A chromatographic separation system and its application, a method for separating mannose

Through the interconnection and enzyme conversion treatment of two chromatographic separation systems, the efficient separation problem of mannose and fructose mixture is solved, and mannose production with high purity and high yield is achieved, which simplifies the operation process and reduces costs.

CN111389051BActive Publication Date: 2025-07-25SHANDONG ZHAOGUANG CHROMATOGRAPHY SEPARATION TECH CO LTD
View PDF 5 Cites 0 Cited by

Patent Information

Application Number
CN202010312220.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-04-20
Publication Date
2025-07-25
Estimated Expiration
2040-04-20

AI Technical Summary

Technical Problem

The prior art is difficult to efficiently separate the mixed solution of mannose and fructose, resulting in low separation, low purity and yield, and poor economic benefits.

Method used

The comprehensive utilization of two chromatographic separation systems is adopted, and the efficient separation of mannose and fructose is achieved through the connection of the water inlet, feed and discharge systems. The raffinate is converted to improve purity and yield.

Benefits of technology

Obtaining mannose products with high purity (97-99%) and high yield (55-65%) reduces equipment investment and operation complexity and improves economic benefits.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN111389051B_ABST
    Figure CN111389051B_ABST
Patent Text Reader

Abstract

The present invention discloses a chromatographic separation system and its application, and a method for separating mannose, belonging to the technical field of substance separation. The chromatographic separation system includes a water inlet system, a feed system, two chromatographic separation systems, and a first liquid outlet system. The water inlet system is respectively connected to the water inlets of the two chromatographic separation systems, the feed system is respectively connected to the feed inlets of the two chromatographic separation systems, and the first liquid outlet system is respectively connected to the liquid outlets of the two chromatographic separation systems for outputting the extract. Through the comprehensive utilization of two sets of chromatographic separation systems, when used for separating mannose, mannose products with high purity and high yield can be obtained, improving economic benefits. The raw material to be separated containing mannose and water are input into the first chromatographic separation system by using the above chromatographic separation system to obtain an extract; the water and the extract separated by the first chromatographic separation system are input into the second chromatographic separation system to obtain mannose. This method is simple and easy to operate.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of substance separation, and in particular, to a chromatographic separation system and its application, and a method for separating mannose. Background Art

[0002] Mannose is an important hexose sugar with high viscosity and has wide application fields in industries such as medicine and food. The mixed solution of mannose is composed of 25% mannose, about 74% fructose, and a small amount of miscellaneous sugars. Mannose and fructose are isomers, and in the liquid chromatogram analysis, the chromatographic peaks of the two are very close, and the resolution is <0.3, with a low resolution. Therefore, in the normal production process, it is very difficult to separate these two substances well. For example, using separation means such as crystallization, nanofiltration membranes, and conventional chromatography, it is difficult to operate; second, it is difficult to achieve a high purity after separation.

[0003] Therefore, at present, large-scale production still mainly uses the extraction method, but this method has low efficiency, and both the purity and yield of the extract are low, and it is difficult to obtain high economic benefits.

[0004] In view of this, the present invention is specifically proposed. Summary of the Invention

[0005] One of the objectives of the present invention includes providing a chromatographic separation system. By comprehensively using two sets of chromatographic separation systems, this chromatographic separation system fundamentally solves the problem that it is very difficult to separate two similar substances in a mixture.

[0006] Another objective of the present invention includes providing an application of the above chromatographic separation system. When it is used to separate mannose, especially to separate the mannose in the mixed solution of mannose and fructose, a mannose product with high purity and high yield can be obtained, improving economic benefits.

[0007] The third objective of the present invention includes providing a method for separating mannose. This method is simple, easy to operate, has low cost, and both the purity and yield of mannose are relatively high after separation.

[0008] The present invention is implemented as follows:

[0009] In a 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 to the water inlet ports of the two chromatographic separation systems, the feed system is respectively connected to the feed ports of the two chromatographic separation systems, and the first liquid outlet system is respectively connected to the liquid outlet ports of the two chromatographic separation systems for outputting the extract.

