CN101954202A - Constant-pressure closed ascending chromatographic column device and application method thereof - Google Patents
Constant-pressure closed ascending chromatographic column device and application method thereof Download PDFInfo
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- CN101954202A CN101954202A CN2009100893405A CN200910089340A CN101954202A CN 101954202 A CN101954202 A CN 101954202A CN 2009100893405 A CN2009100893405 A CN 2009100893405A CN 200910089340 A CN200910089340 A CN 200910089340A CN 101954202 A CN101954202 A CN 101954202A
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000001174 ascending effect Effects 0.000 title abstract description 13
- 229920000742 Cotton Polymers 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 29
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 13
- 238000004587 chromatography analysis Methods 0.000 claims description 103
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 79
- 239000011521 glass Substances 0.000 claims description 35
- 239000000741 silica gel Substances 0.000 claims description 22
- 229910002027 silica gel Inorganic materials 0.000 claims description 22
- 238000007789 sealing Methods 0.000 claims description 13
- 229920001971 elastomer Polymers 0.000 claims description 8
- 238000004809 thin layer chromatography Methods 0.000 claims description 8
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- 239000003795 chemical substances by application Substances 0.000 claims 7
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000004816 latex Substances 0.000 claims 1
- 229920000126 latex Polymers 0.000 claims 1
- 238000005498 polishing Methods 0.000 claims 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 description 27
- 238000000926 separation method Methods 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 238000004440 column chromatography Methods 0.000 description 6
- KIGVOJUDEQXKII-UHFFFAOYSA-N 4-bromo-n-(4-bromophenyl)-n-phenylaniline Chemical compound C1=CC(Br)=CC=C1N(C=1C=CC(Br)=CC=1)C1=CC=CC=C1 KIGVOJUDEQXKII-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- WDFQBORIUYODSI-UHFFFAOYSA-N 4-bromoaniline Chemical compound NC1=CC=C(Br)C=C1 WDFQBORIUYODSI-UHFFFAOYSA-N 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- PCLIMKBDDGJMGD-UHFFFAOYSA-N N-bromosuccinimide Chemical compound BrN1C(=O)CCC1=O PCLIMKBDDGJMGD-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
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- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- -1 4,4-dibromo triphenyl amine compound Chemical class 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
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Abstract
The invention relates to a device for extracting, separating and purifying organic compounds, in particular to a constant-pressure closed ascending chromatographic column device and an application method thereof, belonging to the fields of chemical engineering, chemistry and pharmacy. The device comprises absorbent cotton, a pipe, a seal ring, an adapting pipe, a chromatographic column, a developing solvent, a chromatographic cylinder and a chromatographic cover, wherein the top of the chromatographic column with an opening bottom is connected with a small nozzle; an opening for installing the chromatographic column and a ground hole for installing the adapting pipe are respectively arranged on the chromatographic cylinder cover; the chromatographic column is vertically arranged upside down in the chromatographic cylinder through the opening for installing the chromatographic column on the chromatographic cylinder cover, and the seal ring is arranged between the chromatographic column and the opening on the chromatographic cylinder cover; one end of the adapting pipe is sheathed with the pipe, and the other end is inserted into the ground hole; the other end of the pipe is communicated with the small nozzle; and the first absorbent cotton is installed inside the opening on the top of the chromatographic column, and the second absorbent cotton is installed on the bottom of the chromatographic column. The device has simple structure and high separating efficiency on the organic compounds, and the selection of the developing solvent is convenient.
Description
Technical field
The invention belongs to the device of organic compound extraction, separation and purifying in chemical industry, chemistry, the pharmaceutical field, be particularly related to the airtight ascending chromatography column device of constant voltage to extraction, separation and the purifying of the organic compound that is difficult to separate, and the application process of the airtight ascending chromatography column device of this constant voltage.
