CN111389051A - A kind of chromatographic separation system and its application, a kind of separation method of mannose - Google Patents

Abstract

The invention discloses a chromatographic separation system and application thereof, and a separation method of mannose, and belongs to the technical field of substance separation. The chromatographic separation system comprises a water inlet system, a feeding system, two chromatographic separation systems and a first liquid outlet system, wherein the water inlet system is respectively communicated with water inlets of the two chromatographic separation systems, the feeding system is respectively communicated with feed inlets of the two chromatographic separation systems, and the first liquid outlet system is respectively communicated with liquid outlets of the two chromatographic separation systems, which are used for outputting extracting solutions. By comprehensive utilization of two sets of chromatographic separation systems, the mannose separating system can be used for separating mannose, so that mannose products with high purity and high yield can be obtained, and economic benefits are improved. Inputting the mannose-containing raw materials to be separated and water into a first chromatographic separation system by adopting the chromatographic separation system, and separating to obtain an extracting solution; and (3) inputting the water and the extracting solution obtained by separating the first chromatographic separation system into a second chromatographic separation system, and separating to obtain mannose. The method is simple and easy to operate.

Description

A kind of chromatographic separation system and its application, a kind of separation method of mannose

technical field

The invention relates to the technical field of material separation, in particular to a chromatographic separation system and application thereof, and a method for separating mannose.

Background technique

Mannose is a very important six-carbon sugar with high viscosity and is widely used in medicine, food and other industries. The mixture of mannose is composed of 25% mannose, about 74% fructose and a small amount of miscellaneous sugars. Mannose and fructose are isomers. In the spectral analysis of the liquid phase, the chromatographic peaks of the two are very close, the resolution is less than 0.3, and the resolution is low, so in the normal production process, it is difficult to It is difficult to separate these two substances well, such as using crystallization, nanofiltration membrane, conventional chromatography and other separation methods. First, it is difficult to operate; second, it is difficult to achieve high purity after separation.

Therefore, the extraction method is still the main method for large-scale production at present, but this method has low efficiency, low extract purity and yield, and it is difficult to obtain higher economic benefits.

In view of this, the present invention is proposed.

SUMMARY OF THE INVENTION

One of the objectives of the present invention includes providing a chromatographic separation system, which fundamentally solves the problem that it is difficult to separate two similar substances in a mixture through the comprehensive utilization of two sets of chromatographic separation systems.

The second object of the present invention includes providing an application of the above-mentioned chromatographic separation system, which is used for separating mannose, especially for separating the mannose in the mixed solution of mannose and fructose, which can obtain high purity and high yield. rate of mannose products, improve economic efficiency.

The third object of the present invention includes providing a method for separating mannose, which is simple, easy to operate, low in cost, and high in purity and yield of mannose after separation.

The present invention is realized in this way:

In the first aspect, the present application provides a chromatographic separation system, including a water inlet system, a feed system, a first chromatographic separation system, a second chromatographic separation system, and a first liquid outlet system. The water inlet system is respectively connected with two chromatographic separation systems. The water inlets of the two chromatographic separation systems are respectively communicated with the feeding ports of the two chromatographic separation systems.

The part of the first liquid outlet system for outputting the extract obtained by the first chromatographic separation system is in communication with the part of the feed system for inputting the raw material to the second chromatographic separation system so that the extraction obtained by the first chromatographic separation system is separated The liquid is fed into the second chromatographic separation system as a raw material.

In an optional embodiment, the chromatographic separation system further includes a first evaporative concentration system, and the discharge port of the first evaporative concentration system is connected to the part of the feeding system for connecting with the first chromatographic separation system, so as to The material to be separated after being evaporated and concentrated by the first evaporative concentration system enters the first chromatographic separation system for the first chromatographic separation.

In an optional embodiment, the chromatographic separation system further includes a second evaporative concentration system, and the portion of the first liquid outlet system for outputting the extract obtained by the first chromatographic separation system and the feed port of the second evaporative concentration system communication, and the material outlet of the second evaporative concentration system is communicated with the part of the feed system for inputting raw materials to the second chromatographic separation system.