[0010] The part of the first liquid output system for outputting the extract obtained by separating the first chromatographic separation system is communicated with the part of the feed system for inputting raw materials into the second chromatographic separation system, so that the extract obtained by separating the first chromatographic separation system is input into the second chromatographic separation system as raw materials.

[0011] In an alternative embodiment, the chromatographic separation system further includes a first evaporation and concentration system. The discharge port of the first evaporation and concentration system is connected to the part of the feed system for connecting with the first chromatographic separation system, so as to feed the material to be separated after evaporation and concentration by the first evaporation and concentration system into the first chromatographic separation system for the first chromatographic separation.

[0012] In an alternative embodiment, the chromatographic separation system further includes a second evaporation and concentration system. The part of the first liquid output system for outputting the extract obtained by separating the first chromatographic separation system is communicated with the feed port of the second evaporation and concentration system, and the discharge port of the second evaporation and concentration system is communicated with the part of the feed system for inputting raw materials into the second chromatographic separation system.

[0013] In an alternative embodiment, the chromatographic separation system further includes a second liquid output system. The second liquid output system is respectively communicated with the liquid output ports of the two chromatographic separation systems for outputting raffinate.

[0014] In an alternative embodiment, the chromatographic separation system further includes an enzyme conversion system. The part of the second liquid output system for outputting the raffinate obtained by separating the first chromatographic separation system is communicated with the feed port of the enzyme conversion system, and the discharge port of the enzyme conversion system is communicated with the part of the feed system for inputting raw materials into the first chromatographic separation system.

[0015] In an alternative embodiment, the part of the second liquid output system for outputting the raffinate obtained by separating the second chromatographic separation system is communicated with the part of the feed system for inputting raw materials into the first chromatographic separation system, so that the raffinate obtained by separating the second chromatographic separation system is input into the first chromatographic separation system as raw materials.

[0016] In an alternative embodiment, the first chromatographic separation system includes at least 6 first chromatographic columns. At least 6 first chromatographic columns are sequentially connected end to end through a first circulation pipeline to form a loop system. A circulation pump is provided in the circulation pipeline between adjacent two first chromatographic columns. The water inlet system and the feed system are respectively communicated with the water inlet and feed ports of each first chromatographic column through valves. The first liquid output system and the second liquid output system are respectively communicated with the extract liquid output port and the raffinate liquid output port of each first chromatographic column through valves.

[0017] In an alternative embodiment, the second chromatographic separation system includes at least 6 second chromatographic columns. The at least 6 second chromatographic columns are connected end to end in sequence through a second circulation pipeline to form a loop system. A circulation pump is provided in the circulation pipeline between adjacent two second chromatographic columns. The water inlet system and the feed system are respectively connected to the water inlet and the feed inlet of each second chromatographic column through valves in a corresponding manner. The first liquid outlet system and the second liquid outlet system are respectively connected to the liquid outlet of the extract and the liquid outlet of the raffinate of each second chromatographic column through valves in a corresponding manner.

[0018] In a second aspect, the present application provides an application of the chromatographic separation system according to any one of the foregoing embodiments, and the chromatographic separation system is used to separate mannose from a mixed solution of mannose and fructose.

[0019] In a third aspect, the present application provides a method for separating mannose, including the following steps: using the chromatographic separation system according to any one of the foregoing embodiments, inputting the raw material to be separated containing mannose and water into the first chromatographic separation system through the feed system and the water inlet system respectively, and outputting the separated extract through the first liquid outlet system;

[0020] Inputting water and the extract separated by the first chromatographic separation system into the second chromatographic separation system through the water inlet system and the feed system respectively, and outputting the separated mannose through the first liquid outlet system;

[0021] Preferably, when the chromatographic separation system includes a second liquid outlet system, the raffinate separated by the first chromatographic separation system is subjected to enzyme conversion treatment and then input into the first chromatographic separation system through the feed system for separation;

[0022] Preferably, the raffinate separated by the second chromatographic separation system is input into the feed system through the second liquid outlet system and used as a raw material to be input into the first chromatographic separation system for separation.