Background technology
The separation of organic compound method the most commonly used is the chromatography method.Fine dispersed solids or the liquid that is attached to the surface of solids as fixing phase, in liquid (immiscible) or the system of gas as mobile phase with aforesaid liquid, make each composition in the mixture keep moving respectively simultaneously to the biphase equilibrium state, utilize each composition to fixedly the different caused translational speeds of phase affinity are poor, the qualitative and quantitative analytical method that they are separated from each other, be called the chromatography method, also claim chromatography.Utilize filling fixedly the chromatographic column of the phase method of separating be called column chromatography.According to the difference of mobile phase kind, be divided into two kinds of liquid chromatography(LC), gas chromatographies.Solid with the phase that fixes has silica gel, active carbon, aluminium oxide, ion exchange resin, ion-exchange fibre etc., or adheres to suitable liquid on the carrier of the such non-activity of diatomite and cellulose, also can use other material.Chromatography is divided into three types of absorbent-type, distribution type, ion-exchange types (ion-exchange chromatography) etc. according to the difference of affinity between mutually fixing and solute.The column chromatography device of the Separation of Organic Compounds purifying of modern chemical industry pharmaceutical field has descending adding pressure type, descending gerotor type, descending decompression type etc., the main column of common column chromatography device adopts glass or metal material more, and its weak point is: solvent load is many, Separation of Organic Compounds efficient is low, the fixing shortcomings such as chromatographic column difficulty, operation inconvenience, contaminated environment of loading mutually.
Summary of the invention
One of purpose of the present invention is the weak point that overcomes top common chromatography partition method, provides a kind of and fixing has loaded mutually that chromatographic column is simple, solvent load is few, Separation of Organic Compounds efficient height, that solvent is selected is convenient, simple in structure, need not that the people guards, the airtight ascending chromatography column device of pollution-free, easy-operating constant voltage.
Two of purpose of the present invention provides the application process of the airtight ascending chromatography column device of constant voltage.
The airtight ascending chromatography column device of constant voltage of the present invention comprises: first absorbent cotton, pipe, sealing ring, transfer tube, chromatography cylinder cap (can be glass cover), chromatographic column, second absorbent cotton, solvent and chromatography cylinder (can be glass jar) etc.;
The top that in the bottom is uncovered chromatographic column is connected to a thin mouth;
Described chromatography cylinder has a chromatography cylinder cap, covers at chromatography cylinder and has opening that chromatographic column is installed and the ground hole that transfer tube is installed;
The opening of the installation chromatographic column that described chromatographic column covers through chromatography cylinder vertically is inverted in the chromatography cylinder (chromatographic column uncovered in chromatography cylinder), and between the opening that chromatographic column and chromatography cylinder cover sealing ring is arranged;
One end of described transfer tube is with pipe, and in the ground hole on the other end insertion chromatography cylinder cap of transfer tube, the other end of pipe is connected with the thin mouth at chromatographic column top;
The inside at the opening part at chromatographic column top is equipped with first absorbent cotton, in the bottom of chromatographic column second absorbent cotton is installed;
The length of described chromatographic column can be 10～100cm, and internal diameter can be 1～200mm, and preferred internal diameter is 10～100mm; The thin mouth of chromatographic column is less than the internal diameter of chromatographic column, and preferred internal diameter is 4～12mm.
The top edge of described chromatography cylinder mouth is that frosted is thrown mouthful, the one side of chromatography cylinder cap be frosted throw face (chromatography cylinder and chromatography cylinder cap by frosted throw mouthful combine with frosted throwing face guarantee air tight).
Described chromatographic column material is glass, quartz or metal etc.
Described tubing is vacuum tube, emulsion tube, silicone tube or rubber tube etc.
Described sealing ring material is silica gel or rubber etc.
Described chromatographic column adopts existing chromatographic column.
