column |
| CN201470151U (en) * | 2009-07-08 | 2010-05-19 | 胡彦涛 | Novel chromatographic device |
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Granted publication date: 20130130 Termination date: 20140330 |