[0023] Preferably, the water is pure water.

[0024] Preferably, the purity of the separated mannose is 97-99%, more preferably 98%.

[0025] Preferably, the yield of the separated mannose is 55-65%, more preferably 60%.

[0026] The present invention has the following beneficial effects:

[0027] By comprehensively utilizing two sets of chromatographic separation systems, the raw material to be separated containing mannose and water are input into the first chromatographic separation system to obtain an extract; the extract obtained by separating the first chromatographic separation system is input into the second chromatographic separation system to separate mannose, and a mannose product with high purity and high yield can be obtained, improving economic benefits. The process equipment has less investment, is simple to operate, and has a high degree of automation, fundamentally solving the disadvantages of large traditional equipment investment, complex process routes, and inconvenient operation. The corresponding separation method is simple and easy to operate. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention, and therefore should not be regarded as limiting the scope. For those of ordinary skill in the art, without creative efforts, other related drawings can also be obtained based on these drawings.

[0029] Figure 1 It is a schematic structural diagram of the chromatographic separation system provided for Embodiment 1.

[0030] Description of the 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 - second liquid 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 - main water inlet pipe; 12 - water inlet branch pipe; 21 - first main feeding pipe; 22 - first feeding branch pipe; 23 - second main feeding pipe; 24 - second feeding branch pipe; 51 - first main liquid outlet pipe A; 52 - first liquid outlet branch pipe A; 53 - first main liquid outlet pipe B; 54 - first liquid outlet branch pipe B; 61 - second main liquid outlet pipe A; 62 - second liquid outlet branch pipe A; 63 - second main liquid outlet pipe B; 64 - second liquid outlet branch pipe B; 80 - valve. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0031] 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 clearly and completely described below. For those conditions not specified in the embodiments, they are carried out according to conventional conditions or conditions recommended by the manufacturer. For reagents or instruments not specified by the manufacturer, they are all conventional products that can be obtained through commercial purchase.

[0032] The features and performance of the present invention will be further described in detail below in conjunction with the embodiments.

[0033] Embodiment 1

[0034] This embodiment provides a chromatographic separation system 100. Please refer to Figure 1 , which includes a water inlet system 10, a feed system 20, a first chromatographic separation system 30, a second chromatographic separation system 40, and a first liquid outlet system 50. The water inlet system 10 is respectively communicated with the water inlets of the two chromatographic separation systems, the feed system 20 is respectively communicated with the feed inlets of the two chromatographic separation systems, and the first liquid outlet system 50 is respectively communicated with the liquid outlets for outputting the extract of the two chromatographic separation systems.

[0035] In an alternative embodiment, the first chromatographic separation system 30 includes at least 6 first chromatographic columns 300. At least 6 first chromatographic columns 300 are sequentially connected end to end through a first circulation pipeline 71 to form a loop system. A circulation pump is provided in the circulation pipeline between adjacent two first chromatographic columns 300. The water inlet system 10 and the feed system 20 are respectively communicated with the water inlet and the feed inlet of each first chromatographic column 300 through valves 80. The first liquid outlet system 50 and the second liquid outlet system 60 are respectively communicated with the liquid outlet for the extract and the raffinate outlet of each first chromatographic column 300 through valves 80.

[0036] For reference, the first chromatographic separation system 30 has 6 first chromatographic columns 300, which are respectively represented by the first chromatographic column A301, the first chromatographic column B302, the first chromatographic column C303, the first chromatographic column D304, the first chromatographic column E305, and the first chromatographic column F306. The above 6 first chromatographic columns 300 altogether correspond to four functional zones, including 1 Z1 zone, 2 Z2 zones, 2 Z3 zones, and 1 Z4 zone. Among them, the Z1 zone is the desorption zone, the Z2 zone is the separation zone, the Z3 zone is the adsorption zone, and the Z4 zone 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. During the actual operation process, the inlet and outlet materials of the system are all realized through the continuous switching of the above four functional zones.

