CN102921191A - Multi-path countercurrent grading high-efficiency separation purifying system and method used thereby - Google Patents

Abstract

The invention relates to a high-efficiency separation purifying system and a method used thereby, and especially relates to a multi-path countercurrent grading high-efficiency separation purifying system and a method used thereby. The multi-path countercurrent grading high-efficiency separation purifying system is characterized in that the system comprises a purifying liquid storage tank (1) used for storing a material liquid to be processed, a liquid distribution device (3) connected with the purifying liquid storage tank (1) through a high-pressure material convey pump (2), and a chromatography column system (4) connected with the liquid distribution device (3) and used for separating and purifying the material liquid to be processed. So the multi-path countercurrent grading high-efficiency separation purifying system has the advantages of good purifying effect, high purifying efficiency and the like; and the purifying efficiency on biological effective components is 10-20% higher than that in the prior art.

Description

A multi-channel countercurrent fractionation high-efficiency separation and purification system and its application method

technical field

The invention relates to a high-efficiency separation and purification system and its use method, in particular to a multi-channel countercurrent fractionation high-efficiency separation and purification system and its use method. the

Background technique

In recent years, with the development of science and technology, the development and application of bioactive components has attracted more and more attention from all walks of life. However, the backward separation technology of bioactive components in my country and the low degree of modernization of equipment limit its development. Therefore, it is very important to develop a more popular separation and purification method in order to better improve the purity, reduce impurities, improve production efficiency, reduce production costs, and make bioactive ingredient products have high-quality and low-cost competitiveness. significance. the

Contents of the invention

The present invention mainly solves the technical problems existing in the prior art, and provides the advantages of good purification effect and high purification efficiency; the purification efficiency of biological active ingredients can be increased by 10% to 20% compared with the prior art. A multi-channel countercurrent fractionation and high-efficiency separation and purification system and its application method. the

Above-mentioned technical problem of the present invention is mainly solved by following technical scheme:

A multi-channel countercurrent fractionated high-efficiency separation and purification system is characterized in that it includes a purified liquid storage tank for storing the liquid to be treated, a liquid distributor connected to the purified liquid storage tank through a high-pressure feed pump, and a The liquid distributor is connected to a chromatographic column system for separation and purification of the feed liquid to be treated. the

In the aforementioned multi-channel countercurrent fractionation high-efficiency separation and purification system, the chromatographic column system includes chromatographic column Z1, chromatographic column Z2 ... chromatographic column Zn; the first storage tank, the second storage tank ... the nth storage tank; the top of the chromatography column Z1, the chromatography column Z2 ... the chromatography column Zn is respectively connected to the liquid distributor through the three-way valve J1, the three-way valve J2 ... the three-way valve Jn; the three-way The valve J1 communicates with the first storage tank through the two-way valve CH1 and the two-way valve B1 connected in series, and the three-way valve J2 communicates with the second storage tank through the two-way valve CH2 and the two-way valve B2 connected in series. Communication... The three-way valve Jn communicates with the nth storage tank through the two-way valve CHn and the two-way valve Bn connected in series in sequence; a two-way valve is also provided between the two-way valve CH2 and the two-way valve B2 N1, a two-way valve N2 is also provided between the two-way valve CH3 and the two-way valve B3... A two-way valve Nn-1, the two-way valve Nn-1 is also provided between the two-way valve CHn and the two-way valve Bn There is also a two-way valve Nn between the one-way valve CH1 and the two-way valve B1; the bottom end of the chromatography column Z1 communicates with the three-way valve J1 and the three-way valve N1 through the three-way valve C1 at the same time, and the chromatography column Z2 The bottom end communicates with the three-way valve J2 and the three-way valve N2 through the three-way valve C2 at the same time. The bottom end of the chromatography column Zn communicates with the three-way valve Jn and the three-way valve Nn through the three-way valve Cn at the same time. the

A method for using a multi-channel countercurrent fractionation and high-efficiency separation and purification system, characterized in that it comprises the following steps:

Step A1, the feed liquid to be treated is stored in the purified liquid storage tank, the three-way valve J1 is connected from the left to the right, the three-way valve J2...Jn-1 is connected from the left to the bottom, and the three-way valve Jn is from the right to the bottom. , the three-way valve C1...Cn-1 is connected from the top to the right, the three-way valve Cn is connected from the top to the bottom, the valve CH1 is closed, the valve CH2...CHn is connected, the valve B1 is connected, the valve B2...Bn is closed, the valve N1... Nn connected;