In an optional embodiment, the chromatographic separation system further includes a second liquid outlet system, and the second liquid outlet systems are respectively communicated with the liquid outlets for outputting the raffinate of the two chromatographic separation systems.

In an optional embodiment, the chromatographic separation system further comprises an enzyme conversion system, and the part of the second liquid outlet system for outputting the raffinate obtained by the separation of the first chromatographic separation system is communicated with the feed port of the enzyme conversion system, and the enzyme The outlet of the conversion system is in communication with the portion of the feed system for inputting feedstock to the first chromatographic separation system.

In an optional embodiment, the part of the second liquid outlet system for outputting the raffinate obtained by the separation of the second chromatographic separation system communicates with the part of the feed system for inputting raw materials to the first chromatographic separation system, so that the The raffinate separated by the second chromatographic separation system is input into the first chromatographic separation system as a raw material.

In an optional embodiment, the first chromatographic separation system includes at least 6 first chromatographic columns, and the at least 6 first chromatographic columns are connected end-to-end through the first circulation pipeline to form a loop system. The circulation pipelines between the first chromatographic columns are equipped with circulating pumps. The water inlet system and the feed system are respectively connected with the water inlet and the feed port of each first chromatographic column through valves. The first liquid outlet system and the second The liquid outlet system is respectively communicated with the liquid outlet of the extraction liquid and the liquid outlet of the raffinate of each first chromatographic column through valves.

In an optional embodiment, the second chromatographic separation system includes at least 6 second chromatographic columns, and the at least 6 second chromatographic columns are connected end-to-end through the second circulation pipeline to form a loop system. The circulation pipeline between the two chromatographic columns is equipped with a circulating pump. The water inlet system and the feeding system are respectively connected with the water inlet and the feeding port of each second chromatographic column through valves. The liquid outlet system is respectively communicated with the liquid outlet of the extraction liquid and the liquid outlet of the raffinate of each second chromatographic column through valves.

In a second aspect, the present application provides the application of the chromatographic separation system according to any one of the foregoing embodiments, wherein the chromatographic separation system is used to separate mannose in a mixed solution of mannose and fructose.

In a third aspect, the present application provides a method for separating mannose, comprising the following steps: using the chromatographic separation system according to any one of the foregoing embodiments, passing the raw material to be separated and water containing mannose through the feeding system and the water, respectively The system is input into the first chromatographic separation system, and the separated extract is output from the first liquid outlet system;

The water and the extract obtained by the first chromatographic separation system are respectively input into the second chromatographic separation system through the water inlet system and the feed system, and the separated mannose is output from the first liquid outlet system;

Preferably, when the chromatographic separation system includes the second liquid outlet system, the raffinate obtained by the separation of the first chromatographic separation system is input into the first chromatographic separation system for separation through the feeding system after enzymatic conversion treatment;

Preferably, the raffinate obtained by the second chromatographic separation system is input into the feed system through the second liquid outlet system as the raw material and input into the first chromatographic separation system for separation.

Preferably, the water is pure water.

Preferably, the purity of the isolated mannose is 97-99%, more preferably 98%.

Preferably, the yield of isolated mannose is 55-65%, more preferably 60%.

The present invention has the following beneficial effects:

In the present application, through the comprehensive utilization of two sets of chromatographic separation systems, the raw materials to be separated and water containing mannose are input into the first chromatographic separation system to obtain an extract; the extract obtained by the first chromatographic separation system is input into the second chromatograph The separation system can separate and obtain mannose, which can obtain high-purity and high-yield mannose products and improve economic benefits. The process equipment has low investment, simple operation and high degree of automation, which fundamentally solves the disadvantages of traditional equipment, such as large investment, complex process route and inconvenient operation. The corresponding separation method is simple and easy to operate.

Description of drawings

In order to illustrate the technical solutions of the embodiments of the present invention more clearly, the following briefly introduces the accompanying drawings used in the embodiments. It should be understood that the following drawings only show some embodiments of the present invention, and therefore do not It should be regarded as a limitation of the scope, and for those of ordinary skill in the art, other related drawings can also be obtained according to these drawings without any creative effort.

1 is a schematic structural diagram of the chromatographic separation system provided in Example 1.