[0037] In an alternative embodiment, the second chromatographic separation system 40 includes at least six second chromatographic columns 400. The at least six second chromatographic columns 400 are connected end to end in sequence through a second circulation pipeline 72 to form a loop system. A circulation pump is provided in the circulation pipeline between every two adjacent second chromatographic columns 400. The water inlet system 10 and the feed system 20 are respectively and correspondingly connected to the water inlet and the feed inlet of each second chromatographic column 400 through valves 80. The first liquid outlet system 50 and the second liquid outlet system 60 are respectively and correspondingly connected to the liquid outlet of the extract and the liquid outlet of the raffinate of each second chromatographic column 400 through valves 80.

[0038] For reference, the second chromatographic separation system 40 has six second chromatographic columns 400, which are respectively denoted as second chromatographic column A401, second chromatographic column B402, second chromatographic column C403, second chromatographic column D404, second chromatographic column E405, and second chromatographic column F406. Similarly, the above 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. Among them, the Z1 zone is the desorption zone, the Z2 zone is 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 end to end in sequence through the second circulation pipeline 72 to form a loop system. During the actual operation process, the materials entering and leaving the system are all realized through the continuous switching of the above four functional zones.

[0039] The water inlet system 10 includes a water inlet main pipe 11 and multiple water inlet branch pipes 12. The multiple water inlet branch pipes 12 are arranged in parallel. The water inlet of each water inlet branch pipe 12 is connected to the water outlet of the water inlet main pipe 11, and the water outlets of the multiple water inlet branch pipes 12 are respectively connected to 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 then the water inlet main pipe 11 inputs water into each chromatographic column through the multiple 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 should be noted that in this embodiment, the two chromatographic separation systems share one water inlet system 10, and a chromatographic water inlet pump with frequency conversion control can also be provided on the pipeline of the water inlet system 10, which can not only save electricity but also solve the problem of large pressure fluctuations during chromatographic water inlet.

[0040] The feed system 20 includes a first feed main pipe 21, multiple first feed branch pipes 22, a second feed main pipe 23, and multiple second feed branch pipes 24.

[0041] Multiple first feed branch pipes 22 are arranged in parallel. The feed ports of each first feed branch pipe 22 are communicated with the discharge port of the first feed main pipe 21, and the discharge ports of the multiple first feed branch pipes 22 are respectively communicated with the feed ports of the first chromatographic columns A301 to the first chromatographic columns F306. A valve 80 is provided between each first feed branch pipe 22 and the feed port of the first chromatographic column 300.

[0042] Multiple second feed branch pipes 24 are arranged in parallel. The feed ports of each second feed branch pipe 24 are communicated with the discharge port of the second feed main pipe 23, and the discharge ports of the multiple second feed branch pipes 24 are respectively communicated with the feed ports of the second chromatographic columns A401 to the second chromatographic columns 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 discharge system 50 includes a first liquid discharge main pipe A51, multiple first liquid discharge branch pipes A52, a first liquid discharge main pipe B53, and multiple first liquid discharge branch pipes B54.

[0043] Multiple first liquid discharge branch pipes A52 are arranged in parallel. The liquid inlet ports of the multiple first liquid discharge branch pipes A52 are respectively and correspondingly communicated with the liquid discharge ports of the multiple first chromatographic columns 300 for outputting the extract, and the liquid discharge port of each first liquid discharge branch pipe A52 is communicated with the liquid inlet port of the first liquid discharge main pipe A51. A valve 80 is provided between each first liquid discharge branch pipe A52 and the liquid discharge port of the first chromatographic column 300 for outputting the extract.

[0044] Multiple first liquid discharge branch pipes B54 are arranged in parallel. The liquid inlet ports of the multiple first liquid discharge branch pipes B54 are respectively and correspondingly communicated with the liquid discharge ports of the multiple second chromatographic columns 400 for outputting the extract, and the liquid discharge port of each first liquid discharge branch pipe B54 is communicated with the liquid inlet port of the first liquid discharge main pipe B53. A valve 80 is provided between each first liquid discharge branch pipe B54 and the liquid discharge port of the second chromatographic column 400 for outputting the extract.