Utilize the application process of the airtight ascending chromatography column device of constant voltage of the present invention purification organic compound, this application process may further comprise the steps:
(1) to select a root bottom part be uncovered and the top is connected to the chromatographic column of a thin mouth, and block up thin mouth with first absorbent cotton;
(2) be connected with bottle,suction after the thin mouth of the chromatographic column of step (1) outside puts a turned welt plug, the open-mouth by chromatographic column adds silica white, and adds silica white with suction filtration limit, vavuum pump limit; Beaing simultaneously chromatographic column gently to guarantee the silica white surfacing, is that 3～4cm stops to add silica white until the silica white surface from the open-mouth of chromatographic column;
(3) sample dissolution with solvents to be separated, add the silica white of 5～10 times of example weights to be separated, be spin-dried for then; Again the sample to be separated with silica white absorption is joined in the chromatographic column of step (2), it is smooth to guarantee sample surfaces to beat chromatographic column in the sample to be separated that adds silica white absorption with suction filtration limit, vavuum pump limit gently, and the sample thickness to be separated of silica white absorption is added silica white to uncovered 1cm place then less than 2cm on the surface of the sample to be separated that silica white adsorbs;
(4) on the silica white of step (3) chromatographic column open-mouth, add last layer second absorbent cotton, and it is uncovered more slightly to exceed chromatographic column with this absorbent cotton jam-pack chromatographic column mouth until absorbent cotton; Remove bottle,suction and turned welt plug then, chromatographic column is inverted to thin mouth makes progress, and sealing ring is installed on the cylinder of chromatographic column;
(5) opening of the installation chromatographic column that covers through chromatography cylinder of the chromatographic column that step (4) is obtained, vertically be inverted in the chromatography cylinder (chromatographic column uncovered in chromatography cylinder), and the bottom that makes second absorbent cotton touch chromatography cylinder, reach by sealing ring and make the opening sealing that chromatographic column is installed;
(6) place, the ground hole of the chromatography cylinder cap by step (5) adds solvent in chromatography cylinder, after waiting to add solvent, one transfer tube is installed in ground hole place, and puts pipe, the other end of pipe be connected with the thin mouth at chromatographic column top (formation constant-voltage system) at the other end of transfer tube; Solvent is by up moving in the chromatographic column, and sample to be separated is separated into different colour bands in chromatographic column, and whole process is the individual process of thin-layer chromatography of simulating fully;
(7) solvent for the treatment of step (6) by in the chromatographic column up move to the chromatographic column top after, with chromatographic column by taking out in the chromatography cylinder, be enclosed within on the steel cylinder of Compressed Gas after pipe on the thin mouth takes off being enclosed within, the silica gel cylinder that will be separated into different colour bands with compressed air under uviol lamp blows out, and simultaneously different colour bands is cut respectively in different containers; Select the silica gel cylinder of required colour band and be higher than the dissolution with solvents of used solvent, filter the organic compound ingredient that can obtain required purification then with polarity.
Described solvent adopts thin-layer chromatography (TLC) to analyze employed solvent.
Described compressed-air actuated pressure is 0.1～1 atmospheric pressure.
The airtight ascending chromatography column device of constant voltage of the present invention is isolated fully with external environment condition in the separation process of carrying out sample, the low boiling solvent can not volatilized in the sample separation process, avoided launching solvent in the chromatography process change in polarity and influence separating effect, contaminated environment, influence negative effects such as the operator is healthy.The present invention have fixing load mutually that chromatographic column is simple, solvent load is few, Separation of Organic Compounds efficient height, that solvent is selected is convenient, simple in structure, need not that the people guards, characteristics such as pollution-free, easy to operate.
Description of drawings
Fig. 1. the cross-sectional view of the airtight ascending chromatography column device of constant voltage of the present invention.
Reference numeral
1. absorbent cotton 2. pipes 3. sealing rings
4. transfer tube 5. ground holes 6. chromatography cylinder caps
7. frosted is thrown mouth and is thrown face junction 8. chromatographic columns with frosted
9. sample 10. silica gel 11. absorbent cotton
12. solvent 13. chromatography cylinders
Specific embodiments
See also Fig. 1.The airtight ascending chromatography column device of constant voltage comprises: first absorbent cotton 1, silica gel pipe 2, rubber seal 3, glass transfer tube 4, glass chromatography cylinder cap 6, glass chromatography column 8, second absorbent cotton 11, solvent 12 and glass chromatography cylinder 13 etc.
Adopting existing chromatographic column, is that uncovered length is that the top of the glass chromatography column 8 of 50cm is connected to the thin mouth of a glass in the bottom, and wherein: the internal diameter of glass chromatography column is 30mm, and the internal diameter of the thin mouth of glass is 10mm.