Description of reference numerals: 100-chromatographic separation system; 10-water inlet system; 20-feeding system; 30-first chromatographic separation system; 40-second chromatographic separation system; 50-first liquid outlet system; 60-th Two-outlet system; 300-first chromatographic column; 301-first chromatographic column A; 302-first chromatographic column B; 303-first chromatographic column C; 304-first chromatographic column D; 305-first chromatographic column E; 306-first chromatographic column F; 400-second chromatographic column; 401-second chromatographic column A; 402-second chromatographic column B; 403-second chromatographic column C; 404-second chromatographic column D; 405 -Second chromatographic column E; 406-Second chromatographic column F; 71-First circulation pipeline; 72-Second circulation pipeline; 11-Water inlet manifold; 12-Water inlet branch pipe; 21-First feed manifold ; 22- the first feed branch pipe; 23- the second feed branch pipe; 24- the second feed branch pipe; 51- the first liquid outlet pipe A; 52- the first liquid outlet branch pipe A; B; 54 - the first liquid outlet branch pipe B; 61 - the second liquid outlet main pipe A; 62 - the second liquid outlet branch pipe A; 63 - the second liquid outlet main pipe B; 64 - the second liquid outlet branch pipe B; 80 - the valve .

Detailed ways

In order to make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be described clearly and completely below. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used without the manufacturer's indication are conventional products that can be purchased from the market.

The features and performances of the present invention will be further described in detail below in conjunction with the embodiments.

Example 1

This embodiment proposes a chromatographic separation system 100, please refer to FIG. 1, which includes a water inlet system 10, a feeding system 20, a first chromatographic separation system 30, a second chromatographic separation system 40, and a first liquid outlet system 50. The water system 10 is respectively connected with the water inlets of the two chromatographic separation systems, the feed system 20 is respectively connected with the feed ports of the two chromatographic separation systems, and the first liquid outlet system 50 is respectively connected with the two chromatographic separation systems for output extraction. The liquid outlet is connected.

In an optional embodiment, the first chromatographic separation system 30 includes at least 6 first chromatographic columns 300, and the at least 6 first chromatographic columns 300 are connected in sequence through the first circulation pipeline 71 to form a loop system. The circulation pipeline between the adjacent two first chromatographic columns 300 is provided with a circulating pump, and the water inlet system 10 and the feeding system 20 are respectively connected with the water inlet and the feeding port of each first chromatographic column 300 through the valve 80 correspondingly. , the first liquid outlet system 50 and the second liquid outlet system 60 are respectively communicated with the liquid outlet of the extraction liquid and the liquid outlet of the raffinate of each first chromatographic column 300 through the valve 80 correspondingly.

For reference, the first chromatographic separation system 30 has six first chromatographic columns 300, which are respectively a first chromatographic column A301, a first chromatographic column B302, a first chromatographic column C303, a first chromatographic column D304, and a first chromatographic column E305. And the first chromatographic column F306 represents. The above-mentioned six first chromatographic columns 300 correspond to four functional zones in total, including one Z1 zone, two Z2 zones, two Z3 zones and one Z4 zone, wherein the Z1 zone is the analysis zone, the Z2 zone is the separation zone, Zone Z3 is the adsorption zone, and zone Z4 is the isolation zone. The first chromatographic column A301 to the first chromatographic column F306 are sequentially connected end to end through the first circulation pipeline 71 to form a loop chromatographic separation system. In the actual operation process, the materials entering and leaving the system are realized through the continuous switching of the above four functional areas.

In an optional embodiment, the second chromatographic separation system 40 includes at least 6 second chromatographic columns 400, and the at least 6 second chromatographic columns 400 are connected to each other through the second circulation pipeline 72 to form a loop system. The circulation pipeline between the two adjacent second chromatographic columns 400 is provided with a circulating pump, and the water inlet system 10 and the feeding system 20 are respectively connected with the water inlet and the feeding port of each second chromatographic column 400 through the valve 80 correspondingly. , the first liquid outlet system 50 and the second liquid outlet system 60 are respectively communicated with the liquid outlet of the extraction liquid and the liquid outlet of the raffinate of each second chromatographic column 400 through the valve 80 correspondingly.