[0045] In an alternative embodiment, the part of the first liquid discharge system 50 for outputting the extract separated by the first chromatographic separation system 30 is communicated with the part of the feed system 20 for inputting the raw material into the second chromatographic separation system 40, so that the extract separated by the first chromatographic separation system 30 is input into the second chromatographic separation system 40 as the raw material.

[0046] Specifically, the liquid discharge port of the first liquid discharge main pipe A51 is communicated with the feed port of the second feed main pipe 23, that is, the extract separated by the first chromatographic separation system 30 is used as the raw material of the second chromatographic separation system 40 for further separation.

[0047] The liquid flowing out of the first liquid discharge main pipe B53 is the highly pure mannose separated (the purity can reach more than 98%).

[0048] During operation, the raw material to be separated is first input into the first feed main pipe 21. The first feed main pipe 21 then respectively inputs the raw material into a plurality of first chromatographic columns 300 through a plurality of first feed branch pipes 22. The extract separated by the first chromatographic separation system 30 is collected in the first discharge main pipe A51 through a plurality of first discharge branch pipes A52, and then is respectively input into a plurality of second chromatographic columns 400 through the second feed main pipe 23 and a plurality of second feed branch pipes 24. The extract separated by the second chromatographic separation system 40 is then collected in the first discharge main pipe B53 through a plurality of first discharge branch pipes B54, obtaining the separated mannose.

[0049] In an alternative embodiment, the chromatographic separation system 100 of the present embodiment may further include a first evaporation and concentration system (not shown in the figure). The discharge port of the first evaporation and concentration system is connected to the part of the feed system 20 for connecting to the first chromatographic separation system 30 (i.e., the first feed main pipe 21) to allow the material to be separated that has been evaporated and concentrated by the first evaporation and concentration system to enter the first chromatographic separation system 30 for the first chromatographic separation.

[0050] In an alternative embodiment, the chromatographic separation system 100 of the present embodiment may further include a second evaporation and concentration system (not shown in the figure). The part of the first discharge system 50 for outputting the extract separated by the first chromatographic separation system 30 is in communication with the feed port of the second evaporation and concentration system, and the discharge port of the second evaporation and concentration system is in communication with the part of the feed system 20 for inputting the raw material to the second chromatographic separation system 40. That is, the discharge port of the first discharge main pipe A51 is in communication with the feed port of the second evaporation and concentration system, and the discharge port of the second evaporation and concentration system is in communication with the feed port of the second feed main pipe 23.

[0051] The extract obtained by the first chromatographic separation system 30 enters the second chromatographic separation system 40 for further purification after passing through the second evaporation and concentration, and a mannose product with a purity of more than 98% can be obtained.

[0052] In an alternative embodiment, the chromatographic separation system 100 further includes a second discharge system 60. The second discharge system 60 is respectively in communication with the discharge ports of the two chromatographic separation systems for outputting the raffinate.

[0053] The second discharge system 60 includes a second discharge main pipe A61, a plurality of second discharge branch pipes A62, a second discharge main pipe B63, and a plurality of second discharge branch pipes B64.

[0054] Multiple second liquid outlet branch pipes A62 are arranged in parallel. The liquid inlet ports of the multiple second liquid outlet branch pipes A62 are respectively and correspondingly communicated with the liquid outlet ports of multiple first chromatographic columns 300 for outputting raffinate. The liquid outlet port of each second liquid outlet branch pipe A62 is communicated with the liquid inlet port 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 port of the first chromatographic column 300 for outputting raffinate.

[0055] Multiple second liquid outlet branch pipes B64 are arranged in parallel. The liquid inlet ports of the multiple second liquid outlet branch pipes B64 are respectively and correspondingly communicated with the liquid outlet ports of multiple second chromatographic columns 400 for outputting raffinate. The liquid outlet port of each second liquid outlet branch pipe B64 is communicated with the liquid inlet port 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 port of the second chromatographic column 400 for outputting extract.

