CN107158747B

CN107158747B - Device for decoloring, deionizing and separating mixture and operation method

Info

Publication number: CN107158747B
Application number: CN201710356613.2A
Authority: CN
Inventors: 周日尤; 李瑛�; 伍玉碧; 吴鹏; 曹媛; 杜小霞
Original assignee: Nanjing Kaitong Grain Biochemistry R And D Co ltd
Current assignee: Nanjing Kaitong Grain Biochemistry R And D Co ltd
Priority date: 2017-05-19
Filing date: 2017-05-19
Publication date: 2022-09-16
Anticipated expiration: 2037-05-19
Also published as: CN107158747A

Abstract

The invention discloses a device for decoloring, deionizing and separating a mixture and an operation method, belongs to the technical field of decoloring, deionizing, separating and refining, and aims to provide a method for simultaneously completing decoloring, deionizing and separating the mixture in one device. The technical scheme is as follows: the apparatus consists of two sets of chromatography systems, group 1 being primarily aimed at decolorizing and deionizing and group 2 being aimed at mixture separation. The device is operated periodically, four periods form a cycle, after the period I is finished, the period II is operated, then the period III and the period IV are operated, after the period IV is finished, the period I is returned, and the cycle is carried out; each cycle consists of seven steps. The invention integrates the traditional decolorization and ion exchange process into one device, does not need activated carbon to decolorize, saves a large amount of acid and alkali used in the traditional ion exchange, reduces the production cost, and is beneficial to energy conservation, emission reduction and environmental protection.

Description

Device for decoloring, deionizing and separating mixture and operation method

Technical Field

The invention relates to the technical field of decoloration, deionization, separation and refining, in particular to a decoloration, deionization and mixture separation device and an operation method

Background

The reaction liquid is decolorized and the ions are removed, which is very important for the production of sugar, sugar alcohol and fine chemical products.

The traditional decoloring method is to adsorb pigment by powdered activated carbon, and then filter and remove the carbon and the pigment; or the feed liquid flows through the granular activated carbon to adsorb the pigment on the granular activated carbon, and then the pigment is eluted. Both of the two decolorization methods use activated carbon, and besides the consumption of the activated carbon, the black liquor and black powder of the activated carbon bring unfriendliness to the production environment.

A conventional method of removing impurity ions is an ion exchange method. When the ion exchange method is adopted to remove the impurity ions, the feed liquid flows through the ion exchange resin, and the impurity ions are adsorbed. The adsorption saturated ion exchange resin must be treated with acid and base, consuming large amounts of acid and base.

The simulated moving bed chromatographic separation device is used for separating the mixture, and is a clean, high-efficiency and low-energy-consumption separation means. However, in the case of separating a mixture by simulated moving bed chromatography, the requirements for the raw material to be fed are severe in order to obtain a good separation effect and protect the adsorbent resin. In contrast, the raw material needs to be decolorized and deionized before the chromatographic separation.

Disclosure of Invention

One of the purposes of the invention is to provide a device for decoloring, deionizing and separating mixture, which integrates the decoloring, deionizing and separating mixture into a set of device, can remove a large amount of cations and anions in the feed liquid while decoloring the feed liquid, and can separate the mixture in the feed liquid to obtain the feed liquid rich in extracting solution and the feed liquid rich in raffinate.

The above object of the present invention is achieved by the following technical solutions:

a device for decolorizing, deionizing and separating mixtures, consisting of a chromatographic system of group 1 and a chromatographic system of group 2:

(1) the 1 st group of chromatographic systems consists of m chromatographic columns, and the outlets and inlets of the chromatographic columns are connected through booster pumps, isolating valves, connecting pipes and flow meters; an eluent valve VWW and a material valve VFF are connected to the inlet of the chromatographic column; the eluent valve VWW and the material valve VFF are respectively connected with the eluent main pipe and the material main pipe; an outlet of the chromatographic column is connected with an impurity valve VS and a feeding valve VFS; the feeding valve VFS is connected to a feeding pipe and then connected with the feeding valves VF 1-VFn of the 2 nd group of chromatographic systems; the impurity valve VS is connected with an impurity pipe; the impurity tube is provided with a conductivity meter for detecting the conductivity of the effluent liquid; the impurity pipe is also provided with a flowmeter and a flow regulating valve for detecting and regulating the flow; the impurity pipe is divided into two branches after passing through the flow regulating valve: the impurity branch is connected with the S liquid tank through an impurity main valve VS 1; and the dilute liquid branch is connected with the X liquid tank after passing through a dilute liquid main valve VX.