For reference, the second chromatographic separation system 40 has 6 second chromatographic columns 400, which are respectively a second chromatographic column A401, a second chromatographic column B402, a second chromatographic column C403, a second chromatographic column D404, and a second chromatographic column E405. And the second chromatographic column F406 represents. Similarly, the above-mentioned six second chromatographic columns 400 correspond to four functional zones in total, including one Z1 zone, two Z2 zones, two Z3 zones and one Z4 zone, wherein the Z1 zone is the analytical zone and the Z2 zone For the separation zone, the Z3 zone is the adsorption zone, and the Z4 zone is the isolation zone. The second chromatographic column A401 to the second chromatographic column F406 are connected in sequence through the second circulation pipeline 72 to form a loop system. In the actual operation process, the materials entering and leaving the system are realized through the continuous switching of the above four functional areas.

The water inlet system 10 includes a water inlet main pipe 11 and a plurality of water inlet branch pipes 12, and the plurality of water inlet branch pipes 12 are arranged in parallel. The water outlets of the branch pipes 12 are respectively communicated with the water inlets of the first chromatographic column A301 to the first chromatographic column F306 and the second chromatographic column A401 to the second chromatographic column F406. During operation, water is first supplied to the water inlet main pipe 11 , and the water inlet main pipe 11 then inputs water into each chromatographic column through a plurality of water inlet branch pipes 12 . A valve 80 is provided between each water inlet branch pipe 12 and the water inlet of the chromatographic column. It is worth noting that in this embodiment, the two chromatographic separation systems share a water inlet system 10, and the pipeline of the water inlet system 10 can also be provided with a chromatographic inlet pump controlled by frequency conversion, which can save electricity and solve the problem of The problem of large pressure fluctuations when the chromatography enters the water.

The feeding system 20 includes a first feeding manifold 21 , a plurality of first feeding branch pipes 22 , a second feeding manifold 23 and a plurality of second feeding branch pipes 24 .

A plurality of first feeding branch pipes 22 are arranged in parallel, the feeding port of each first feeding branch pipe 22 is connected with the discharging port of the first feeding main pipe 21, and the discharging ports of the plurality of first feeding branch pipes 22 are respectively It communicates with the feed ports of the first chromatographic column A301 to the first chromatographic column F306. A valve 80 is provided between each of the first feed branch pipes 22 and the feed port of the first chromatographic column 300 .

A plurality of second feeding branch pipes 24 are arranged in parallel, the feeding port of each second feeding branch pipe 24 is connected with the discharging port of the second feeding main pipe 23, and the discharging ports of the plurality of second feeding branch pipes 24 are respectively It communicates with the feed ports of the second chromatographic column A401 to the second chromatographic column F406. A valve 80 is provided between each second feed branch pipe 24 and the feed port of the second chromatographic column 400 . The first liquid outlet system 50 includes a first liquid outlet main pipe A51, a plurality of first liquid outlet branch pipes A52, a first liquid outlet main pipe B53, and a plurality of first liquid outlet branch pipes B54.

A plurality of first liquid outlet branch pipes A52 are arranged in parallel, and the liquid inlets of the plurality of first liquid outlet branch pipes A52 are respectively connected with the liquid outlet ports of the plurality of first chromatographic columns 300 for outputting the extraction liquid in one-to-one correspondence. The liquid outlet of the first liquid outlet branch pipe A52 is connected with the liquid inlet of the first liquid outlet main pipe A51. A valve 80 is provided between each first liquid outlet branch pipe A52 and the liquid outlet of the first chromatographic column 300 for outputting the extraction liquid.

A plurality of first liquid outlet branch pipes B54 are arranged in parallel, and the liquid inlets of the plurality of first liquid outlet branch pipes B54 are respectively connected with the liquid outlet ports of the plurality of second chromatographic columns 400 for outputting the extraction liquid in one-to-one correspondence. The liquid outlet of a liquid outlet branch pipe B54 is all communicated with the liquid inlet of the first liquid outlet main pipe B53. A valve 80 is provided between each of the first liquid outlet branch pipes B54 and the liquid outlet of the second chromatographic column 400 for outputting the extraction liquid.