[0056] In an optional embodiment, the chromatographic separation system 100 further includes an enzyme conversion system (not shown in the figure). The part of the second liquid outlet system 60 for outputting the raffinate separated by the first chromatographic separation system 30 is communicated with the feed inlet of the enzyme conversion system. The discharge outlet of the enzyme conversion system is communicated with the part of the feed system 20 for inputting raw materials into the first chromatographic separation system 30.

[0057] That is, the liquid outlet port of the first liquid outlet main pipe A51 is communicated with the feed inlet of the enzyme conversion system, and the discharge outlet of the enzyme conversion system is communicated with the feed inlet of the first feed main pipe 21. That is, the raffinate separated by the first chromatographic separation system 30 can be used as the raw material of the first chromatographic separation system 30 after enzyme conversion.

[0058] The above operation is because the content of fructose in the raffinate separated by the first chromatographic separation system 30 is relatively high. By converting it into mannose with an enzyme and using it as the raw material of the second chromatographic separation system 40, that is, the by-product raffinate is reused after conversion, thus greatly reducing the cost.

[0059] Further, in an optional embodiment, the part of the second liquid outlet system 60 for outputting the raffinate separated by the second chromatographic separation system 40 is communicated with the part of the feed system 20 for inputting raw materials into the first chromatographic separation system 30 so that the raffinate separated by the second chromatographic separation system 40 is input into the first chromatographic separation system 30 as a raw material.

[0060] That is, the liquid outlet port of the second liquid outlet main pipe B63 can be communicated with the feed inlet of the first feed main pipe 21. That is, the raffinate separated by the second chromatographic separation system 40 is used as the raw material of the first chromatographic separation system 30 and continues to be used.

[0061] It should be noted that before the raffinate obtained by the second chromatographic separation system 40 is input into the first chromatographic separation system 30 as a raw material, it can also be converted by an enzyme conversion system and then reused as the raw material of the first chromatographic separation system 30.

[0062] For reference, the valves 80 involved in this embodiment can all be automatic control ball valves.

[0063] Embodiment 2

[0064] This embodiment provides an application of the chromatographic separation system 100 as in Embodiment 1, which is used to separate mannose from a mixed solution of mannose and fructose. This mixed solution mainly consists of about 25% mannose, about 74% fructose, and a small amount of miscellaneous sugars.

[0065] The specific separation steps include: using the above chromatographic separation system 100, inputting the mixed solution containing mannose and pure water into the first chromatographic separation system 30 through the feeding system 20 and the water inlet system 10 respectively, and outputting the separated extract through the first liquid outlet system 50.

[0066] Input water and the extract separated by the first chromatographic separation system 30 into the second chromatographic separation system 40 through the water inlet system 10 and the feeding system 20 respectively, and output the separated mannose through the first liquid outlet system 50.

[0067] When the chromatographic separation system 100 includes the second liquid outlet system 60, the raffinate separated by the first chromatographic separation system 30 is input into the first chromatographic separation system 30 for separation after enzyme conversion treatment through the feeding system 20, or can also be input into the feeding system 20 through the second liquid outlet system 60 and then input into the first chromatographic separation system 30 for separation.

[0068] Input the raffinate separated by the second chromatographic separation system 40 into the first chromatographic separation system 30 as a raw material through the feeding system 20 for separation.

[0069] The separation procedure of chromatography is realized through three sub-steps. Taking the first chromatographic column 300 as an example, its separation process is as follows:

[0070] The first cycle step:

[0071] Turn on all the circulation pumps in the first chromatographic separation system 30, and the chromatography circulates itself to complete the chromatographic separation process.

[0072] The second step is to introduce water and output the raffinate:

[0073] Open the valve 80 for controlling the inlet water of the first chromatographic column 300, turn on the circulation pumps of the five chromatographic columns from the first chromatographic column A301 to the first chromatographic column E305, and open the valve 80 for controlling the raffinate of the first chromatographic column E305. In this way, the chromatographic process takes in water from the first chromatographic column A301 and discharges the raffinate from the first chromatographic column E305.

