阅读说明：本技术 一种新型自动层析分离提纯装置 (Novel automatic chromatographic separation purification device ) 是由 王楠楠 耿浩博 郭娇娇 于 2020-07-29 设计创作，主要内容包括：本发明公开了一种新型自动层析分离提纯装置,包括：接液机构,其可旋转支撑设置在水平面上；层析柱,其支撑设置在所述接液机构的上方；振动机构,其设置在所述层析柱的外壁上；橡胶套,其套设在所述振动结构外部；搅拌机构,其连通设在所述层析柱上方；两个进液罐,其分别与所述搅拌机构相连通,并设置在所述搅拌机构的上方。本装置设计了一种自动层析分离提纯的新装置,可实现将传统的层析柱和自动化设备紧密相连的全新装置,该装置不仅具有普通的柱层析分离提纯作用,与此同时该设备解决了柱层析实验过程中硅胶填装、上样繁琐、洗脱剂预先调配,洗脱剂浪费、流速控制、试管频繁更换等一系列自动化程度低的问题,节省了人力和时间。(The invention discloses a novel automatic chromatographic separation and purification device, which comprises: the liquid receiving mechanism is rotatably supported and arranged on a horizontal plane; the chromatographic column is supported and arranged above the liquid receiving mechanism; a vibrating mechanism disposed on an outer wall of the chromatography column; the rubber sleeve is sleeved outside the vibration structure; the stirring mechanism is communicated with and arranged above the chromatographic column; and the two liquid inlet tanks are respectively communicated with the stirring mechanism and are arranged above the stirring mechanism. This device has designed a new installation of automatic chromatography separation purification, can realize the brand-new device that closely links to each other with traditional chromatographic column and automation equipment, and the device not only has ordinary column chromatography separation purification effect, and this equipment has solved simultaneously that silica gel is loaded in the column chromatography experimentation, the appearance is loaded down with trivial details, the eluent allotment in advance, and the problem that a series of degree of automation such as eluent waste, flow rate control, test tube frequent change have been hanged down has saved manpower and time.)

1. The utility model provides a novel automatic chromatography separation purification device which characterized in that includes:

the liquid receiving mechanism is rotatably supported and arranged on a horizontal plane;

the chromatographic column is supported and arranged above the liquid receiving mechanism;

a vibrating mechanism disposed on an outer wall of the chromatography column;

the rubber sleeve is sleeved outside the vibration structure;

the stirring mechanism is communicated with and arranged above the chromatographic column;

and the two liquid inlet tanks are respectively communicated with the stirring mechanism and are arranged above the stirring mechanism.

2. The novel automatic chromatographic separation and purification device according to claim 1, further comprising:

and the iron support is horizontally arranged, and the liquid receiving mechanism is arranged on the iron support.

3. The automatic chromatographic separation and purification device of claim 2, wherein the chromatographic column is fixedly arranged on the iron support.

4. The novel automatic chromatographic separation and purification device according to claim 3, wherein the liquid receiving device comprises:

a disc;

the two conveyor belts are respectively arranged on the inner wall and the outer wall of the disc;

and the test tube rack is fixedly arranged on the disc and is coaxial with the disc.

5. The novel automatic chromatographic separation and purification device according to claim 4, wherein the vibration mechanism comprises:

and the motor vibration sheets are respectively arranged on the outer wall of the chromatographic column.

6. The novel automatic chromatographic separation and purification device of claim 5, wherein one end of the chromatographic column is provided with a first cock, and the other end of the chromatographic column is provided with a second cock, and the first cock is axially provided with a spiral channel.

7. The novel automatic chromatographic separation and purification device according to claim 6, further comprising:

the liquid discharger is arranged at one end of the chromatographic column and communicated with the first cock;

one end of the first filter is communicated with one end of the liquid discharger;

and one end of the first liquid inlet pump is communicated with the other end of the first filter, and the other end of the first liquid inlet pump is communicated with the stirring mechanism.

8. The novel automatic chromatographic separation and purification device according to claim 7, wherein the stirring device comprises:

a stirring tank;

the stirrer is arranged at the bottom of the stirring tank;

and one end of the connecting pipe is arranged in the stirring tank, and the other end of the connecting pipe is communicated with the other end of the first liquid inlet pump.

9. The novel automatic chromatographic separation and purification device according to claim 8, further comprising:

the three-way pipe comprises a vertical end, a first horizontal end and a second horizontal end, wherein the first horizontal end and the second horizontal end are oppositely arranged, the vertical end is communicated with the stirring tank, and the first horizontal end and the second horizontal end are respectively communicated with the liquid inlet tank.

10. The automatic chromatographic separation and purification device according to claim 9, wherein a second filter and a second liquid inlet pump are sequentially communicated between the first horizontal end and the liquid inlet tank.