In an optional embodiment, the part of the first liquid outlet system 50 used to output the extract obtained by the first chromatographic separation system 30 and the part of the feed system 20 used to input raw materials to the second chromatographic separation system 40 Communication is carried out so that the extract obtained by the separation of the first chromatographic separation system 30 is input into the second chromatographic separation system 40 as a raw material.

Specifically, the liquid outlet of the first liquid outlet manifold A51 is communicated with the feed inlet of the second feed manifold 23 , that is, the extract separated by the first chromatographic separation system 30 continues to be used as the raw material of the second chromatographic separation system 40 to separate.

The liquid flowing out of the first liquid outlet manifold B53 is the separated high-purity mannose (purity can reach more than 98).

During operation, the raw materials to be separated are first input into the first feed manifold 21 , and the first feed manifold 21 then passes through the plurality of first feed branch pipes 22 to respectively input the raw materials into the plurality of first chromatographic columns 300 . The extraction liquid separated by the first chromatographic separation system 30 is collected in the first liquid outlet manifold A51 through a plurality of first liquid outlet branch pipes A52, and then correspondingly inputted through the second feed manifold 23 and a plurality of second feed branch pipes 24. to the plurality of second chromatographic columns 400 . The extraction liquid separated by the second chromatographic separation system 40 is collected in the first liquid outlet main pipe B53 through a plurality of first liquid outlet branch pipes B54 to obtain the separated mannose.

In an optional embodiment, the chromatographic separation system 100 of this embodiment may further include a first evaporative concentration system (not shown in the figure), and the outlet of the first evaporative concentration system and the feeding system 20 are used to communicate with the first evaporative concentration system. The connected part of the chromatographic separation system 30 (ie, the first feed manifold 21 ) is connected to enter the first chromatographic separation system 30 for the first chromatographic separation of the material to be separated after being evaporated and concentrated by the first evaporative concentration system.

In an optional embodiment, the chromatographic separation system 100 of this embodiment may further include a second evaporation and concentration system (not shown), and the first liquid outlet system 50 is used to output the extraction obtained by the first chromatographic separation system 30 The liquid part communicates with the feed port of the second evaporative concentration system, and the outlet port of the second evaporative concentration system communicates with the part of the feed system 20 for inputting raw materials to the second chromatographic separation system 40 . That is, the liquid outlet of the first liquid outlet manifold A51 is communicated with the feed port of the second evaporative concentration system, and the outlet port of the second evaporative concentration system is communicated with the feed port of the second feed manifold 23 .

The extract obtained by the first chromatographic separation system 30 is concentrated by the second evaporation and enters the second chromatographic separation system 40 for further purification, and a mannose product with a purity of more than 98% can be obtained.

In an optional embodiment, the chromatographic separation system 100 further includes a second liquid outlet system 60, and the second liquid outlet system 60 is respectively communicated with the liquid outlets of the two chromatographic separation systems for outputting the raffinate.

The second liquid outlet system 60 includes a second liquid outlet main pipe A61, a plurality of second liquid outlet branch pipes A62, a second liquid outlet main pipe B63, and a plurality of second liquid outlet branch pipes B64.

A plurality of second liquid outlet branch pipes A62 are arranged in parallel, and the liquid inlets of the plurality of second liquid outlet branch pipes A62 are respectively connected with the liquid outlet ports of the plurality of first chromatographic columns 300 for outputting the raffinate in one-to-one correspondence. The liquid outlets of the second liquid outlet branch pipes A62 are all communicated with the liquid inlets of the second liquid outlet main pipe A61. A valve 80 is provided between each second liquid outlet branch pipe A62 and the liquid outlet of the first chromatographic column 300 for outputting the raffinate.

A plurality of second liquid outlet branch pipes B64 are arranged in parallel, and the liquid inlets of the plurality of second liquid outlet branch pipes B64 are respectively connected with the liquid outlet ports of the plurality of second chromatographic columns 400 for outputting the raffinate in one-to-one correspondence. The liquid outlet ports of the second liquid outlet branch pipes B64 are all communicated with the liquid inlet ports of the second liquid outlet main pipe B63. A valve 80 is provided between each second liquid outlet branch pipe B64 and the liquid outlet of the second chromatographic column 400 for outputting the extraction liquid.

