CN107413072A - Modular multistage chromatographic column and its sampling, separation method - Google Patents
Modular multistage chromatographic column and its sampling, separation method Download PDFInfo
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- CN107413072A CN107413072A CN201710734224.9A CN201710734224A CN107413072A CN 107413072 A CN107413072 A CN 107413072A CN 201710734224 A CN201710734224 A CN 201710734224A CN 107413072 A CN107413072 A CN 107413072A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
- B01D15/1864—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns using two or more columns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
Abstract
The present invention provides a kind of modular multistage chromatographic column and its sampling, separation method, modular multistage chromatographic column includes from top to bottom the capital of nesting, at least a segmented column body and post bottom successively, a capital sampling aperture is through with the nested face of capital, a top sampling aperture is through with the nested face of cylinder upper end, a bottom sampling aperture is through with the nested face of cylinder lower end, cylinder bottom is provided with core, and a post bottom sampling aperture is through with the nested face at post bottom.Compared with prior art, the beneficial effects of the invention are as follows：During separating-purifying, situation can be separated in chromatographic column to monitor, realizes dynamic monitoring in real time to being sampled in post；It can also flexibly select to increase or reduce cylinder number as needed；When different components are separated in cylinder, the cylinder with different components can be separated, be combined respectively with capital and post bottom, be assembled into branched chromatographic column and use；With practical, flexibility is high, it is widely applicable the characteristics of.
Description
Technical field
, can real time sample to liquid in post the present invention relates to a kind of modular multistage chromatographic column and its sampling, separation method
Analysis, the chromatographic column of separable independent assortment, it is mainly used in separating-purifying in chemical experiment, especially in Experiment of Organic Chemistry
In, it will use more extensive.
Background technology
At present, in organic chemical synthesis laboratory, the chromatographic column that is typically used for, capital, cylinder and post bottom are one whole
Body, it is inseparable, column body liquid sampling can not be analyzed；Pillar height is fixed and specification is various.These chromatographic columns were using
Cheng Zhong, there is many weak points, during separating-purifying, to component in post can not sampling analysis, post bottom can only be passed through
The whether isolated pure compound of liquid outlet sampling analysis, separation process is full of uncertain and pure for not separating
Mixed composition is felt simply helpless, and separating-purifying, waste ample resources and human cost, extreme influence separating-purifying can only be imitated again
Rate；When separating the big compound component of two kinds of different polarities, when isolating the small component of polarity, can not immediately by top not
The component of expansion elutes entirely to be filled pillar height degree, is separated from liquid outlet, it is necessary to cover top component using a large amount of eluant, eluents,
A large amount of eluant, eluents are expended, it is not economic and environment-friendly enough；In compound, particularly isomer similar in separating polar, it is difficult to point
From again increase pillar height is limited by chromatographic column height, the higher chromatographic column of customization, expends great amount of cost, and utilization rate is not high, also
Limited by operation field, operation difficulty is big.Disadvantages described above determine current chromatographic column can not economic and environment-friendly, efficient energy-saving, pole is not
Adapt to current increasingly sophisticated separation system.
As the requirement to chromatography improves constantly, the improvement to chromatographic column also gradually increases, such as：For flexibly setting
The height of separation process chromatographic column and adsorbent, CN201320200721.8 disclose a kind of combined type chromatographic column, but its
Cylinder number can only be freely configured before separating-purifying operation to be used；In order to save the dosage of eluant, eluent, sample is improved
Yield, CN201521102771.8 discloses a kind of combined type chromatography column, but it is not solved in cylinder separation process
It is preceding how more effective determination separate in cylinder whether isolated pure compound；In order to realize that cylinder separates, enter simultaneously
Row elution separation respectively, CN201420693338.5 discloses a kind of detachable more piece chromatographic column, but it can not accurately be detected
Whether component is segregated into different post sections in post, and is difficult to during separating-purifying to overcome huge vacuum pressure to fill
The chromatography post separation of full liquid, and need to take out filler in single-stage cylinder in eluted product respectively, increase operating procedure.It is comprehensive
Analysis is closed, can be detected in time during chromatographic column separating-purifying to separating situation in post without a kind of scheme well, root
Carrying out cylinder separation according to detection and analysis result, elution or increase and decrease cylinder number continue purification ＆ isolation respectively.