[0074] The third step: all-in all-out:

[0075] Open the valve 80 for controlling the inlet water of the first chromatographic column A301, turn on the circulation pump of the first chromatographic column A301, and open the valve 80 for controlling the extract of the first chromatographic column A301 to discharge the extract; open the valve 80 for controlling the feed of the first chromatographic column D304, turn on the circulation pumps of the first chromatographic column D304 and the first chromatographic column E305, and open the valve 80 for controlling the raffinate of the first chromatographic column E305 to discharge the raffinate.

[0076] After these three steps, a small cycle is completed.

[0077] 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, and then a large cycle of chromatography is completed. Then the chromatography continues to repeat the above steps.

[0078] While the first set of chromatography is in progress, the extract separated by the chromatography is used as the raw material for the second set of chromatography after evaporation and concentration. And since the raffinate has a high fructose content, it can be mixed with the raw materials and used as the chromatographic raw material for the second time after conversion.

[0079] The operating steps of the second set of chromatography are the same as those of the first set of chromatography, with only slight adjustments in the operating parameters (such as the chromatographic feed concentration, water-to-material ratio, throughput, feed flow rate, inlet water flow rate, extract discharge flow rate, and raffinate discharge flow rate). The above operating parameters can be adjusted according to the actual situation.

[0080] For reference, during specific operations, the feed concentration can be set to 40 - 60 wt%, such as 40 wt%, 45 wt%, 50 wt%, 55 wt% or 60 wt%, etc. The water-to-material ratio can be set to 2 - 3 (mass ratio), such as 2, 2.5 or 3, etc. The inlet water flow rate can be set to 2 - 3 VB / h, such as 2 VB / h, 2.5 VB / h or 3 VB / h, etc. The feed flow rate can be set to 1 - 2 VB / h, such as 1 VB / h, 1.5 VB / h or 2 VB / h, etc. The extract discharge flow rate can be set to 1.2 - 1.8 VB / h, such as 1.2 VB / h, 1.5 VB / h or 1.8 VB / h, etc. The raffinate discharge flow rate can be set to 2.5 - 3.5 VB / h, such as 2.5 VB / h, 3 VB / h or 3.5 VB / h, etc.

[0081] Similarly, after three sub-steps, the extract obtained from chromatography is evaporated and concentrated, and then crystallized to produce a mannose product with a purity of 98%, preferably more than 99%. The raffinate can be returned to the raw material tank of the first set of chromatography for secondary utilization.

[0082] The purity of the mannose separated by the above method is 98%, and the yield is 60%.

[0083] In summary, the chromatographic separation system, its application, and the method for separating mannose provided in this application have at least the following advantages:

[0084] 1. During the conversion process of the whole material, pure water is used instead of tap water, resulting in a lower conductivity of the converted material, and the ion exchange process can be omitted.

[0085] 2. Two sets of chromatography share the same water inlet system, and the chromatographic inlet water pump is controlled by frequency conversion, which can not only save electricity but also solve the problem of large pressure fluctuations during chromatographic water inlet.

[0086] 3. The two sets of chromatography can be operated synchronously. Even when the feed purity fluctuates, we can fine-tune the operating parameters to ensure the stability of the chromatographic outlet purity to the greatest extent.

[0087] 4. The greatest advantage of this set of chromatography is that it can reasonably distribute the raffinate, minimizing the cost to the greatest extent.

[0088] 5. This process has low equipment investment, is easy to operate, and has a high degree of automation, fundamentally solving the disadvantages of large traditional equipment investment, complex process routes, and inconvenient operation.

