CN105570493B - A kind of multiple valve and chromatographic column - Google Patents

A kind of multiple valve and chromatographic column Download PDF

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Publication number
CN105570493B
CN105570493B CN201610081487.XA CN201610081487A CN105570493B CN 105570493 B CN105570493 B CN 105570493B CN 201610081487 A CN201610081487 A CN 201610081487A CN 105570493 B CN105570493 B CN 105570493B
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Prior art keywords
valve
column
sieve plate
internal cavity
valve body
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CN105570493A (en
Inventor
崔万臣
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Beijing Chuangxin Tongheng Science and Technology Co Ltd
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Beijing Chuangxin Tongheng Science and Technology Co Ltd
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K11/00Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves
    • F16K11/02Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves with all movable sealing faces moving as one unit
    • F16K11/04Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves with all movable sealing faces moving as one unit comprising only lift valves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/60Construction of the column
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/60Construction of the column
    • G01N30/6004Construction of the column end pieces

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Pathology (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Immunology (AREA)
  • Mechanical Engineering (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The present invention provides a kind of multiple valve, which includes valve body, valve rod;Concentric inside and outside cavity up and down is arranged in the valve body, the valve rod is set to the internal cavity of the valve body, and controls the folding of the internal cavity.The present invention also provides the chromatographic columns including the multiple valve.The present invention improves the cleaning performance of chromatographic column, and easy to operate.