Therefore, to meet the sampling and cylinder separation during chromatography compound, a kind of new analysis point is designed
It is very necessary from scheme.
The content of the invention
The problem of existing for background technology, the present invention provide a kind of practical, flexibility height, and strong operability is widely applicable
Chromatographic column.
What the present invention was realized in：Modular multistage chromatographic column, including nested capital, at least one successively from top to bottom
Segmented column body and post bottom, the nested face that the nested place between capital, cylinder and post bottom cooperates is frosting, capital be provided with into
Sample mouth, post is beneath to be provided with liquid outlet, and liquid outlet is provided with control valve, and it is small that a capital sampling is through with the nested face of capital
Hole, a top sampling aperture is through with the nested face of cylinder upper end, a bottom is through with the nested face of cylinder lower end
Aperture is sampled, the top that cylinder bottom is located at bottom sampling aperture is provided with core, a post bottom is through with the nested face at post bottom
Aperture is sampled, can be communicated between capital sampling aperture and top sampling aperture by rotating capital with the relative position of cylinder or not
Communicate, pass through the relative position between rotating cylinder between the bottom sampling aperture of upper segmented column body and the top sampling aperture of lower segmented column body
Put and communicate or be not communicated with, bottom samples can be by rotating cylinder and the relative position phase at post bottom between aperture and post bottom sampling aperture
Lead to or be not communicated with.
Vacuum silicon grease is coated between frosting at nesting.
Capital sampling aperture, top sampling aperture, bottom sampling aperture and post bottom sample the aperture all same of aperture.
The diameter of core and the internal diameter of cylinder match.
Grinding port plug is detachably connected on injection port.
The sampling method of modular multistage chromatographic column, it is divided into normal pressure sampling and sampling below atmospheric pressure in post in post；Normal pressure takes in post
Sample makes the upper of the bottom sampling aperture of upper segmented column body and lower segmented column body by rotating the relative position of the body of segmented column up and down at nested place
Portion samples apertures align, and liquid is flowed out due to pressure in post, is sampled；Sampling below atmospheric pressure in post, in trabeation before sampling
It is closed plus a corresponding grinding port plug at nesting, then continue to flow out solvent at the liquid outlet of post bottom, when post bottom liquid outlet liquid
When body slowly drips, that is, the control valve at post bottom is closed, rotate double sectioned column body up and down, above solvent outside negative pressure and cavity and sampling aperture
Slow down solvent discharge rate at sampling aperture under the collective effect of portion's atmospheric pressure, the trace solvent of sampling aperture outflow can be carried out
Sampling.
The separation method of modular multistage chromatographic column, before cylinder separation, the grinding port plug in capital plus sealing, while make
Liquid outlet solvent is continued to flow out to the complete control valve for stopping, now closing post bottom, by the sampling aperture of every one-level and air
Communicate, air is now had at sampling aperture and is entered at the nesting below core, you can the part that will be sampled above aperture is overall
Separate, solvent more than core can be because of the surface tension at core and the suction function above liquid without flowing out, i.e.,
Cylinder can be freely separating or be combined.
Compared with prior art, the beneficial effects of the invention are as follows：Dynamic monitoring is carried out to post internal solvent separate substance situation, can be certainly
Cylinder is combined by separation, is assembled into branched chromatographic column, increases and decreases pillar height；In the case where not influenceing conventional pressurized decompression separation, tool
Have practical, flexibility is high, and strong operability is widely applicable, disclosure satisfy that increasingly complicated and diversified organic matter separation needs.
Brief description of the drawings
Fig. 1 is the structural representation of capital；
Fig. 2 is the structural representation of cylinder；
Fig. 3 is the structural representation at post bottom；
Fig. 4 is the modular multistage chromatographic column and its sampling, the structural representation of separation method for including three section chromatographic columns；
Fig. 5 is the structural representation when thief hole in Fig. 4 at E sections is not communicated with；
Fig. 6 is the structural representation when thief hole in Fig. 4 at E sections communicates.
Wherein, 1- capitals, 2- cylinders, 3- posts bottom, 4- injection ports, 5- liquid outlets, 6- control valves, 7- capitals sampling aperture,
8- tops sample aperture, 9- bottoms sampling aperture, 10- posts bottom sampling aperture, 11- cores.
Specific embodiment
In order that the object, technical solutions and advantages of the present invention are more clearly understood, below in conjunction with drawings and Examples pair
The present invention is described in further details.
