CN102078706A - Ion exchange chromatography filtration method and chromatographic separation column thereof - Google Patents

Ion exchange chromatography filtration method and chromatographic separation column thereof Download PDF

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Publication number
CN102078706A
CN102078706A CN 201010584359 CN201010584359A CN102078706A CN 102078706 A CN102078706 A CN 102078706A CN 201010584359 CN201010584359 CN 201010584359 CN 201010584359 A CN201010584359 A CN 201010584359A CN 102078706 A CN102078706 A CN 102078706A
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cylindrical shell
chromatographic column
liquid
chromatographic
microwell plate
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CN 201010584359
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CN102078706B (en
Inventor
宋显洪
宋志骥
宋志胜
胡良分
陈金富
赵石凯
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ZHEJIANG DONGOU FILTER MANUFACTURING Co.,Ltd.
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Dongou Microporous Filtering Co Ltd Wenzhou City
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Abstract

The invention relates to an ion exchange chromatography filtration method. The steps of ion exchange, chromatography, solid-liquid separation, liquid-liquid separation, washing, filtration and regeneration are hermetically completed at one time in a chromatographic separation column. The invention also relates to the chromatographic separation column, which comprises a barrel, an upper cover and a lower cover, wherein a micropore plate and a guide plate are arranged between the upper cover and the barrel and between the lower cover and the barrel; the upper cover and the lower cover are provided with a distributor and a pipeline port; the distributor is provided with a positive blowing port and a micropore plate leakage port; a spray distribution head capable of moving up and down is arranged in the distributor; the spray distribution head is provided with a feeding hole; and a loading and uploading column apparatus, a resin tank, a cleaning solution tank and a collecting tank, which are connected with the barrel through pipelines, are also arranged outside the barrel. The ion exchange chromatography filtration method has the advantages of stable quality and high efficiency; and the chromatographic separation column has the advantage of realizing all steps of ion exchange chromatography filtration in a closed space.