Description

A kind of multiple valve and chromatographic column
Technical field
The present invention relates to preparing chromatograph in industry fields, specifically, are related to a kind of multiple valve and chromatographic column.
Background technology
The main purpose of preparing chromatograph in industry is that pure material is obtained from mixture, and current industrial prepares the color that chromatography uses Compose the tubular body that column is typically vertical.In tubular body filler and inject solvent carry out chromatography preparation.In existing low-pressure chromatography In column purification separation production, generally use major diameter, the chromatographic column of low clearance.
There are mainly two types of modes for the loading of filler in the prior art:1) lid non-central location opens hole on a column, By pipeline be pumped into or vacuum suck chromatographic column in;2) in the lower section of top end sieve plate, vial wall lateral opening hole passes through pipeline pump Enter or vacuum suck chromatographic column in.There are larger drawbacks for this kind of mode:1) top drilling in order to avoid follow-up solvent injection not Middle position can be opened in, the filler secundly being pumped into can be caused to fall in this way, the filler surface after filling have gradient or on Protrusion eventually influences the effect isolated and purified;2) side openings there is a problem of same and more obvious, and more major diameter Chromatographic column can influence to aggravate.
The discharge of filler also mainly uses two ways in the prior art:1) in chromatographic column lower cover (containing sieve plate) non-central position It sets and opens hole, used in pump or vacuum suck chromatographic column by pipeline;2) in the top of column bottom end sieve plate, vial wall side is opened Hole is used by pipeline in pump or vacuum suck chromatographic column.Discharge mode is arranged that there is also very big drawbacks:1) column tube side wall is opened Hole or lower sieve plate trepanning will produce certain dead volume, can not clean to remaining filler in hole well in technical process The sample or impurity of absorption can not be accomplished thoroughly to clean;2) trepanning on lower sieve plate can not make the eluent on hole top at this Smoothly outflow, meeting strong influence separating effect, product elution generate trailing phenomenon, and yield substantially reduces, and solvent consumption increases.
Invention content
In order to overcome above-mentioned technical problem, the purpose of the present invention is to provide a kind of multiple valves, improve chromatographic column Cleaning performance, and it is easy to operate.
Another object of the present invention is to provide a kind of chromatographic columns including the multiple valve.
To achieve the goals above, the present invention provides a kind of multiple valves, including:
Valve body, valve rod;
Concentric inside and outside cavity up and down is arranged in the valve body, the valve rod is set to the interior sky of the valve body Chamber, and control the folding of the internal cavity.
In a kind of optional embodiment, the longitudinal profile of the tail portion opening of the internal cavity is inverted trapezoidal.
In a kind of optional embodiment, the external cavity is being equipped with the first entrance close to the tail portion of the valve body, It is being equipped with the second entrance close to the top of valve body.
In a kind of optional embodiment, the ratio of the diameter of the diameter of the valve body and the internal cavity is 5:1 to 50:1.
In a kind of optional embodiment, the end face that the valve rod is located at the tail portion opening of the internal cavity is sealing Face.
In a kind of optional embodiment, sieve plate is set in the sealing surface, is equipped with and connects in the stem internal center Sieve plate and the fluid passage of the valve rod is penetrated through in logical sealing surface.
In a kind of optional embodiment, the valve rod is manual rotation bar, Pneumatic lifting arm or hydraulic lifting arm.
The present invention also provides a kind of chromatographic column including multiple valve described in above-mentioned any one, which also wraps It includes:
Column sieve plate, the distributor being connected to external cavity, pressing plate, column tube;
The column sieve plate, the distributor and the pressing plate are bonded successively to be arranged in the column tube, the multiple valve It is set in the leakage hole of the column sieve plate, the distributor and the pressing plate centre.
In a kind of optional embodiment, the column sieve plate includes:
Sieve plate seat, several deck units;
The sieve plate seat is equipped with that several shapes are identical and the through-hole of equidistantly distributed, several described deck units and institute It states through-hole to match, be placed in the through-hole.
In a kind of optional embodiment, the cross section of the deck unit is circle, equilateral triangle, square, just Hexagon or octagon.
Multiple valve described in the embodiment of the present invention and the chromatographic column using the multiple valve, which includes valve body And valve rod, the cavity up and down of concentric inside and outside two is arranged in valve body, valve rod is set to the internal cavity of valve body, and in controlling The folding of cavity.The multiple valve is easy to control, multi-purpose valve, and filler can be realized by being equipped with the chromatographic column of the multiple valve It is carried out while outflow is with gas, liquid discrepancy chromatographic column, and more preferable to the cleaning performance inside chromatographic column.
Description of the drawings
Fig. 1 is the structural schematic diagram of the multiple valve under closed state provided in an embodiment of the present invention;