The problem of existing for background technology, the present invention provide a kind of practical, flexibility height, and strong operability is applicable
Wide chromatographic column, there is provided during chromatography, the monitoring project and cylinder of analysis are sampled to component in post
Separate and freely assemble the scheme of combination.
Figure is included with lower component：Capital 1, cylinder 2, post bottom 3, injection port 4, liquid outlet 5, control valve 6, capital sampling are small
Hole 7, top sampling aperture 8, bottom sampling aperture 9, post bottom sampling aperture 10 and core 11.
As shown in figures 1 to 6, modular multistage chromatographic column and its sampling, separation method, including it is nested successively from top to bottom
Capital, at least a segmented column body and post bottom, the nested face that the nested place between capital, cylinder and post bottom cooperates is frosting,
Capital is provided with injection port, is provided with liquid outlet under post, liquid outlet is provided with control valve, one is through with the nested face of capital
Capital samples aperture, and a top sampling aperture is through with the nested face of cylinder upper end, is penetrated on the nested face of cylinder lower end
There is a bottom sampling aperture, the top that cylinder bottom is located at bottom sampling aperture is provided with core, penetrated on the nested face at post bottom
There is post bottom sampling aperture, can be by rotating the relative position of capital and cylinder between capital sampling aperture and top sampling aperture
Put and communicate or be not communicated with, pass through rotating cylinder between the bottom sampling aperture of upper segmented column body and the top sampling aperture of lower segmented column body
Between relative position communicate or be not communicated with, can pass through rotating cylinder and post bottom between bottom sampling aperture and post bottom sampling aperture
Relative position is communicated or is not communicated with.
Vacuum silicon grease is coated between frosting at nesting.
Capital sampling aperture, top sampling aperture, bottom sampling aperture and post bottom sample the aperture all same of aperture.
The diameter of core and the internal diameter of cylinder match.
Grinding port plug is detachably connected on injection port.
The sampling method of modular multistage chromatographic column, it is divided into normal pressure sampling and sampling below atmospheric pressure in post in post；Normal pressure takes in post
Sample makes the upper of the bottom sampling aperture of upper segmented column body and lower segmented column body by rotating the relative position of the body of segmented column up and down at nested place
Portion samples apertures align, and liquid is flowed out due to pressure in post, is sampled；Sampling below atmospheric pressure in post, in trabeation before sampling
It is closed plus a corresponding grinding port plug at nesting, then continue to flow out solvent at the liquid outlet of post bottom, when post bottom liquid outlet liquid
When body slowly drips, that is, the control valve at post bottom is closed, rotate double sectioned column body up and down, above solvent outside negative pressure and cavity and sampling aperture
Slow down solvent discharge rate at sampling aperture under the collective effect of portion's atmospheric pressure, the trace solvent of sampling aperture outflow can be carried out
Sampling.
The separation method of modular multistage chromatographic column, before cylinder separation, the grinding port plug in capital plus sealing, while make
Liquid outlet solvent is continued to flow out to the complete control valve for stopping, now closing post bottom, by the sampling aperture of every one-level and air
Communicate, air is now had at sampling aperture and is entered at the nesting below core, you can the part that will be sampled above aperture is overall
Separate, solvent more than core can be because of the surface tension at core and the suction function above liquid without flowing out, i.e.,
Cylinder can be freely separating or be combined.
Embodiment
Each segmented column body individually can be assembled into a chromatographic column with capital and post bottom, also can be by more piece cylinder and post
Top, post bottom are applied in combination；The position of the sampling aperture at adjacent columns nesting can also be adjusted in use, be sampled
Analysis, realizes dynamic detection, according to the requirement of sampling process, can carry out in the post to a small amount of loss of solvent normal pressure sampling and molten
Sampling below atmospheric pressure in the post of agent insubstantial loss；It can also separate cylinder during separating-purifying, be respectively self-assembled into new chromatography
Post, respectively elution separation；The cylinder of component can not also be being separated, reduce cylinder number of the top without component, increase lower section is filled out
The cylinder number of separation material is filled, flexibly tackles produced problem during separating-purifying.
Embodiment 1：Normal pressure samples in dynamic monitoring-post
Normal pressure sampling makes upper section using the principle of liquid pressure by the relative position for rotating the body of segmented column up and down at nesting in post
The top of the bottom sampling aperture and lower segmented column body of cylinder samples apertures align, and liquid is flowed out due to pressure in post, is taken
It sample, to reduce solvent loss, need to quickly rotate, reduce the time of two sampling aperture faces.