Description

A kind of ion-exchange chromatography filter method and chromatographic isolation chromatographic column thereof
Technical field
The present invention relates to the method and the equipment thereof of a kind of ion-exchange, chromatography, Separation of Solid and Liquid, the separation of liquid liquid, washing, filtration, regeneration, especially a kind of ion-exchange chromatography filter method and chromatographic isolation chromatographic column of on medicine and food service industry, using thereof that relate to.
Background technology
At present, ion-exchange, chromatography are under certain pressure, and resin (or other filler) is gone up and stratifiedly under the different flow velocitys to be separated different classes of or different components, and obtain active princlple or the composition planning to obtain.The ion-exchange chromatography filter method of prior art will multiple devices and through multiple working procedure just can finish ion-exchange, chromatography, Separation of Solid and Liquid, liquid liquid separates, wash, filter, regenerate in steps, have quality instability, inefficient shortcoming.In addition, the diameter of the separation equipment that is used for the chromatographic column industry of prior art is less, and the anti-reverse flow of microwell plate is poor, causes the regeneration effect of microwell plate poor.Microwell plate also exists the aperture inhomogeneous, the quality instability, and the easy leakage of material, disposal ability is limited, and maximizing has circumscribed shortcoming.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art exactly, and a kind of steady quality, ion-exchange chromatography filter method and chromatographic isolation chromatographic column thereof that efficient is high are provided.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of ion-exchange chromatography filter method, ion-exchange, chromatography, Separation of Solid and Liquid, the separation of liquid liquid, washing, filtration, regeneration step disposable airtight finishing in a chromatographic isolation chromatographic column.
The chromatographic isolation chromatographic column that is used for said method, comprise that sidewall is provided with the cylindrical shell of visor, the loam cake of fixedlying connected with cylindrical shell and lower cover, be provided with microwell plate, deflector between loam cake and the cylindrical shell and between lower cover and the cylindrical shell, loam cake and under cover and be provided with distributor and pipe joint, on distributor, be provided with positive mouthpiece and microwell plate leakage hole, in distributor, be provided with spray dispensing head moving up and down, the spray dispensing head is provided with charging aperture, also is provided with loading and unloading post device, resin container, washing liquid tank and is connected with the cylindrical shell pipeline with collecting tank outside cylindrical shell.
The invention has the beneficial effects as follows: ion-exchange, chromatography, Separation of Solid and Liquid, the separation of liquid liquid, washing, filtration, regeneration step disposable airtight finishing in a chromatographic isolation chromatographic column has steady quality, advantage that efficient is high.Chromatographic isolation chromatographic column of the present invention is provided with cylindrical shell, loam cake and lower cover, be provided with microwell plate, deflector between loam cake and the cylindrical shell and between lower cover and the cylindrical shell, loam cake and under cover and be provided with distributor and pipe joint, on distributor, be provided with positive mouthpiece and microwell plate leakage hole, in distributor, be provided with spray dispensing head moving up and down, the spray dispensing head is provided with charging aperture, also is provided with loading and unloading post device, resin container, washing liquid tank and is connected with the cylindrical shell pipeline with collecting tank outside cylindrical shell.Therefore, chromatographic column of the present invention have in an airtight space realize that ion-exchange chromatography filters advantage in steps.
Description of drawings
Fig. 1 is the structural representation of chromatographic isolation chromatographic column of the present invention;
Fig. 2 is the attached view of Fig. 1;
Fig. 3 is the I portion enlarged drawing of Fig. 1;
Fig. 4 is the II portion enlarged drawing of Fig. 1;
Fig. 5 is the III portion enlarged drawing of Fig. 1;
Fig. 6 is the IV portion enlarged drawing of Fig. 1;
Fig. 7 is the improvement figure of Fig. 4;
Fig. 8 is the improvement figure of Fig. 7;
Fig. 9 is the structural representation of spray dispensing head;
Figure 10 is the longitudinal sectional view of microwell plate;
Figure 11 is the A-A cutaway view of Figure 10;
Figure 12 is the improvement figure of Figure 11;
Figure 13 is the B-B cutaway view of Fig. 7;
Figure 14 is the process chart of ion-exchange chromatography filter method of the present invention.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples:
As shown in figure 14, a kind of ion-exchange chromatography filter method, ion-exchange, chromatography, Separation of Solid and Liquid, the separation of liquid liquid, washing, filtration, regeneration step disposable airtight finishing in a chromatographic isolation chromatographic column.