(2) The 2 nd group of chromatographic systems are formed by connecting n chromatographic columns in series, and a booster pump, an isolating valve and a connecting pipe are arranged among the chromatographic columns; an eluent valve VW 1-VWn and a material valve VF 1-VFn are connected to the inlet of each chromatographic column of the 2 nd group of chromatographic systems; the eluent valve and the material valve are respectively connected with the eluent main pipe and the feeding pipe; the outlet of each chromatographic column of the 2 nd group of chromatographic systems is connected with raffinate valves VM 1-VMn and extract valves VN 1-VNn; the raffinate valves VM 1-VMn are connected with a raffinate pipe; the extraction liquid valve VN 1-VNn is connected with an extraction liquid pipe; a second conductivity meter is arranged on the raffinate pipe and used for detecting the conductivity of the effluent; the residual liquid extracting pipe is also provided with a second flowmeter and a second flow regulating valve which are used for detecting and regulating the flow; the raffinate pipe is divided into two branches after passing through a flow regulating valve II: the impurity branch II is connected with the S liquid tank after passing through an impurity main valve II VS 2; a raffinate branch is connected with a liquid C tank after passing through a liquid C main valve VC; and a third flow meter and a third flow regulating valve are arranged on the extracting solution pipe and are used for detecting and regulating the flow, and then the extracting solution pipe is connected with the B liquid tank after passing through the extracting solution branch.

(3) The group 1 chromatographic system operation process at least comprises three steps: feeding, eluting and internally circulating; the group 2 chromatographic system operation process at least comprises three steps: feeding, eluting and internally circulating.

(4) Separating pigment and impurity ions from the chromatographic system of group 1 and simultaneously feeding the chromatographic system of group 2; the 2 nd group chromatographic system separates the mixture and also separates part of the pigment and impurity ions.

Furthermore, in the 1 st group of chromatographic systems, m is 1-2; in the 2 nd group of chromatographic systems, n is 4-6.

Further, the eluent is pure water, a methanol water solution, an ethanol water solution, an organic acid solution or an inorganic acid solution.

Further, the columns of the group 1 chromatography system are packed with adsorbent. The adsorbent media is selected according to the nature of the ions contained in the feed to be treated and the nature of the mixture. The adsorption medium is strong acid cation adsorption resin, or weak base anion adsorption resin, or acrylic acid anion adsorption resin, or cation molecular sieve. The chromatographic column of the 1 st group of chromatographic systems is connected with a feeding valve besides an impurity valve, and the feeding valve is connected to a feeding pipe; when the feed valve is opened, feed liquid flows out, and the feed liquid flows to the 2 nd group of chromatographic systems through the feed pipe and is used as the feed of the 2 nd group of chromatographic systems. In the group 1 chromatography system, since the adsorbent packed in the column has a weak adsorption ability for the dye and impurity ions and a strong adsorption ability for the substances such as sugars and alcohols, the dye and impurity ions are separated from the substances such as sugars and alcohols and are discharged from the system one after another. The feed liquid flowing into the impurity tank is rich in pigment and impurity ions.

4 columns of the group 2 chromatography system are packed with adsorbent. The adsorbent media is selected according to the nature of the mixture to be separated. The adsorbent is strong acid cation adsorption resin, or weak base anion adsorption resin, or acrylic acid anion adsorption resin, or cation molecular sieve.

Furthermore, the separation temperature is 20-90 ℃, the pressure in the chromatographic column is 0.1-1 MPa, and the linear velocity of the materials in the chromatographic column is 1-5 m/h.

The volume of the separated product and the volume of the internal circulation liquid are obtained after measurement and accumulation through a flowmeter and are used for controlling the opening and closing of corresponding valves, controlling the inlet and outlet of materials and controlling the starting and stopping of the internal circulation.

Besides, the conventional auxiliary facilities such as a feeding system, an eluent inlet system, a discharging storage tank, pressure measurement, flow measurement and the like are provided.

The feed liquid flowing into the dilute liquid tank has similar components and relatively dilute concentration as the feed raw material. The feed liquid is collected, concentrated and mixed with the feed material to enter the system again.

The device of the present invention can be used for decolorizing deionization and mixture separation of the following substances but is not limited to: the sulfurous acid cooking liquor for making paper, various molasses containing monosaccharide, disaccharide and polysaccharide, high fructose syrup, glucose-mannose polysaccharide liquor, invert sugar mixture, maltose syrup, maltitol liquor, mannitol-sorbitol mixed liquor, sugar alcohol production crystallization mother liquor, organic acid, plant extract and the like.