Technical Field

The invention relates to a novel automatic chromatographic separation and purification device, and belongs to the field of chemical instruments.

Background

In the course of the separation and purification operation of chemical experiment, the chemical reaction is mostly homogeneous, and in general, the side reaction of organic reaction is many, so that the substance obtained after the experiment is a mixture in which the rest raw materials, the by-products of the reaction, the catalyst and the required products are mixed. In this case, it is necessary to separate the mixed substances, and column chromatography separation and purification is the most widely used and most adaptable method for separating these substances, and is the most basic separation means. The principle of column chromatography separation and purification is to separate the components according to the difference of adsorption force of the substances on silica gel. In general, substances with higher polarity are easily adsorbed by silica gel, and substances with weaker polarity are not easily adsorbed by silica gel. When solvent elution is adopted, a series of processes of adsorption → desorption → re-adsorption → re-desorption occur, components with stronger adsorption force move for a short distance, and then are discharged from the column; the component with weaker adsorption force moves a larger distance to come out of the column.

In current column chromatography experiment operation, the experimenter need strike the chromatographic column manually or adopt modes such as pressurization to make the silica gel layer compact and get rid of the system bubble, need the experimenter to let the sample hug closely the chromatographic column inner wall with the rubber head burette and slowly flow down when the appearance, reduce the impact of sample to the silica gel layer, still need with in the incessant joining chromatographic column of the eluant of joining in advance that prepares well in advance, need the experimenter to debug the cock control flow rate frequently during the experiment, incessantly change and receive the test tube, make work very loaded down with trivial details, the complexity of experimental operation has been increased like this, the uncertain solvent that produces of eluant quantity is extravagant, experimenter's work load has been increased, cause unavoidable injury to.

Disclosure of Invention

The invention designs and develops a novel automatic chromatographic separation and purification device, which can overcome the problems that the prior experimenter needs to manually knock a chromatographic column or adopt modes such as pressurization and the like to chateau silica gel when performing column chromatography experiments, the sample loading of a teaching head dropper is frequent, and the replacement of a receiving test tube is frequent.

Another object of the invention is: the opening and the flow of the column chromatography piston can be controlled in real time.

The technical scheme provided by the invention is as follows:

a novel automatic chromatographic separation and purification device comprises:

the liquid receiving mechanism is rotatably supported and arranged on a horizontal plane;

the chromatographic column is supported and arranged above the liquid receiving mechanism;

a vibrating mechanism disposed on an outer wall of the chromatography column;

the rubber sleeve is sleeved outside the vibration structure;

the stirring mechanism is communicated with and arranged above the chromatographic column;

and the two liquid inlet tanks are respectively communicated with the stirring mechanism and are arranged above the stirring mechanism.

Preferably, the method further comprises the following steps:

and the iron support is horizontally arranged, and the liquid receiving mechanism is arranged on the iron support.

Preferably, the chromatography column is fixedly arranged on the iron support.

Preferably, the liquid receiving device includes:

a disc;

the two conveyor belts are respectively arranged on the inner wall and the outer wall of the disc;

and the test tube rack is fixedly arranged on the disc and is coaxial with the disc.

Preferably, the vibration mechanism includes:

and the motor vibration sheets are respectively arranged on the outer wall of the chromatographic column.

Preferably, one end of the chromatographic column is provided with a first cock, the other end of the chromatographic column is provided with a second cock, and the first cock is axially provided with a spiral channel.

Preferably, the method further comprises the following steps:

the liquid discharger is arranged at one end of the chromatographic column and communicated with the first cock;

one end of the first filter is communicated with one end of the liquid discharger;

and one end of the first liquid inlet pump is communicated with the other end of the first filter, and the other end of the first liquid inlet pump is communicated with the stirring mechanism.

Preferably, the stirring device includes:

a stirring tank;

the stirrer is arranged at the bottom of the stirring tank;

and one end of the connecting pipe is arranged in the stirring tank, and the other end of the connecting pipe is communicated with the other end of the first liquid inlet pump.

Preferably, the method further comprises the following steps:

the three-way pipe comprises a vertical end, a first horizontal end and a second horizontal end, wherein the first horizontal end and the second horizontal end are oppositely arranged, the vertical end is communicated with the stirring tank, and the first horizontal end and the second horizontal end are respectively communicated with the liquid inlet tank.

Preferably, a second filter and a second liquid inlet pump are sequentially communicated between the first horizontal end and the liquid inlet tank.

The invention has the following beneficial effects:

1. the micro motor vibration piece is added on the basis of the original common chromatographic column, and in the process that an experimenter fills silica gel and eluent mixture into the chromatographic column, the micro motor vibration piece arranged in a rubber interlayer of the chromatographic column starts to work, so that the silica gel filling surface is smooth under the vibration of the micro motor vibration piece, the bed layer compactness is improved, and bubbles in a system are removed.