Step A2, the feed liquid enters the chromatography column Z1 from the top of the chromatography column Z1 through the valve J1, discharges the material from the bottom of the chromatography column Z1, enters Z2 through the valves C1, N1, and CH2 until Zn, and the remaining liquid is absorbed by the chromatography The material discharged from the bottom of the column Zn enters the first storage tank through the valves Cn, Nn, and B1 to complete the component adsorption operation. the

A method for using a multi-channel countercurrent fractionation and high-efficiency separation and purification system, characterized in that it comprises the following steps:

Step B1, connect the three-way valves J1...Jn to the left and right, the three-way valves C1...Cn-1 are connected to the top and the right to go out, the three-way valve Cn is connected to the top and bottom, the valves CH1...CHn are closed, and the valves B1... Bn is connected, valve N1...Nn is connected;

Step B2, the eluting solvent enters the chromatography column Z1...Zn from the top of the chromatography column Z1...Zn through the three-way valve J1...Jn respectively, passes through the chromatography column Z1...Zn, and the analytical solution flows from the bottom of the chromatography column Z1...Zn respectively End discharge, through the two-way valve N1...two-way valve Nn, two-way valve B2...two-way valve Bn, two-way valve B2, respectively into the second storage tank...the nth storage tank to complete the downstream elution of components operate. the

A method for using a multi-channel countercurrent fractionation and high-efficiency separation and purification system, characterized in that it comprises the following steps:

Step C1, the three-way valve J1...Jn is connected to the left and the bottom is out, the three-way valve C1...Cn is connected to the left and the top is out, the two-way valve CH1...the two-way valve CHn is connected, the two-way valve B1...the two-way valve Bn On, the two-way valves N1...Nn are closed. The elution solvent enters the chromatography column Z1...Zn from the bottom of the chromatography column Z1...Zn through the valve J1...Jn, and passes through the chromatography column Z1...Zn;

Step C2, the analytical solution is discharged from the top of the chromatography column Z1...Zn respectively, and enters the first storage tank...the nth storage tank through the two-way valve CH1...the two-way valve CHn, the two-way valve B1...the two-way valve Bn respectively , to complete the component countercurrent elution operation. the

Therefore, the present invention has the following advantages: good purification effect and high purification efficiency; the purification efficiency of biological active ingredients can be increased by 10% to 20% compared with the prior art. the

Description of drawings

Accompanying drawing 1 is a kind of structural principle schematic diagram of the present invention;

Detailed ways

The technical solutions of the present invention will be further specifically described below through the embodiments and in conjunction with the accompanying drawings. the

Example 1:

A multi-channel countercurrent fractionated high-efficiency separation and purification system, including a purified liquid storage tank 1 for storing the liquid to be treated, a liquid distributor 3 connected to the purified liquid storage tank 1 through a high-pressure feed pump 2, and a The liquid distributor 3 is connected to a chromatographic column system 4 for separation and purification of the feed liquid to be treated. the

The chromatography column system 4 includes a chromatography column Z1, a chromatography column Z2 ... a chromatography column Zn; a first storage tank, a second storage tank ... an nth storage tank; the chromatography column Z1, a chromatography column Z2 ... ...the top of the chromatography column Zn is connected to the liquid distributor 3 through the three-way valve J1, the three-way valve J2...the three-way valve Jn; The valve B1 communicates with the first storage tank, and the three-way valve J2 communicates with the second storage tank through the two-way valve CH2 and the two-way valve B2 connected in series in sequence... The three-way valve Jn communicates with the second storage tank through the sequentially connected series The two-way valve CHn and the two-way valve Bn communicate with the nth storage tank; the two-way valve N1, the two-way valve CH3 and the two-way valve B3 are also arranged between the two-way valve CH2 and the two-way valve B2 There is also a two-way valve N2 between the two-way valve Nn-1 between the two-way valve CHn and the two-way valve Bn, and a two-way valve Nn-1 between the two-way valve CH1 and the two-way valve B1. Two-way valve Nn; the bottom end of the chromatography column Z1 communicates with the three-way valve J1 and the three-way valve N1 through the three-way valve C1 at the same time, and the bottom end of the chromatography column Z2 communicates with the three-way valve J2 through the three-way valve C2 at the same time It communicates with the three-way valve N2... The bottom end of the chromatography column Zn communicates with the three-way valve Jn and the three-way valve Nn through the three-way valve Cn at the same time