Described glass chromatography cylinder 13 has a glass chromatography cylinder cap 6, has opening that glass chromatography column 8 is installed and the ground hole 5 that glass transfer tube 4 is installed on glass chromatography cylinder cap 6; Wherein: the top edge of glass chromatography cylinder mouth is that frosted is thrown mouthful, the one side of glass chromatography cylinder cap 6 be frosted throw face (chromatography cylinder and chromatography cylinder cap by frosted throw mouthful combine with frosted throwing face guarantee air tight).
The opening of the installation glass chromatography column 8 of described glass chromatography column 8 on glass chromatography cylinder cap 6, vertically be inverted in the glass chromatography cylinder 13 (glass chromatography column uncovered in glass chromatography cylinder 13), and between the opening on glass chromatography column 8 and the glass chromatography cylinder cap 6, rubber seal arranged.
One end of described glass transfer tube 4 is with silica gel pipe 2, and in the ground hole 5 on the other end insertion glass chromatography cylinder cap 6 of glass transfer tube 4, the other end of silica gel pipe 2 is connected with the thin mouth of glass at glass chromatography column 8 tops.
The inside at the opening part at glass chromatography column 8 tops is equipped with first absorbent cotton 1, and second absorbent cotton 11 is installed in the bottom of glass chromatography column 8.
Purification compound 4,4-dibromo triphenylamine.Because compound 4,4-dibromo triphenylamine is that the N-bromo-succinimide reaction by triphenylamine and twice obtains, and the existing 4-monobromo of product triphenylamine has three (4-bromophenyl) amine again.And raw material triphenylamine, 4-monobromo triphenylamine, 4, the polarity of four kinds of compounds of 4-dibromo triphenylamine and three (4-bromophenyl) amine is all very similar, therefore with common descending normal pressure column chromatography, descending pressurized column chromatography and descending decompression column chromatography separating effect are not fine.Obtain four points, the R of four points with the analysis of TLC chromatoplate
fValue is respectively 0.48,0.30,0.26,0.15 (R
fValue is that 0.26 compound is a target compound).
Adopt the capillarity principle, simulate the thin-layer chromatography condition fully, utilize the airtight ascending chromatography column device of the constant voltage purification compound 4 of the invention described above, 4-dibromo triphenylamine.
(1) with the stifled thin mouth of going up chromatographic column of first absorbent cotton;
(2) be connected with bottle,suction after the thin mouth of the chromatographic column of step (1) outside puts a turned welt plug, the open-mouth by chromatographic column adds silica white H, and adds silica white H with suction filtration limit, vavuum pump limit; Beaing simultaneously chromatographic column gently to guarantee silica white H surfacing, is that 4cm stops to add silica white H until silica white H surface from the open-mouth of chromatographic column;
(3) compound to be separated 4,4-dibromo triphenylamine dissolves with carrene, adds to be separatedly 4, and the silica white H that 4-dibromo triphenylamine example weight is 5 times is spin-dried for then; Again with to be separated 4 of silica white H absorption, 4-dibromo triphenylamine sample joins in the chromatographic column of step (2), adding to be separated 4 of silica white H absorption with suction filtration limit, vavuum pump limit, it is smooth to guarantee sample surfaces to beat chromatographic column in the time of 4-dibromo triphenylamine sample gently, silica white H absorption to be separated 4,4-dibromo triphenylamine sample thickness is 1cm; To be separated 4 in silica white H absorption added silica white H to uncovered 1cm place on the surface of 4-dibromo triphenylamine sample then;
(4) on the silica white H of step (3) chromatographic column open-mouth, add last layer second absorbent cotton, and it is uncovered more slightly to exceed chromatographic column with this absorbent cotton jam-pack chromatographic column mouth until absorbent cotton; Remove bottle,suction and turned welt plug then, chromatographic column is inverted to thin mouth makes progress, and rubber seal is installed on the cylinder of chromatographic column;
(5) opening of the installation chromatographic column that covers through chromatography cylinder of the chromatographic column that step (4) is obtained, vertically be inverted in the chromatography cylinder (chromatographic column uncovered in chromatography cylinder), and the bottom that makes second absorbent cotton touch chromatography cylinder, reach by rubber seal and make the opening sealing that chromatographic column is installed;