In an optional embodiment, the chromatographic separation system 100 further includes an enzymatic conversion system (not shown in the figure), and the second liquid outlet system 60 is used for outputting the part of the raffinate obtained by the separation of the first chromatographic separation system 30 to be converted with the enzyme The inlet of the system is communicated with, and the outlet of the enzymatic conversion system is communicated with the part of the feeding system 20 for inputting raw materials to the first chromatographic separation system 30 .

That is, the liquid outlet of the first liquid outlet manifold A51 is communicated with the liquid inlet of the enzyme conversion system, and the liquid outlet of the enzyme conversion system is communicated with the feed port of the first feed manifold 21, that is, the first chromatographic separation system 30. The separated raffinate can be used as the raw material of the first chromatographic separation system 30 after enzymatic conversion.

The above operation is due to the fact that the fructose content in the raffinate obtained by the first chromatographic separation system 30 is relatively high, and it is converted into mannose by using an enzyme to continue to be used as the raw material of the second chromatographic separation system 40, that is, the by-product raffinate is about to be used. After conversion, it can be reused, thus reducing the cost to a great extent.

Further, in an optional embodiment, the part of the second liquid outlet system 60 used to output the raffinate obtained by the second chromatographic separation system 40 and the feeding system 20 are used to feed the first chromatographic separation system 30 Parts of the input feedstock are communicated so that the raffinate separated by the second chromatographic separation system 40 is fed into the first chromatographic separation system 30 as feedstock.

That is, the liquid outlet of the second liquid outlet manifold B63 can be communicated with the feed port of the first feed manifold 21, that is, the raffinate obtained by the second chromatographic separation system 40 is continued as the raw material of the first chromatographic separation system 30. use.

It is worth noting that the raffinate obtained by the separation of the second chromatographic separation system 40 can also be converted by an enzyme conversion system before being input into the first chromatographic separation system 30 as a raw material, and then reused as a raw material of the first chromatographic separation system 30. .

For reference, the valves 80 involved in this embodiment can all be self-controlled on-off ball valves.

Example 2

This example provides an application of the chromatographic separation system 100 as in Example 1, which is used to separate mannose in a mixture of mannose and fructose. The mixture is mainly composed of about 25% of mannose, about 74% of fructose and a small amount of miscellaneous sugars.

The specific separation steps include: using the above-mentioned chromatographic separation system 100, the mixed solution containing mannose and pure water are respectively input into the first chromatographic separation system 30 through the feeding system 20 and the water feeding system 10, and output from the first liquid outlet system 50 The resulting extract was isolated.

The water and the extract separated by the first chromatographic separation system 30 are respectively input into the second chromatographic separation system 40 through the water inlet system 10 and the feed system 20, and the separated mannose is output from the first liquid outlet system 50.

When the chromatographic separation system 100 includes the second liquid outlet system 60, the raffinate obtained by the first chromatographic separation system 30 is subjected to enzymatic conversion treatment and then input to the first chromatographic separation system 30 through the feeding system 20 for separation. It is input to the feed system 20 through the second liquid outlet system 60 and then input to the first chromatographic separation system 30 for separation.

The raffinate feeding system 20 separated by the second chromatographic separation system 40 is input into the first chromatographic separation system 30 as a raw material for separation.

The chromatographic separation procedure is accomplished in three sub-steps. Taking the first chromatographic column 300 as an example, the separation process is as follows:

The first cycle step:

All circulation pumps in the first chromatographic separation system 30 are turned on, and the chromatograph circulates itself to complete the chromatographic separation process.

The second step is to take out the raffinate:

Turn on the valve 80 of the first chromatographic column 300 for controlling the water inlet, turn on the circulating pumps of the 5 chromatographic columns from the first chromatographic column A301 to the first chromatographic column E305, and turn on the first chromatographic column E305 for controlling the raffinate valve 80. In this way, the chromatography enters water from the first chromatographic column A301, and the raffinate is extracted from the first chromatographic column E305.