2. This device has designed a cock, lets eluant and sample hug closely the chromatographic column inner wall under the action of gravity and flows down, has reduced the impact to the silica gel layer, improves the accuracy of experiment.

3. This device has designed a special test tube conveyer of column chromatography experiment, special test tube conveyer of column chromatography experiment include test tube conveyer belt, peristaltic pump, bee calling organ, four subassemblies of iron stand platform are constituteed. The test tube conveyer belt is of a disc structure, the conveyer belt is arranged on two side walls of a disc, a test tube workbench is arranged above the disc, a plurality of independent test tube racks are arranged on the workbench, and the test tube rack is used for receiving eluent dripped after chromatography. Whether the substances in the eluent are the same or not is distinguished by using a thin layer chromatography, if the substances are the same, the substances are mixed together, and the eluent is evaporated by rotary evaporation, so that the work and complexity of experimenters are reduced.

4. This device has designed an automatic inlet means of laboratory chromatographic column, can detect the liquid level height of eluent in the chromatographic column to the liquid level is according to the liquid feeding volume of actual conditions automatic preparation calculation and control chromatography liquid.

This device has designed a new installation of automatic chromatography separation and purification, can realize the brand-new device that closely links to each other with traditional chromatographic column and automation equipment, the device not only has ordinary column chromatography separation and purification effect, meanwhile this equipment has solved the column chromatography experimentation in silica gel and has loaded, it is loaded down with trivial details to go up the appearance, the eluant is alloted in advance, the eluant is extravagant, flow rate control, the problem that a series of degree of automation such as test tube frequent change is low, no longer need the experimenter to watch for on next door of device always, manpower and time have been saved, the accuracy nature of experiment has been improved, the injury to the experimenter health has been avoided to very big degree.

Drawings

Fig. 1 is a schematic structural diagram of the novel automatic chromatographic separation and purification device of the invention.

Fig. 2 is a schematic view of the first cock according to the present invention.

Detailed Description

The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.

As shown in fig. 1, the present invention provides a novel automatic chromatographic separation and purification apparatus, comprising: the device comprises a first conveyor belt 110, a test tube rack 120, a second conveyor belt 130, a switch 140, a display 150, a speed regulator 160, a buzzer 170, an iron stand 200, a storage battery 310, a peristaltic pump 320, a rubber sleeve 330, a micro motor 340, a chromatography column 350, a first ultrasonic distance detector 360, a liquid discharger 370, a first filter 380, a first liquid inlet pump 390, a stirring tank 410, a second ultrasonic distance detector 420, an audio alarm 430, an air inlet pipe 440, an air filter 450, a three-way pipe 460 and a liquid inlet tank 500.

Iron stand platform 200 sets up on the horizontal plane, connects liquid mechanism to set up on iron stand platform 200, and rotatable support setting of test-tube rack 120 is connecing liquid mechanism top, and chromatography column 350 is fixed to be set up on iron stand platform 200 to be located the top that connects liquid mechanism, vibration mechanism sets up on chromatography column 350's outer wall, still overlaps at vibration mechanism outside and is equipped with the rubber sleeve, avoids the injury to the chromatography column. Rabbling mechanism is linked together with chromatographic column 350's one end, and rabbling mechanism is linked together through three-way pipe 450 and two feed liquor jar 500 simultaneously, and two feed liquor jar 500 settings are in the top of rabbling mechanism, and two feed liquor jar 500 drip into the rabbling mechanism with different solvents in, stir two feed liquor jar inflow rabbling mechanism's liquid through the agitator that sets up in the rabbling mechanism bottom, flow into chromatographic column 350 after the stirring and elute to connect the liquid through connecing liquid mechanism, accomplish the column chromatography experiment.

Connect liquid mechanism to set up on iron stand platform 200, include: the test tube rack comprises a circular disc, a first conveyor belt 110, test tube racks 120 and a second conveyor belt 130, wherein the first conveyor belt 110 is arranged inside the circular disc and is an inner conveyor belt, the second conveyor belt 130 is arranged outside the circular disc and is an outer conveyor belt, and the plurality of test tube racks 110 are respectively arranged on the circular disc at equal intervals and receive eluent dripped after chromatography.

As shown in fig. 2, the chromatography column 350 is fixed to be set up on the iron support, is provided with vibration mechanism in the outside of chromatography column 350, and vibration mechanism includes a plurality of micro motor 340, and a plurality of micro motor 340 evenly arrange in the outside of chromatography column 350, can vibrate the silica gel in the chromatography column, still overlaps in the micro motor 340 outside and is equipped with rubber sleeve 360. One end of the chromatographic column 350 is communicated with a first cock 351, the other end is communicated with a second cock, wherein the second cock is connected with the peristaltic pump 320, and the first cock 351 is radially provided with a spiral channel. The first cock 351 is communicated with one end of the liquid discharger 370, one end of the liquid discharger 370 is further provided with a first ultrasonic detector 360, the other end of the liquid discharger 370 is connected with one end of a first filter 380, the other end of the first filter 380 is communicated with one end of a first liquid inlet pump 390, and the other end of the first liquid inlet pump 390 is communicated with and arranged in the stirring tank 410 through a connecting pipe.