The main function of the 1 st group of chromatographic systems is to separate most of the pigment and impurity ions out of the system, the rest material liquid is used as the feed of the 2 nd group of chromatographic systems, and the material liquid is continuously separated in the 2 nd group of chromatographic systems to remove a small amount of pigment and impurity ions, and simultaneously, the mixture is also separated.

The feed, elution, and circulation sections of group 1 chromatography systems were all completed in 1 column. And (3) feeding the feed liquid containing the pigment, the impurity ions and the mixture into a chromatographic column, flowing through the chromatographic column, removing the pigment and the impurity ions from the mixture, flowing out of the lower part of the chromatographic column, and flowing into the 2 nd group of chromatographic system to be used as the feed of the 2 nd group of chromatographic system.

In the chromatographic system of group 1, the adsorption resin has no adsorption force or weak adsorption force on the pigment and impurity ions, so that the pigment, impurity ions and sugar alcohols have different migration speeds in the adsorption medium, the pigment and impurity ions move fast, the sugar alcohols move slowly, and the pigment, impurity ions and sugar alcohols are gradually separated during feeding, elution and internal circulation.

In the 2 nd group of chromatographic systems, the partition valves between the chromatographic columns are opened, and 4 chromatographic columns are connected in series to form an internal circulation. During the internal circulation, the feeding and the eluent are stopped, no material flows out of the column, and the system performs the internal circulation. In the internal circulation, the pigment, the impurity and B, C are gradually separated in the chromatographic column by the adsorption and desorption of the adsorption resin because of their different migration speeds in the adsorption medium.

It is another object of the present invention to provide a method of operating an apparatus for decolorizing, deionizing and separating mixtures.

The technical purpose of the invention is realized by the following technical scheme:

the device is operated periodically, four periods form a cycle, after the period I is finished, the period II is operated, then the period III and the period IV are operated, after the period IV is finished, the period I is returned, and the cycle is carried out; in each cycle, the chromatographic column of the chromatographic system of the 1 st group is a Y1 area; the 4 columns of the chromatography system of group 2 were zone Z1, zone Z2, zone Z3 and zone Z4 and moved forward with increasing number of cycles.

For group 1 chromatography systems, the Y1 zone is both the elution and feed sections.

For group 2 systems, zone Z1 is the elution zone, eluent enters the column from the top of zone Z1 and exits the column at the bottom of zone Z1. The extracting solution flows into the B liquid tank after being metered by a flowmeter and the flow of the extracting solution is regulated by a regulating valve.

The zone Z2 is a mixing section.

Zone Z3 is the feed zone, feed from group 1 chromatography system enters the column from the top of zone Z3, and pigment and impurity ions are removed from the bottom of zone Z3. The pigment and impurity ions in the part are mixed liquid of pigment and impurity ions which are remained after being separated by the 1 st group of chromatographic systems. The mixed liquid of the pigment and the impurity ions flows into an S liquid tank after the conductivity is detected by a conductivity meter, the flow is measured by a flowmeter and the flow is regulated by a regulating valve. The raffinate is discharged following the mixed liquid of the pigment and the impurity ions. And the raffinate flows into the C liquid tank after being metered by a flowmeter and the flow of the raffinate is regulated by a regulating valve.

The zone Z4 is a divided segment.

Further, each cycle consists of seven steps, and the seven steps of each cycle are as follows:

step 1: group 1 chromatography system, Y1 feed, which is a mixture of sugar alcohols, chiral species to be separated, collectively referred to as a mixture; y1, discharging the mixture after primary decolorization and ion removal in the previous period; the mixture from Y1 was fed to group 2 chromatography system via feed line. And in the 2 nd group of chromatographic systems, Z1 enters an eluent, Z1 produces an extracting solution, and the extracting solution is discharged into a liquid tank B through an extracting solution pipe, a third flow meter, a third flow regulating valve and an extracting solution branch. Feeding Z3, discharging pigment and impurity ion liquid from Z3, and discharging the pigment and the impurity ion liquid into an S liquid tank through a raffinate pipe, a second conductivity meter, a second flowmeter, a second flow regulating valve, a second impurity main valve VS2 and a second impurity branch.