The third step is all in and all out:

Open the valve 80 of the first chromatographic column A301 for controlling the water inlet, open the circulating pump of the first chromatographic column A301, and open the valve 80 of the first chromatographic column A301 for controlling the extraction liquid to discharge the extraction liquid; open the first chromatographic column The valve 80 of D304 for controlling the feed is opened, the circulating pumps of the first chromatographic column D304 and the first chromatographic column E305 are opened, and the valve 80 of the first chromatographic column E305 for controlling the raffinate is opened to extract the raffinate.

After three steps in this way, a small cycle is completed.

Then, the system switches to the first chromatographic column B302 and repeats the above procedure in sequence until the first chromatographic column A301 to the first chromatographic column F306 are completed, that is, a large cycle of chromatography is completed. The chromatography then continues to repeat the above steps.

At the same time as the above-mentioned first set of chromatographic separation, the chromatographic extract is used as the raw material of the second set of chromatographic materials after evaporation and concentration, and the raffinate can be mixed with the raw materials and converted as the second set of chromatographic raw materials due to its high fructose content. times used.

The operation steps of the second set of chromatography are the same as those of the first set of chromatography. The above operating parameters can be adjusted according to the actual situation.

For reference, in a specific operation, the feed concentration can be set to 40-60 wt %, such as 40 wt %, 45 wt %, 50 wt %, 55 wt % or 60 wt % and the like. The water-material ratio can be set to 2-3 (mass ratio), such as 2, 2.5 or 3, etc. The inlet water flow can be set to 2-3VB/h, such as 2VB/h, 2.5VB/h or 3VB/h, etc. The feed flow can be set to 1-2VB/h, such as 1VB/h, 1.5VB/h or 2VB/h, etc. The extraction liquid discharge flow rate can be set to 1.2-1.8VB/h, such as 1.2VB/h, 1.5VB/h or 1.8VB/h, etc. The raffinate discharge flow rate can be set to 2.5-3.5VB/h, such as 2.5VB/h, 3VB/h or 3.5VB/h, etc.

Similarly, after three sub-steps, the extract from the chromatography is evaporated and concentrated, and then decrystallized to produce a mannose product with a purity of 98%, preferably more than 99%, and the raffinate can be returned to the first set of chromatography. The raw material tank is reused.

The purity of the mannose separated by the above method was 98%, and the yield was 60%.

To sum up, the chromatographic separation system and application and the separation method of mannose provided by this application at least have the following advantages:

1. In the whole conversion process of the material, pure water is used instead of tap water, so that the conductivity of the converted material is lower, and the separation process can be omitted;

2. Two sets of chromatographs share a set of water inlet system at the same time, and the chromatographic inlet pump adopts frequency conversion control, which can not only save electricity, but also solve the problem of large pressure fluctuation during the chromatographic water inlet;

3. Two sets of chromatography can be operated synchronously. Even when the purity of the feed fluctuates, we can fine-tune the operating parameters to ensure the stability of the purity of the chromatographic output to the greatest extent.

4. The biggest advantage of the set of chromatography is that the raffinate can be distributed reasonably, which reduces the cost to the greatest extent;

5. The process equipment has low investment, simple operation and high degree of automation, which fundamentally solves the disadvantages of traditional equipment such as large investment, complex process route and inconvenient operation.

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims (10)