As shown in Figure 1, the chromatographic isolation chromatographic column that is used for said method, comprise that sidewall is provided with the cylindrical shell 9 of visor 11, loam cake 14 of fixedlying connected and lower cover 6 with cylindrical shell 9, be provided with microwell plate 5 between loam cake 14 and the cylindrical shell 9 and between lower cover 6 and the cylindrical shell 9, deflector 7, on loam cake 14 and lower cover 6, be provided with distributor 3 and pipe joint 16, on distributor 3, be provided with positive mouthpiece 13 and microwell plate leakage hole 12, in distributor 3, be provided with spray dispensing head 4 moving up and down, spray dispensing head 4 is provided with charging aperture 8, also is provided with loading and unloading post device outside cylindrical shell 9, resin container, washing liquid tank is connected with cylindrical shell 9 pipelines with collecting tank.Lower cover 6 is installed on the support 2, and support 2 bottoms are provided with adjustable bottom feet dish 1, guarantees chromatographic column installation level.The material of described deflector 7 is a ultra-high molecular weight polyethylene, wall liner plastic layer 10 in the cylindrical shell 9, and visor 11 is arranged in dislocation on upper the depositing of cylindrical shell 9 sidewalls, guarantees that the inner four corner of chromatographic column is all visual; Distributor control box 22 is pneumatic operated valve group or magnetic valve group, by 17 motions of tracheae 18 control cylinders, spray dispensing head 4 is stretched, and makes spray distribute to be in and closes, sprays, loads and unloads three positions of material.Described cylindrical shell 9 outer walls are provided with chuck layer 19, and chuck layer 19 is provided with chuck import and JO, and adjustment liquid flows into from the chuck import, flow out from JO, and the material in the cylindrical shell 9 is carried out adjustment.
As shown in Figure 2, lifting bolt 15 is fixed on the loam cake 14, is used to change microwell plate 5 or maintenance or carrying.
As shown in Figure 3, described visor 11 inner surfaces are arc, flush with cylindrical shell 9 inwalls, all around side and 9 seamless cooperations of cylindrical shell.Prevent solid accumulation in its slit, grow bacterium and contaminated material.And also have scale on the visor 11, use as metering.
Shown in Fig. 4 and 6, microwell plate 5 is installed in the deflector 7, and deflector 7 utilizes screw 21 to be fixed in lower cover 6 and the loam cake 14 by sealing ring 20.
As shown in Figure 5, inner seal ring 33 is connected with T type connecting ring 29 by screw thread and compresses, and deflector axle core 30, outer seal ring 32, frustum base 34 and sealing ring 31 utilize bolt 35 to compress sealing; Spray dispensing head 4 is installed in the middle of microwell plate 5.
As shown in Figure 7, withstand voltage deflector 23 is that flow-guiding channel with deflector 7 is by contacting the inside that changes at deflector with the lining plastic cover of lower cover 6; Before not improving, the pressure of 7 abilities of deflector depends on the quantity and the distribution of screw 21, and the pressure of ability is limited, when changing into its inside, only relevant with the type shape and the material of its passage, but superpressure prolongs the pulse cleaning effect in the microwell plate 5 to the above pressure reduction of 0.6MPa.
As shown in Figure 8, described microwell plate 5 is integrative-structures with deflector 23.Monoblock type is withstand voltage, and water conservancy diversion microwell plate 24 is that microwell plate 5 and withstand voltage deflector 23 are made an integral body, and its beneficial effect is that the installation replacing is simpler, convenient, improves maintenance efficiency.
As shown in Figure 9, described spray dispensing head 4 upper surfaces are sphere, make liquid on it flow through sphere more smoothly and enter into filtering area, and anti-ly when underflow pile up material on it; Spray apertures 25 is located on the arcuation face of cylinder 26 and connects with endoporus 27, and the longitudinal section of spray apertures 25 is provided with angle [alpha], makes that liquid or gas spreads in course of injection, speedup, and the impulsive force when strengthening injection makes the quicker dispersion of solid (resin).The sectional area sum of all spray apertures 25 equals the sectional area of 0.1~1 times endoporus 27.
As shown in figure 10, the material of described microwell plate 5 is ultra-high molecular weight polyethylene or stainless steel or Titanium or pottery.Described microwell plate 5 one sides are micropore face 36, and another side is a solid surfaces 37, and border outer cylinder 38 is the micropore face, middle through hole inner cylinder 39 is a solid surfaces, be provided with passage 28 between micropore face 36 and solid surfaces 37, liquid compiles outflow from micropore face 36 admission passages 28 from border outer cylinder 38; Purge gas evenly spreads the back from micropore face 36 quick-fried gas from border outer cylinder 38 admission passages 28 in passage 28.
The cross section of described passage 28 is circular or oval, and the longitudinal section is provided with angle beta near a side of solid surfaces 37.The β angle makes the resistance of passage 28 inner fluid each points identical, and the resistance and the flow velocity of micropore face 36 each points of assurance microwell plate 5 are the same; The each point instantaneous velocity of material turnover microwell plate is controlled within the acceptable range.
As shown in figure 11, the passage 28 of microwell plate 5 is fan-shaped distribution, and making micropore face 36 is 1~5 times of short lines distance to the longest air line distance of passage 28, has guaranteed the flow velocity uniformity of micropore face 36.
As shown in figure 12, passage 28 has the γ angle, by improving behind the computer computer simulation, shortens the range difference of micropore face 36 each points to passage 28, makes the flow velocity of micropore face 36 more even.
As shown in figure 13, just flowing to of liquid is that the micropore face 36 of microwell plate 5 advances, and to the filtration pore channel of microwell plate 5, to passage 28, to outer tunnel 40, to split channel 41, to internal channel 42, to outlet 43, goes out to pipe joint 16 at last; Reverse direction flow is opposite with it.Described microwell plate and deflector can the pressure reduction of anti-0.6MPa gas or liquid; The chromatographic column body can bear 10MPa pressure, diameter at φ more than 1800.
The present invention is specially adapted to pharmaceuticals industry, or industry such as food, agricultural chemicals, chemical industry, metallurgy.