Fig. 2 is the structural schematic diagram of the multiple valve under open state provided in an embodiment of the present invention;
Fig. 3 is the structural schematic diagram of chromatographic column provided in an embodiment of the present invention;
Fig. 4 is the structural schematic diagram of column sieve plate provided in an embodiment of the present invention;
Fig. 5 is the structural schematic diagram of the multiple valve provided in an embodiment of the present invention with fluid passage.
Specific implementation mode
Below with reference to the accompanying drawings illustrate the embodiment of the present invention.It is retouched in the attached drawing of the present invention or a kind of embodiment The elements and features stated can be combined with elements and features shown in one or more other drawings or embodiments.It answers When note that for purposes of clarity, being omitted known to unrelated to the invention, those of ordinary skill in the art in attached drawing and explanation Component or processing expression and description.
The present invention is described further below in conjunction with the accompanying drawings.
An embodiment of the present invention provides a kind of multiple valves, as shown in Figure 1, the multiple valve 1 includes:
Valve body 11, valve rod 12.
Concentric internal cavity 111 and external cavity 112 are arranged in valve body 11.Internal cavity 111 and external cavity 112 are up and down The structure of perforation.Valve rod 12 is set in the internal cavity 111 of valve body 11, and controls the folding of internal cavity 111.
Specifically, the structure of internal cavity 111 up and down is:Internal cavity 111 forms tail portion in the tail portion of valve body 11 113 and opens Mouth 1111, and outlet 1112 is opened up near the top of valve body 11 114, to form inside up and down.
The structure of external cavity 112 up and down is specially:External cavity 112 is opened close to the position of the tail portion 113 of valve body 11 If the first entrance 1121, the second entrance 1122 is being opened up close to the position at the top 114 of valve body 11, to be formed on inside Lower perforation.In Fig. 1,4 to 32 equally distributed first entrances 1121 have schematically been symmetrical arranged and two second go out The set-up mode of entrance 1122, practical application split shed is not limited to this.
As shown in Figure 1, the top 121 of valve rod 12 passes through the top 114 of valve body 11, the end of valve rod 12 is end face 122. Preferably, the shape of the end face 122 is matched with the shape of the tail portion of valve body 11 opening 1111, specifically in Fig. 1, internal cavity The longitudinal profile of 111 tail portion opening 1111 can be inverted trapezoidal, the shape of the longitudinal profile of end face 122 be also inverted trapezoidal and with Tail portion opening 1111 longitudinal profile to coincide.
When valve rod 12 is moved to the tail portion 113 of valve body 11, the tail portion opening 1111 of valve body 11 is left in end face 122, makes interior Cavity 111 is opened, as shown in Figure 2.
When valve rod 12 is moved to the top 114 of valve body 11, end face 122 returns to the tail portion opening 1111 of valve body 11, makes interior Cavity 111 is closed, as shown in Figure 1.
Optionally, the ratio of the diameter of the diameter of valve body 11 and internal cavity 111 is 5 in the embodiment of the present invention:1 to 50:1.
Optionally, the end face 122 that valve rod 12 is located at tail portion opening 1111 is sealing surface.The end face 122 is sealed around, prevents Internal cavity 111 in off position when column in liquid through end face 122 enter internal cavity 111, pollute.
Further, as shown in figure 5, being provided with sieve plate 1221 in the sealing surface, and liquid is set in 12 center of inside of valve rod Body channel 123, sieve plate 1221 in fluid passage one end communication seals face, and run through valve rod 12, by sieve plate in sealing surface The liquid of 1221 filterings can be flowed out via fluid passage 123.
Valve rod 12 in the embodiment of the present invention can be manual rotation bar, Pneumatic lifting arm or hydraulic lifting arm.
The embodiment of the present invention additionally provides a kind of chromatographic column, as shown in figure 3, the chromatographic column includes multiple valve 1, column sieve plate 2, distributor 3, pressing plate 4 and column tube 5.
The structure of wherein multiple valve 1 can refer to the description of the embodiment of the present invention above, and details are not described herein again.
Column sieve plate 2, distributor 3 and pressing plate 4 are bonded successively to be arranged in column tube 5, and multiple valve 1 is set to column sieve plate 2, divides In the leakage hole of 4 centre of orchestration 3 and pressing plate.
In practical application scene, one group of column sieve plate 2, distributor can be respectively set on the column tube head of chromatographic column and bottom 3, the combination of pressing plate 4.
The column sieve plate 2 of the embodiment of the present invention includes:Sieve plate seat and several deck units.Wherein sieve plate seat is equipped with several Shape is identical and the through-hole of equidistantly distributed, several deck units are matched with through-hole, are placed in through-hole.Deck unit can Using materials such as nonmetallic or metals, for general pore size control at 1 micron to 100 microns, which can be such that liquid smoothly flows through.
The sieve plate seat of the embodiment of the present invention is in the form of annular discs, the cross section of deck unit be circle, equilateral triangle, square, Regular hexagon or octagon.Fig. 4 shows that a kind of shape and structure of column sieve plate, sieve plate seat 41 are discoid, deck unit 42 cross section is circle.