(6) place, the ground hole of the chromatography cylinder cap by step (5) adds solvent in chromatography cylinder, after waiting to add solvent, one transfer tube is installed in ground hole place, and puts pipe, the other end of pipe be connected with the thin mouth at chromatographic column top (formation constant-voltage system) at the other end of transfer tube; Solvent is by up move in the chromatographic column, and is to be separated 4, and 4-dibromo triphenylamine sample is separated into 4 colour bands in chromatographic column, and whole process is to simulate the process of thin-layer chromatography fully;
(7) solvent for the treatment of step (6) by in the chromatographic column up move to the chromatographic column top after, with chromatographic column by taking out in the chromatography cylinder, be enclosed within on the steel cylinder of Compressed Gas after pipe on the thin mouth takes off being enclosed within, with 0.3 atmospheric compressed air silica white H cylinder is blown out, can see obviously that under uviol lamp silica white H cylinder is separated into 4 colour bands, simultaneously 4 colour bands be cut respectively in different containers; Select the Rf value and be the silica white H cylinder of 0.26 colour band and, filter then and can obtain 4,4-dibromo triphenylamine with the ethyl acetate solvent dissolving.Separate the rate of recovery and reached 98%, separate obtain 4,4-dibromo triphenyl amine compound can be directly by Mass Spectrometer Method and nmr analysis.
Described solvent is the mixed liquor of carrene and benzinum, and wherein: the volume ratio of carrene and benzinum is 1: 15.
Claims (9)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100893405A CN101954202B (en) | 2009-07-16 | 2009-07-16 | Constant-pressure closed ascending chromatographic column device and application method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100893405A CN101954202B (en) | 2009-07-16 | 2009-07-16 | Constant-pressure closed ascending chromatographic column device and application method thereof |
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| CN101954202A true CN101954202A (en) | 2011-01-26 |
| CN101954202B CN101954202B (en) | 2012-07-25 |
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| CN2009100893405A Expired - Fee Related CN101954202B (en) | 2009-07-16 | 2009-07-16 | Constant-pressure closed ascending chromatographic column device and application method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102989199A (en) * | 2012-12-11 | 2013-03-27 | 聊城万合工业制造有限公司 | Inner storage constant-pressure preparative column device |
| CN105203377A (en) * | 2015-09-29 | 2015-12-30 | 齐国良 | Purifying device for pretreatment of Aspergillus flavus and method adopting same |
| CN106526139A (en) * | 2016-11-18 | 2017-03-22 | 中国石油大学(北京) | Funnel for analysis of crude oil family components and method for separating asphaltene from crude oil family |
| CN106914035A (en) * | 2015-12-28 | 2017-07-04 | 江南大学 | A kind of chromatographic separating process of soluble carbon point system |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH674315A5 (en) * | 1987-11-23 | 1990-05-31 | Werner Hafner | |
| CN2469454Y (en) * | 2001-03-12 | 2002-01-02 | 易求实 | Closed continuous column chromatography analyse device |
| 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 | A new type of chromatographic column |
-
2009
- 2009-07-16 CN CN2009100893405A patent/CN101954202B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102989199A (en) * | 2012-12-11 | 2013-03-27 | 聊城万合工业制造有限公司 | Inner storage constant-pressure preparative column device |
| CN102989199B (en) * | 2012-12-11 | 2014-09-03 | 聊城万合工业制造有限公司 | Inner storage constant-pressure preparative column device |
| CN105203377A (en) * | 2015-09-29 | 2015-12-30 | 齐国良 | Purifying device for pretreatment of Aspergillus flavus and method adopting same |
| CN106914035A (en) * | 2015-12-28 | 2017-07-04 | 江南大学 | A kind of chromatographic separating process of soluble carbon point system |
| CN106526139A (en) * | 2016-11-18 | 2017-03-22 | 中国石油大学(北京) | Funnel for analysis of crude oil family components and method for separating asphaltene from crude oil family |
| CN106526139B (en) * | 2016-11-18 | 2019-02-22 | 中国石油大学(北京) | Funnel for component analysis of crude oil family and method for separating asphaltenes in crude oil family |
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| CN101954202B (en) | 2012-07-25 |
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