Claims (10)

1. an ion-exchange chromatography filter method is characterized in that: ion-exchange, chromatography, Separation of Solid and Liquid, the separation of liquid liquid, washing, filtration, regeneration step disposable airtight finishing in a chromatographic isolation chromatographic column.
2. the chromatographic isolation chromatographic column that is used for the described method of claim 1, it is characterized in that: comprise that sidewall is provided with the cylindrical shell of visor, loam cake of fixedlying connected and lower cover with cylindrical shell, be provided with microwell plate between loam cake and the cylindrical shell and between lower cover and the cylindrical shell, deflector, loam cake and under cover and be provided with distributor and pipe joint, on distributor, be provided with positive mouthpiece and microwell plate leakage hole, in distributor, be provided with spray dispensing head moving up and down, the spray dispensing head is provided with charging aperture, also is provided with loading and unloading post device outside cylindrical shell, resin container, washing liquid tank is connected with the cylindrical shell pipeline with collecting tank.
3. chromatographic isolation chromatographic column according to claim 2 is characterized in that: the material of described microwell plate is ultra-high molecular weight polyethylene or stainless steel or Titanium or pottery.
4. chromatographic isolation chromatographic column according to claim 2, it is characterized in that: described microwell plate simultaneously is the micropore face, another side is a solid surfaces, the border outer cylinder is the micropore face, middle through hole inner cylinder is a solid surfaces, be provided with passage between micropore face and solid surfaces, liquid compiles outflow from micropore face admission passage from the border outer cylinder; Purge gas evenly spreads the back from the quick-fried gas of micropore face from border outer cylinder admission passage in passage.
5. chromatographic isolation chromatographic column according to claim 4 is characterized in that: the cross section of described passage is for circular or oval, and the longitudinal section is provided with angle beta near a side of solid surfaces, and passage is fan-shaped distribution.
6. chromatographic isolation chromatographic column according to claim 2 is characterized in that: described microwell plate and deflector are integrative-structures.
7. chromatographic isolation chromatographic column according to claim 2 is characterized in that: the material of described deflector is a ultra-high molecular weight polyethylene, cylinder inboard wall lining plastic layer.
8. chromatographic isolation chromatographic column according to claim 2 is characterized in that: described visor inner surface is an arc, flushes with cylinder inboard wall, and the side cooperates with cylindrical shell is seamless all around.
9. chromatographic isolation chromatographic column according to claim 2 is characterized in that: described spray dispensing head upper surface is a sphere, and the longitudinal section of spray apertures is provided with angle [alpha].
10. chromatographic isolation chromatographic column according to claim 2, it is characterized in that: described cylinder body outer wall is provided with the chuck layer, and the chuck layer is provided with chuck import and JO, and adjustment liquid flows into from the chuck import, flow out from JO, the material in the cylindrical shell is carried out adjustment.
CN 201010584359 2010-12-02 2010-12-02 Ion exchange chromatography filtration method and chromatographic separation column thereof Active CN102078706B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103182331A (en) * 2013-03-29 2013-07-03 浙江海牛环境科技有限公司 End cap guiding device for efficient shallow resin bed
CN107457125A (en) * 2017-09-29 2017-12-12 江苏汉邦科技有限公司 A kind of liquid-inlet valve

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6610200B1 (en) * 1998-10-31 2003-08-26 Amersham Biosciences Ab System and its units
CN2635174Y (en) * 2003-09-10 2004-08-25 大连依利特分析仪器有限公司 Radial preparation liquid chromatographic column used for integrated bed layer separation medium
CN1795034A (en) * 2003-05-23 2006-06-28 通用电气健康护理生物科学股份公司 Chromatography column with movable adapter
CN1891086A (en) * 2005-07-08 2007-01-10 陕西师范大学 Apple juice harmful metal ion adsorption separation exchanger
CN201997135U (en) * 2010-12-02 2011-10-05 温州市东瓯微孔过滤有限公司 Chromatograph separation chromatographic column

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6610200B1 (en) * 1998-10-31 2003-08-26 Amersham Biosciences Ab System and its units
CN1795034A (en) * 2003-05-23 2006-06-28 通用电气健康护理生物科学股份公司 Chromatography column with movable adapter
CN2635174Y (en) * 2003-09-10 2004-08-25 大连依利特分析仪器有限公司 Radial preparation liquid chromatographic column used for integrated bed layer separation medium
CN1891086A (en) * 2005-07-08 2007-01-10 陕西师范大学 Apple juice harmful metal ion adsorption separation exchanger
CN201997135U (en) * 2010-12-02 2011-10-05 温州市东瓯微孔过滤有限公司 Chromatograph separation chromatographic column

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103182331A (en) * 2013-03-29 2013-07-03 浙江海牛环境科技有限公司 End cap guiding device for efficient shallow resin bed
CN103182331B (en) * 2013-03-29 2015-01-28 浙江海牛环境科技有限公司 End cap guiding device for efficient shallow resin bed
CN107457125A (en) * 2017-09-29 2017-12-12 江苏汉邦科技有限公司 A kind of liquid-inlet valve
CN107457125B (en) * 2017-09-29 2024-04-02 江苏汉邦科技股份有限公司 Liquid inlet valve

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