As shown in figure 4, so that 3 segmented column bodies are combined into a three-level chromatographic column as an example, its Section 2 cylinder and Section 3 cylinder
Profile at nesting is shown in Fig. 5.The present embodiment includes：The segmented column body 2 of capital 1,3 and post bottom 3, each intermodule are handled by frosted
Nested surface cover connects guarantee sealing, and lubricant, such as vacuum silicon grease are smeared between nested face, and vacuum silicon grease can both ensure air-tightness
And can ensures freely relatively rotate between each module, does not influence to separate.
As shown in Figure 5 and Figure 6, the separation situation to Section 2 cylinder is sampled analysis, directly passes through fixed Section 3 post
Body and following part, rotating the part of Section 2 cylinder and the above makes the bottom of Section 2 cylinder sample aperture 9 and Section 3 cylinder
Top sampling aperture 8 it is relative, now cylinder is sampled at aperture and communicated with air herein, and post internal solvent is in the case where fluid pressure acts on
From sampling aperture outflow, you can to carrying out solvent sampling herein.
To down-sample the solvent loss to chromatography, the time for shortening two sampling aperture faces need to be quickly rotated.
Embodiment 2：Sampling below atmospheric pressure in dynamic monitoring-post
Sampling below atmospheric pressure in post, it is closed plus a corresponding grinding port plug at trabeation nesting before sampling, then go out post bottom
Solvent continues to flow out at liquid mouth, and now cavity produces negative pressure above chromatographic column internal solvent, and when post bottom, liquid outlet liquid slowly drips
When, that is, the control valve at post bottom is closed, now, pressure caused by the negative pressure of cavity is enough to balance most solvent above solvent
Gravity, if making the inside and outside sampling aperture at nesting relative, communicated with air, negative pressure and cavity and sampling aperture outside are big above solvent
Slow down solvent discharge rate at sampling aperture under the collective effect of air pressure, it is quick to rotate double sectioned column body up and down, can be to sampling aperture
The trace solvent of outflow is sampled analysis.
Grinding port plug is added at the injection port 4 of capital 1 before sampling, the sealing of cylinder is realized, allows post internal solvent to continue to flow
Go out, Section 1 cylinder solvent upper cavity is produced negative pressure because solvent is reduced, when the solvent of liquid outlet 5 at post bottom 3 slowly drips,
Counteracted by pressure caused by negative pressure in the cavity of solvent top is fallen most solvent gravity, now repeat above-mentioned sampling operation, i.e.,
Substantially less solvent flux at aperture can be sampled, reach the purpose for controlling solvent loss.
According to aforesaid operations, you can to being sampled analysis at each sampling aperture of more piece chromatographic column cylinder, to reach
The purpose of dynamic monitoring.
Embodiment 3：Independent assortment-cylinder separation
Before cylinder separation, the grinding port plug in capital plus sealing, while make to continue to flow out to complete in liquid outlet solvent and stop, i.e.,
It can form complete negative pressure above liquid in post, the gravitational equilibrium of pressure difference caused by negative pressure and whole chromatographic column liquid in post,
The control valve at post bottom is now closed, when being communicated at the sampling aperture per one-level with air, it is big to sample the pressure difference formed at aperture
Liquid gravity above sampling aperture, air is now had at sampling aperture and is entered at the nesting below core, you can will be taken
Part overall separation above sample aperture is opened, and solvent more than core can be because of negative above the surface tension at core and liquid
Pressure is acted on without flowing out, and so can be achieved with chromatographic column is freely separating combination, elutes respectively, and increase reduces pillar height etc. flexibly
Operation.
Equally by Section 2 cylinder with exemplified by the nested place of Section 3 cylinder, double sectioned column body is separated, referring to above-mentioned sampling below atmospheric pressure
Operate, under similarity condition, grinding port plug is added at the injection port of capital 1, the sealing of cylinder is realized, allows post internal solvent to continue to flow out
Stop to complete, pressure caused by negative pressure caused by the cavity of solvent top is reached balance with solvent gravity, now rotate Section 3
The upper section of cylinder, make sampling aperture relative, and communicated with air, due to negative pressure caused by post internal cavity and whole branch chromatographic column
Internal solvent balances, therefore pressure caused by its negative pressure is more than the gravity of solvent above sampling aperture, and air enters column body sand
Below core, and solvent more than core will not continue to flow out, now and separable Section 2 cylinder and Section 3 cylinder.