The deck unit that the embodiment of the present invention uses, since each deck unit diameter is smaller, non-deformability is aobvious It writes and reinforces, column sieve plate integrally has better crushing resistance.
Along its center, several fluid phase partitioning fluid path, each fluid phase partitioning liquid is arranged in tree-like diverging outward on the dispenser The end on road is arranged dispensing orifice, and the length of the fluid phase partitioning fluid path at the center of distributor to each dispensing orifice is identical, sieve plate seat Through-hole be oppositely arranged with dispensing orifice.About the detailed description of the distributor including fluid phase partitioning fluid path, can refer to ZL200910170013.2 patents provide a kind of mobile phase distributor of chromatographic column in the patent, which sets It sets in tubular body, column sieve plate is equipped on distributor.The distributor can make mobile phase equal with identical speed Even flows through entire column sieve plate, and mobile phase is made uniformly to be distributed.
As shown in Figures 2 and 3, the external cavity 112 in multiple valve 1 is connected to distributor 3, specifically, going out by first Entrance 1121 is connected to distributor 3.
The chromatographic column that multiple valve is carried in the embodiment of the present invention, comes in and goes out when liquid enters from top end in column by second Mouth 1122 enters gas and liquid, by the first entrance 1121 injection distributor 3 of external cavity 112, distributor 3 passes through stream Liquid is transported to corresponding deck unit central point by body phase partitioning fluid path, and by sub-distribution again, liquid uniformly passes through sieve plate Unit enters in column;When liquid is flowed out from column bottom end, liquid is collected to sieve plate after deck unit, by deck unit bottom end Unit center is collected to the central area of entire distributor by the fluid phase partitioning fluid path of distributor again, comes in and goes out by first Mouth 1121 flow to external cavity 112, is flowed out outside column using the second entrance 1122.
When moving up valve rod 12, sieve plate sealing surface is opened, and internal cavity 111 is opened, and the filler in column tube 5 is from internal cavity 111 outlet 1112 is discharged.Since chromatographic column is generally relatively large in diameter, and filler has been compacted during use before, is It can be good at excluding filler completely, can be passed through gas and pumping liquid simultaneously in the second entrance 1122 respectively will be in column Uniform filling jack-up is broken up, and then smoothly flows into internal cavity 111, is flowed out through outlet 1112.
When moving down valve rod 12, when internal cavity 111 is closed, sieve plate sealing surface and column sieve plate 2 are a planes.It sieves at this time Plate sealing surface can pass through liquid, and be flowed out by internal cavity 111.
Pressing plate 4 positioned at 5 bottom of column tube is further secured on blind flange.Blind flange plays the role of supporting column tube 5, 5 bottom of column tube and the junction of blind flange are additionally provided with flange.
Multiple valve provided in an embodiment of the present invention realizes multi-purpose valve, easy to operate, can control solid fillers, liquid Body, gas pass in and out chromatographic column, and the multiple valve can be mounted in the column cap or column tail of chromatographic column.When multiple valve is mounted in column When head, it is located at chromatographic column upper end center position, and the longitudinal profile of the tail portion opening of internal cavity is inverted trapezoidal, passes through internal cavity Carry out filler into chromatographic column, filler uniformly therefrom can be settled into a plane under clan along inclined surface, will not secundly fall Under.When multiple valve is mounted in column tail, chromatographic column can be discharged in filler by internal cavity, since chromatographic column is generally relatively large in diameter And filler has been compacted during use before, it, can be respectively each second in order to exclude filler completely well Entrance is passed through gas and pumping liquid and breaks up uniform filling jack-up in column simultaneously, and then smoothly flows into internal cavity, through discharge Mouth outflow, cleaning effect is more preferable, and solvent loss is low, and promotes yield.It can be realized and be filled out using the chromatographic column of the multiple valve It is carried out while the outflow of material is with gas, liquid discrepancy chromatographic column.And it realizes more by the leakage hole installation of a small area For channel valve to which the filler of the bigger column bottom perimeter of area is all gone out chromatographic column from multiple valve, cleaning performance is good.
Although the present invention and its advantage has been described in detail it should be appreciated that without departing from by the attached claims Defined by can carry out various changes, replacement and transformation in the case of the spirit and scope of the present invention.Moreover, the model of the application Enclose the specific embodiment for being not limited only to process, equipment, means, method and steps described in specification.In the art is common Technical staff executes and corresponding reality described herein from the disclosure it will be readily understood that can be used according to the present invention Apply the essentially identical function of example or obtain the result essentially identical with it, existing and process to be developed in future, equipment, Means, method or step.Therefore, the attached claims are intended to include such process, equipment, hand in the range of them Section, method or step.