[0089] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention can have various modifications and changes. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for separating mannose, characterized in that, Comprising the following steps: Adopting a chromatographic separation system; The chromatographic separation system includes a feed water system, a feed system, a first chromatographic separation system, a second chromatographic separation system, and a first liquid outlet system. The feed water system is respectively connected to the water inlets of the two chromatographic separation systems. The feed system is respectively connected to the feed inlets of the two chromatographic separation systems. The first liquid outlet system is respectively connected to the liquid outlets for outputting the extract of the two chromatographic separation systems; A part of the first liquid outlet system for outputting the extract separated by the first chromatographic separation system is connected to a part of the feed system for inputting raw materials into the second chromatographic separation system, so that the extract separated by the first chromatographic separation system is input into the second chromatographic separation system as raw materials; The chromatographic separation system further includes a first evaporation and concentration system. The discharge port of the first evaporation and concentration system is connected to a part of the feed system for connecting with the first chromatographic separation system, so as to enable the material to be separated after evaporation and concentration by the first evaporation and concentration system to enter the first chromatographic separation system for the first chromatographic separation; A part of the first liquid outlet system for outputting the extract separated by the first chromatographic separation system is connected to the feed inlet of the second evaporation and concentration system, and the discharge port of the second evaporation and concentration system is connected to a part of the feed system for inputting raw materials into the second chromatographic separation system; The chromatographic separation system further includes a second liquid outlet system. The second liquid outlet system is respectively connected to the liquid outlets for outputting the raffinate of the two chromatographic separation systems; The chromatographic separation system further includes an enzyme conversion system. A part of the second liquid outlet system for outputting the raffinate separated by the first chromatographic separation system is connected to the feed inlet of the enzyme conversion system, and the discharge port of the enzyme conversion system is connected to a part of the feed system for inputting raw materials into the first chromatographic separation system; A part of the second liquid outlet system for outputting the raffinate separated by the second chromatographic separation system is connected to a part of the feed system for inputting raw materials into the first chromatographic separation system, so that the raffinate separated by the second chromatographic separation system is input into the first chromatographic separation system as raw materials; The first chromatographic separation system includes at least 6 first chromatographic columns. The at least 6 first chromatographic columns are sequentially connected end to end through a first circulation pipeline to form a loop system. A circulation pump is provided in the circulation pipeline between adjacent two first chromatographic columns. The feed water system and the feed system are respectively connected to the water inlet and the feed inlet of each first chromatographic column through valves. The first liquid outlet system and the second liquid outlet system are respectively connected to the liquid outlet for the extract and the liquid outlet for the raffinate of each first chromatographic column through valves; The second chromatographic separation system includes at least six second chromatographic columns. The at least six second chromatographic columns are connected end to end in sequence through a second circulation pipeline to form a loop system. A circulation pump is provided in the circulation pipeline between every two adjacent second chromatographic columns. The water inlet system and the feed system are respectively and correspondingly connected to the water inlet and the feed inlet of each second chromatographic column through valves. The first liquid outlet system and the second liquid outlet system are respectively and correspondingly connected to the liquid outlet of the extract and the liquid outlet of the raffinate of each second chromatographic column through valves; The separation process includes: inputting the raw material to be separated containing mannose and water into the first chromatographic separation system through the feed system and the water inlet system respectively, and outputting the separated extract through the first liquid outlet system; the raw material to be separated mainly consists of 25% mannose, 74% fructose and a small amount of miscellaneous sugars; Inputting water and the extract separated by the first chromatographic separation system into the second chromatographic separation system through the water inlet system and the feed system respectively, and outputting the separated mannose through the first liquid outlet system; Inputting the raffinate separated by the first chromatographic separation system into the first chromatographic separation system for separation after enzyme conversion treatment through the feed system; Inputting the raffinate separated by the second chromatographic separation system into the feed system through the second liquid outlet system as a raw material into the first chromatographic separation system for separation; The purity of the separated mannose is 97-99%, and the yield of the separated mannose is 55-65%.

2. The separation method according to claim 1, characterized in that, The water is pure water.

3. The separation method according to claim 1, characterized in that The purity of the separated mannose is 98%.

4. The separation method according to claim 1, characterized in that, The yield of the separated mannose is 60%.

Citation Information

Patent Citations

  • Method for preparing D-mannose

    CN102329340A

  • Chromatographic separation system and separation method thereof

    CN110025983A

  • Chromatographic separation system

    CN212091012U

  • Method for separating and obtaining mannose

    JP1994237782A

  • Process for separating a mixture with measurement of purity or yield on an intermediate tank

    WO2019097181A1