1. a chromatographic separation system, is characterized in that, comprises water inlet system, feed system, the first chromatographic separation system, the second chromatographic separation system, the first liquid outlet system, and described water inlet system is separated from two chromatographic separations respectively The water inlet of the system is communicated, the feed system is communicated with the feed ports of the two chromatographic separation systems respectively, and the first liquid outlet system is communicated with the outlet ports of the two chromatographic separation systems respectively for outputting the extraction liquid; The part of the first liquid outlet system for outputting the extract obtained by the separation of the first chromatographic separation system communicates with the part of the feed system for inputting raw materials into the second chromatographic separation system, so that the The extract obtained by the separation of the first chromatographic separation system is input into the second chromatographic separation system as a raw material. 2. The chromatographic separation system according to claim 1, characterized in that, the chromatographic separation system further comprises a first evaporative concentration system, and the discharge port of the first evaporative concentration system is used in the feeding system for The part connected to the first chromatographic separation system is connected to be used for entering the first chromatographic separation system for the first chromatographic separation of the material to be separated after being evaporated and concentrated by the first evaporative concentration system. 3. The chromatographic separation system according to claim 2, wherein the chromatographic separation system further comprises a second evaporative concentration system, and the first liquid outlet system is used to output the obtained results obtained by the first chromatographic separation system. The part of the extracted liquid is communicated with the feed port of the second evaporative concentration system, and the discharge port of the second evaporative concentration system is connected to the feed port used for inputting raw materials to the second chromatographic separation system in the feed system. Partially connected. 4. The chromatographic separation system according to any one of claims 1-3, characterized in that, the chromatographic separation system further comprises a second liquid outlet system, and the second liquid outlet system is respectively associated with the two chromatographic separation systems. The liquid outlet for outputting the raffinate is connected. 5. The chromatographic separation system according to claim 4, characterized in that, the chromatographic separation system further comprises an enzymatic conversion system, and the second liquid outlet system is used to output the extract obtained by the separation of the first chromatographic separation system. The part of the residual liquid is communicated with the inlet of the enzyme conversion system, and the outlet of the enzyme conversion system is communicated with the part of the feed system for inputting the raw material to the first chromatographic separation system. 6. The chromatographic separation system according to claim 4, characterized in that, in the second liquid outlet system, the part used to output the raffinate obtained by the separation of the second chromatographic separation system is different from that in the feed system. The part for feeding the raw material to the first chromatographic separation system is communicated so that the raffinate obtained by the separation of the second chromatographic separation system is fed into the first chromatographic separation system as a raw material. 7 . The chromatographic separation system according to claim 4 , wherein the first chromatographic separation system comprises at least 6 first chromatographic columns, and the at least 6 first chromatographic columns pass through the first circulation pipeline in sequence. 8 . The first connection forms a loop system, the circulating pipeline between the two adjacent first chromatographic columns is provided with a circulating pump, and the water inlet system and the feeding system are respectively connected to each other through valves. The water inlet and the feed port of the first chromatographic column are correspondingly communicated, and the first liquid outlet system and the second liquid outlet system are respectively connected with the liquid outlet and the liquid outlet of the extraction liquid of each of the first chromatographic columns through valves. The liquid outlet of the raffinate is communicated correspondingly. 8 . The chromatographic separation system according to claim 7 , wherein the second chromatographic separation system comprises at least 6 second chromatographic columns, and the at least 6 second chromatographic columns end in sequence through the second circulation pipeline. 9 . The first connection forms a loop system, the circulating pipeline between the two adjacent second chromatographic columns is provided with a circulating pump, and the water inlet system and the feeding system are respectively connected with each other through valves. The water inlet and the feed port of the second chromatographic column are correspondingly communicated, and the first liquid outlet system and the second liquid outlet system are respectively connected with the liquid outlet and the liquid outlet of the extraction liquid of each of the second chromatographic columns through valves. The liquid outlet of the raffinate is communicated correspondingly. 9 . The application of the chromatographic separation system according to claim 1 , wherein the chromatographic separation system is used to separate the mannose in the mixture of mannose and fructose. 10 . 10. A separation method of mannose, characterized in that, comprising the steps of: adopting the chromatographic separation system as claimed in any one of claims 1-9 to separate raw materials to be separated and water containing mannose, respectively, through the described chromatographic separation system. The feed system and the water inlet system are input into the first chromatographic separation system, and the separated extract is output from the first liquid outlet system; The water and the extract obtained by the first chromatographic separation system are respectively input into the second chromatographic separation system through the water inlet system and the feed system, and the separated manna is output from the first liquid outlet system. sugar; Preferably, when the chromatographic separation system includes a second liquid outlet system, the raffinate obtained by the first chromatographic separation system is subjected to enzymatic conversion treatment and then input to the first chromatographic separation through the feed system separation in the system; Preferably, the raffinate obtained by the second chromatographic separation system is input into the feed system through the second liquid outlet system as a raw material input into the first chromatographic separation system for separation; Preferably, the water is pure water; Preferably, the purity of the separated mannose is 97-99%, more preferably 98%; Preferably, the yield of isolated mannose is 55-65%, more preferably 60%.

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