The rabbling mechanism includes: a stirring tank 410, a second ultrasonic distance detector 420, an audio alarm 430, an air inlet pipe 440, an air filter 450 and a three-way pipe 460. At agitator tank 410 bottom, be provided with the agitator, audio alarm 430 sets up the top at agitator tank 410, and the one end intercommunication of intake pipe 440 sets up in agitator tank 410, and the other end has been provided with air cleaner 450. The three-way pipe 460 comprises a vertical end and two opposite horizontal ends, wherein the vertical end of the three-way pipe is arranged in the stirring tank 410, the two horizontal ends are arranged above the stirring tank, and the two horizontal ends are respectively communicated with the liquid inlet tank 500. One end of the second liquid inlet pump is communicated with the liquid inlet tank 500, the other end of the second liquid inlet pump is communicated with one end of a second filter, and one end of the second filter is communicated with the horizontal end of the three-way pipe 460.

Before the experiment, connect liquid mechanism monolithic stationary on iron stand platform 200 that constitutes first conveyer belt 110, test-tube rack 120, second conveyer belt 130, switch 140, display 150, speed regulator 160, bee calling organ 170, and by electric drive, after the chromatographic column 350 adjustment height, fix and connect liquid mechanism stationary on iron stand platform 200, and lie in and connect liquid mechanism top, on the outer wall of chromatographic column 350, evenly arrange a plurality of micro motor pieces 340, the power of micro motor piece 340 is provided by battery 310, and the outside cover at micro motor piece 340 is equipped with rubber sleeve 330, avoid the injury to the chromatographic column. The second stopcock is connected to peristaltic pump 320.

When the experiment starts, adding the prepared mixture of silica gel and eluent into the chromatographic column 350, opening the second cock by the peristaltic pump 320, starting the work of the plurality of micro motor pieces 340 at the same time until the upper surface of the silica gel layer on the page is finished, and screwing the second cock by the peristaltic pump 320; through the operation, the mixture of the silica gel with extremely low density and the washing and dehydrating machine has a smooth surface and is uniform without bubbles, so that the compactness of a bed layer is improved. After the silica gel is filled, the sample is added, and the sample slowly clings to the inner wall of the chromatographic column in a spiral shape under the neutral action of the first cock 351 and flows into the upper surface of the silica gel layer in the chromatographic column 350. After the sample is added, the two liquid inlet tanks 500 respectively start to work through the second liquid inlet pump, and the two liquid inlet tanks 500 enter the stirring tank 410 through the second liquid inlet pump, the second filter and the three-way pipe 460 according to a preset proportion and are mixed through the stirrer to form final eluent.

When liquid enters the agitator tank 410, the second ultrasonic distance probe 420 starts to operate while the agitator at the bottom starts to rotate. If the liquid level in the stirring tank 410 enters the range of the second ultrasonic distance detector 420, the second liquid inlet pumps of the two liquid inlet tanks 500 are closed, and the eluent enters the liquid storage tank above the chromatographic column 350 through the liquid discharger 370, the first liquid inlet pump 390 and the first filter 380, and slowly clings to the inner wall of the chromatographic column 350 in a spiral shape under the neutral action through the first cock 351 to flow into the chromatographic column 350.

There is the liquid level in the liquid storage pipe of first ultrasonic distance detector 360 control liquid storage pipe in the liquid storage pipe, and when the liquid level of liquid storage pipe entered into the detection scope of first ultrasonic distance detector 360, the first feed liquor pump 390 automatic stop of agitator tank 410. After the addition of eluent is complete, the peristaltic pump 320 is adjusted to control the opening of the second stopcock, thereby controlling the flow rate of eluent in the column 350. Open test tube transfer switch 140, display screen 150 will show the operating condition who connects liquid mechanism, confirm to drip the used little periodic time of a test tube, transfer the speed regulator 160 who connects liquid mechanism, the eluant drips into the test tube from the bottom cock of chromatographic column 350, do not drip a test tube fully, first conveyer belt 110 and second conveyer belt 130 drive test tube rack 120 and rotate next receiving test tube, multiple repetition operation, when full by dripping, connect liquid mechanism's bee calling organ 170 to begin to report to the police, remind the experimenter to prepare to change receiving test tube, and then realized the work of laboratory chromatographic separation automatic purification.

While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.