Three-level chromatographic column is divided into two parts up and down, former capital and the 1st, 2 segmented column bodies combine with 1 new post bottom can be again
A new chromatographic column is assembled into, 1 new capital is combined with Section 3 cylinder and former post bottom can be assembled into the new chromatography of another
Post；Can also be further added by as needed between Section 3 cylinder and former post bottom separated a section or the populated filler of more piece and
The cylinder of solvent, assemble continuation chromatography.The purpose of chromatographic column cylinder separation and independent assortment can thus be reached.
These are only presently preferred embodiments of the present invention, not to limit the present invention, all spirit in the present invention and
The all any modification, equivalent and improvement made in principle, should be included within the scope of the present invention.
Claims (7)
1. modular multistage chromatographic column, including nested capital, at least a segmented column body and post bottom successively from top to bottom, capital, post
The nested face that nested place between body and post bottom cooperates is frosting, and capital is provided with injection port, liquid is provided with out under post
Mouthful, liquid outlet is provided with control valve, it is characterised in that：Sampling aperture in capital is through with the nested face of capital, on cylinder
A top sampling aperture is through with the nested face at end, a bottom sampling aperture is through with the nested face of cylinder lower end,
The top that cylinder bottom is located at bottom sampling aperture is provided with core, and a post bottom sampling aperture is through with the nested face at post bottom,
Capital samples between aperture samples aperture with top and can communicated or be not communicated with the relative position of cylinder by rotating capital, upper section
Cylinder bottom sampling aperture and lower segmented column body top sampling aperture between communicated by the relative position between rotating cylinder or
It is not communicated with, can be communicated between bottom sampling aperture and post bottom sampling aperture by rotating cylinder with the relative position at post bottom or not phase
It is logical.
2. modular multistage chromatographic column according to claim 1, it is characterised in that：It is coated between frosting at nesting true
Empty silicone grease.
3. modular multistage chromatographic column according to claim 1, it is characterised in that：Capital sampling aperture, top sampling are small
The aperture all same in hole, bottom sampling aperture and post bottom sampling aperture.
4. modular multistage chromatographic column according to claim 1, it is characterised in that：The internal diameter phase of the diameter of core and cylinder
Matching.
5. modular multistage chromatographic column according to claim 1, it is characterised in that：Ground is detachably connected on injection port
Plug.
6. the sampling method of modular multistage chromatographic column according to claim 1, it is characterised in that：It is divided into normal pressure in post to take
Sampling below atmospheric pressure in sample and post；Normal pressure sampling makes upper segmented column body by rotating the relative position of the body of segmented column up and down at nesting in post
Bottom samples the top sampling apertures align of aperture and lower segmented column body, and liquid is flowed out due to pressure in post, is sampled；In post
Sampling below atmospheric pressure, it is closed plus a corresponding grinding port plug at trabeation nesting before sampling, then make molten at the liquid outlet of post bottom
Agent continues to flow out, and when liquid outlet liquid slowly drips when post bottom, that is, closes the control valve at post bottom, rotates double sectioned column body up and down, molten
Slow down solvent discharge rate at sampling aperture above agent under the collective effect of negative pressure and cavity and sampling aperture external pressure, can be right
The trace solvent of sampling aperture outflow is sampled.
7. the separation method of modular multistage chromatographic column according to claim 1, it is characterised in that：Before cylinder separation,
Capital makes to continue to flow out to the complete control for stopping, now closing post bottom in liquid outlet solvent plus the grinding port plug sealed
It valve, will be communicated at the sampling aperture of every one-level with air, air now had at sampling aperture and is entered at the nesting below core,
The part overall separation sampled above aperture can be opened, solvent more than core can be because of surface tension and liquid at core
The suction function of top is without flowing out, you can cylinder is freely separating or combined.
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| CN108165759A (en) * | 2018-01-30 | 2018-06-15 | 芒市海华开发有限公司 | A kind of combined type desorption column |
| WO2020258705A1 (en) * | 2019-06-28 | 2020-12-30 | 信达生物制药(苏州)有限公司 | Modular chromatography device |
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