In this embodiment, the method of use includes the following steps:

Step A1, the feed liquid to be treated is stored in the purified liquid storage tank 1, the three-way valve J1 is connected from the left to the right, the three-way valve J2...Jn-1 is connected from the left to the bottom, and the three-way valve Jn is from the right to the bottom Out, the three-way valve C1...Cn-1 is connected up and right out, the three-way valve Cn is connected up and down, the valve CH1 is closed, the valve CH2...CHn is connected, the valve B1 is connected, the valve B2...Bn is closed, and the valve N1 ...Nn connected;

Step A2, the feed liquid enters the chromatography column Z1 from the top of the chromatography column Z1 through the valve J1, discharges the material from the bottom of the chromatography column Z1, enters Z2 through the valves C1, N1, and CH2 until Zn, and the remaining liquid is absorbed by the chromatography The material discharged from the bottom of the column Zn enters the first storage tank through the valves Cn, Nn, and B1 to complete the component adsorption operation. the

Example 2:

The difference from Example 1 is that the chromatographic columns Z1...Zn are connected in parallel, and the eluting solvent enters the bottom end from the top of the chromatographic column Z1...Zn to discharge, and the components are eluted in a downstream operation, which specifically includes the following steps:

Step B1, connect the three-way valves J1...Jn to the left and right, the three-way valves C1...Cn-1 are connected to the top and the right to go out, the three-way valve Cn is connected to the top and bottom, the valves CH1...CHn are closed, and the valves B1... Bn is connected, valve N1...Nn is connected;

Step B2, the eluting solvent enters the chromatography column Z1...Zn from the top of the chromatography column Z1...Zn through the three-way valve J1...Jn respectively, passes through the chromatography column Z1...Zn, and the analytical solution flows from the bottom of the chromatography column Z1...Zn respectively End discharge, through the two-way valve N1...two-way valve Nn, two-way valve B2...two-way valve Bn, two-way valve B2, respectively into the second storage tank...the nth storage tank to complete the downstream elution of components operate. the

Example 3:

The difference from Example 2 is that the chromatographic columns Z1...Zn are connected in parallel, and the eluting solvent enters the top from the bottom of the chromatographic column Z1...Zn and discharges, which is a countercurrent elution operation for components, specifically including the following steps:

Step C1, the three-way valve J1...Jn is connected to the left and the bottom is out, the three-way valve C1...Cn is connected to the left and the top is out, the two-way valve CH1...the two-way valve CHn is connected, the two-way valve B1...the two-way valve Bn On, the two-way valves N1...Nn are closed. The elution solvent enters the chromatography column Z1...Zn from the bottom of the chromatography column Z1...Zn through the valve J1...Jn, and passes through the chromatography column Z1...Zn;

Step C2, the analytical solution is discharged from the top of the chromatography column Z1...Zn respectively, and enters the first storage tank...the nth storage tank through the two-way valve CH1...the two-way valve CHn, the two-way valve B1...the two-way valve Bn respectively , to complete the component countercurrent elution operation. In this embodiment, the chromatographic column system can be 6, and ethanol is used for gradient elution, with concentrations of 0%, 20%, 40%, 60%, 80%, and 100%, and the amount of each gradient solvent is 2 times the column volume , a sample is collected for every 1/4 column volume, and a total of 288 samples can be obtained. the

The specific embodiments described herein are merely illustrative of the spirit of the invention. Those skilled in the art to which the present invention belongs can make various modifications or supplements to the described specific embodiments or adopt similar methods to replace them, but they will not deviate from the spirit of the present invention or go beyond the definition of the appended claims range. the

Although terms such as purified liquid storage tank 1, high-pressure feed pump 2, liquid distributor 3, and chromatography column system 4 are frequently used in this paper, the possibility of using other terms is not excluded. These terms are used only for the purpose of describing and explaining the essence of the present invention more conveniently; interpreting them as any kind of additional limitation is against the spirit of the present invention. the

Claims (5)

1. the efficient separation and purification of multi-path counter-current fractionation system, it is characterized in that, comprise the liquid distributor (3) that links to each other with described refined solution storage tank (1) be used to the refined solution storage tank (1) of storing pending feed liquid, by a high pressure dehvery pump (2) and link to each other for the chromatography column system (4) of pending feed liquid separation and purification with described liquid distributor (3).