Claims (10)

1. a kind of multiple valve, which is characterized in that including:
Valve body, valve rod;
Concentric internal cavity up and down, external cavity are arranged in the valve body, wherein the external cavity is sheathed in described On the outside of cavity;
The valve rod is set to the internal cavity of the valve body, and controls the folding of the internal cavity;
The substance flowed in the internal cavity, the external cavity is not interfere with each other.
2. multiple valve according to claim 1, which is characterized in that the longitudinal profile of the tail portion of internal cavity opening is Inverted trapezoidal.
3. multiple valve according to claim 1, which is characterized in that the external cavity is set in the tail portion close to the valve body There is the first entrance, the second entrance is being equipped with close to the top of valve body.
4. multiple valve according to claim 1, which is characterized in that the diameter of the diameter of the valve body and the internal cavity Ratio be 5:1 to 50:1.
5. multiple valve according to claim 1, which is characterized in that the valve rod is located at the tail portion opening of the internal cavity End face be sealing surface.
6. multiple valve according to claim 5, which is characterized in that sieve plate is arranged in the sealing surface, in the valve rod Center of inside is equipped with sieve plate in communication seals face and penetrates through the fluid passage of the valve rod.
7. multiple valve as claimed in any of claims 1 to 6, which is characterized in that the valve rod is manual rotation Bar, Pneumatic lifting arm or hydraulic lifting arm.
8. a kind of chromatographic column including any one of claim 1 to 7 multiple valve, which is characterized in that further include:
Column sieve plate, the distributor being connected to external cavity, pressing plate, column tube;
The column sieve plate, the distributor and the pressing plate are bonded successively to be arranged in the column tube, the multiple valve setting In the leakage hole of the column sieve plate, the distributor and the pressing plate centre.
9. chromatographic column according to claim 8, which is characterized in that the column sieve plate includes:
Sieve plate seat, several deck units;
The sieve plate seat is equipped with that several shapes are identical and the through-hole of equidistantly distributed, several described deck units with it is described logical Hole matches, and is placed in the through-hole.
10. chromatographic column according to claim 8, which is characterized in that the cross section of the deck unit is round, positive triangle Shape, square, regular hexagon or octagon.
CN201610081487.XA 2016-02-05 2016-02-05 A kind of multiple valve and chromatographic column Active CN105570493B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2144226Y (en) * 1992-10-20 1993-10-20 蒋和青 Water saver for washing hands
CN2403952Y (en) * 1999-09-27 2000-11-01 宋吉庆 Forward stop valve for water tank
CN200943738Y (en) * 2006-08-22 2007-09-05 先锋电器集团有限公司 Modified multiple-pass one-way valve
CN101632878A (en) * 2009-09-01 2010-01-27 北京创新通恒科技有限公司 Distribution method and distribution device of mobile phases of chromatographic columns
CN201643783U (en) * 2009-12-22 2010-11-24 大连依利特分析仪器有限公司 Multi-hole grooved distribution disc for making chromatographic column heads
CN103083943A (en) * 2011-11-03 2013-05-08 辽宁科技大学 Drainage-type preparation chromatographic column
CN203580089U (en) * 2013-11-19 2014-05-07 郑建财 Die head filter plate for plastic granulator

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2144226Y (en) * 1992-10-20 1993-10-20 蒋和青 Water saver for washing hands
CN2403952Y (en) * 1999-09-27 2000-11-01 宋吉庆 Forward stop valve for water tank
CN200943738Y (en) * 2006-08-22 2007-09-05 先锋电器集团有限公司 Modified multiple-pass one-way valve
CN101632878A (en) * 2009-09-01 2010-01-27 北京创新通恒科技有限公司 Distribution method and distribution device of mobile phases of chromatographic columns
CN201643783U (en) * 2009-12-22 2010-11-24 大连依利特分析仪器有限公司 Multi-hole grooved distribution disc for making chromatographic column heads
CN103083943A (en) * 2011-11-03 2013-05-08 辽宁科技大学 Drainage-type preparation chromatographic column
CN203580089U (en) * 2013-11-19 2014-05-07 郑建财 Die head filter plate for plastic granulator

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Denomination of invention: A multi-channel valve and chromatographic column

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