2. the efficient separation and purification of a kind of multi-path counter-current fractionation according to claim 1 system is characterized in that described chromatography column system (4) comprises chromatographic column Z1, chromatographic column Z2 ... chromatographic column Zn; The 1st storage tank, the 2nd storage tank ... the n storage tank; Described chromatographic column Z1, chromatographic column Z2 ... chromatographic column Zn top is respectively by triple valve J1, triple valve J2 ... triple valve Jn is connected with described liquid distributor (3); Two-port valve CH1 and the two-port valve B1 that described triple valve J1 passes through successively series connection is communicated with described the 1st storage tank, described triple valve J2 is communicated with described the 2nd storage tank by two-port valve CH2 and the two-port valve B2 that connects successively ... described triple valve Jn is communicated with described n storage tank by two-port valve CHn and the two-port valve Bn of successively series connection; Also be provided with between described two-port valve CH2 and the two-port valve B2 between two-port valve N1, described two-port valve CH3 and the two-port valve B3 and also be provided with two-port valve N2 ... also be provided with between described two-port valve CHn and the two-port valve Bn between two-port valve Nn-1, described two-port valve CH1 and the two-port valve B1 and also be provided with two-port valve Nn; Described chromatographic column Z1 bottom by triple valve C1 is communicated with triple valve J1 and triple valve N1 simultaneously, described chromatographic column Z2 bottom is communicated with triple valve J2 and triple valve N2 by the triple valve C2 while ... described chromatographic column Zn bottom is communicated with triple valve Jn and triple valve Nn by triple valve Cn simultaneously.

3. the using method of the efficient separation and purification of a multi-path counter-current fractionation claimed in claim 1 system is characterized in that, may further comprise the steps:

Steps A 1, pending feed liquid are stored in the refined solution storage tank (1), the right side is entered on a triple valve J1 left side to be gone out to connect, triple valve J2 ... go out to connect under Jn-1 advances on a left side, go out triple valve C1 under triple valve Jn advances on the right side ... the enterprising right side of Cn-1 goes out to connect, triple valve Cn upper entering and lower leaving is connected, valve CH1 is closed, valve CH2 ... CHn connects, and valve B1 connects, valve B2 ... Bn is closed, valve N1 ... Nn connects;

Steps A 2, feed liquid is entered chromatographic column Z1 from valve J1 by chromatographic column Z1 top, from chromatographic column Z1 bottom discharging, enter Z2 through valve C1, N1, CH2, until Zn, the absorption raffinate is entered in the 1st storage tank through valve Cn, Nn, B1 by chromatographic column Zn bottom discharging, finishes the component adsorption operations.

4. the using method of the efficient separation and purification of a multi-path counter-current fractionation claimed in claim 1 system is characterized in that, may further comprise the steps:

Step B1, with triple valve J1 ... Jn enters on a left side right side and goes out to connect triple valve C1 ... the enterprising right side of Cn-1 goes out to connect, and triple valve Cn upper entering and lower leaving is connected, valve CH1 ... CHn is closed, valve B1 ... Bn connects, valve N1 ... Nn connects;

Step B2, with eluting solvent respectively from triple valve J1 ... Jn is by chromatographic column Z1 ... the Zn top enters chromatographic column Z1 ... Zn, through chromatographic column Z1 ... Zn, desorbed solution is respectively by chromatographic column Z1 ... the discharging of Zn bottom, through two-port valve N1 ... two-port valve Nn, two-port valve B2 ... two-port valve Bn, two-port valve B2, enter the 2nd storage tank respectively ... in the n storage tank, finish the operation of component following current wash-out.

5. the using method of the efficient separation and purification of a multi-path counter-current fractionation claimed in claim 1 system is characterized in that, may further comprise the steps:

Step C1, triple valve J1 ... under advancing on a left side, Jn goes out to connect triple valve C1 ... on advancing on a left side, Cn goes out to connect two-port valve CH1 ... two-port valve CHn connects, two-port valve B1 ... two-port valve Bn connects, two-port valve N1 ... Nn is closed.Eluting solvent is respectively from valve J1 ... Jn is by chromatographic column Z1 ... the Zn bottom enters chromatographic column Z1 ... Zn is through chromatographic column Z1 ... Zn;

Step C2, with desorbed solution respectively by chromatographic column Z1 ... the discharging of Zn top is through two-port valve CH1 ... two-port valve CHn, two-port valve B1 ... two-port valve Bn enters respectively the 1st storage tank ... in the n storage tank, finish the operation of component adverse current wash-out.

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