And 2, step: and 2, feeding eluent into the chromatographic system 1, feeding eluent into the chromatographic system Y1, and discharging Y1, wherein the discharged material is a mixture and becomes the feed material of the chromatographic system 2 through a feeding pipe. And in the 2 nd group of chromatographic systems, feeding materials by Z3, discharging pigment and impurity ionic liquid by Z3, and discharging the pigment and the impurity ionic liquid into an S liquid tank through a raffinate pipe, a second conductivity meter, a second flowmeter, a second flow regulating valve, a second impurity main valve VS2 and a second impurity branch pipe.

And step 3: and in the group 1 of chromatographic systems, eluent is fed into Y1, and Y1 is discharged, wherein the discharged material is a mixed solution of a dilute mixture and pigment impurity ions and is discharged into an X liquid tank through an impurity pipe, a first conductivity meter, a first flowmeter, a first flow regulating valve, a first dilute liquid control valve VX and a dilute liquid branch. And in the 2 nd group of chromatographic systems, Z1 is filled with eluent, raffinate is extracted from Z3 through Z1, Z2 and Z3 and is discharged into a liquid C tank through a raffinate pipe, a second conductivity meter, a second flow regulating valve, a main liquid C valve VC and a raffinate branch.

And 4, step 4: group 1 chromatography system, Y1 with no feed nor discharge, Y1 was subjected to internal recycle. And in the 2 nd group of chromatographic systems, Z1 is filled with eluent, raffinate is extracted from Z3 through Z1, Z2 and Z3 and is discharged into a liquid C tank through a raffinate pipe, a second conductivity meter, a second flow regulating valve, a main liquid C valve VC and a raffinate branch.

And 5: group 1 chromatography system, no feed nor discharge of Y1, internal recycle of Y1; and 2, in the chromatographic system, materials do not enter and exit the system and are subjected to internal circulation.

And 6: in the group 1 of chromatographic systems, eluent is fed into Y1, and Y1 is discharged, wherein the discharged material is ion liquid rich in pigment and impurities and is discharged into an S liquid tank through an impurity pipe, a conductivity meter I, a flow regulating valve I and an impurity master valve VS 1; and 2, in the chromatographic system, materials do not enter and exit the system and are subjected to internal circulation.

And 7: in the group 1 of chromatographic systems, eluent is fed into Y1, and Y1 is discharged to form a mixed solution of a dilute mixture and pigment impurity ions, and the mixed solution is discharged into an X liquid tank through an impurity pipe, a conductivity meter I, a flow regulating valve and a dilute liquid main valve VX; and 2, in the chromatographic system, materials do not enter and exit the system and are subjected to internal circulation.

Further, after the cycle one is completed, the cycle two is operated, wherein the chromatographic system in the group 1 repeats the step of the cycle one, the chromatographic system in the group 2 also repeats the step of the cycle one, and the four zones Z1, Z2, Z3 and Z4 all advance to the next chromatographic column; after the second period is finished, the third period is operated, at this time, the chromatographic system in the 1 st group repeats the step of the second period, the chromatographic system in the 2 nd group also repeats the step of the second period, and the four zones Z1, Z2, Z3 and Z4 all advance one step to the next chromatographic column; after the cycle three is completed, running the cycle four, wherein the chromatographic system in the 1 st group repeats the step of the cycle three, the chromatographic system in the 2 nd group also repeats the step of the cycle three, and the four zones of Z1, Z2, Z3 and Z4 all advance one step to the next chromatographic column; and after the fourth period is finished, the first period is repeatedly operated, and the cycle is continuous.

As a modification of the present invention, the extract from the group 1 chromatography system is introduced into a buffer tank, and the extract is concentrated to a concentration of 55. + -.5% by mass and then pumped to the group 2 chromatography system, thereby improving the productivity of the group 2 chromatography system.

As another improvement of the invention, in the 2 nd group of chromatographic systems, the raffinate can be further subdivided into liquid C and liquid D, which are respectively fed into different storage tanks, so as to achieve the purpose of separating three components.

The invention provides a device for decoloring, deionizing and separating mixture and an operation method thereof, which integrate the traditional decoloring, filtering and ion exchange processes into a set of device for solution, do not need activated carbon for decoloring, save a large amount of acid and alkali used for ion exchange, reduce the production cost and have great benefits in the aspects of energy conservation, emission reduction and environmental protection.

Drawings

FIG. 1 is a view showing an assembly of an apparatus for decoloring, deionizing and separating a mixture. Group 1 chromatography systems consist of 1 column and group 2 chromatography systems consist of 4 columns. The solution flowing into the B liquid tank is extracting solution, the solution flowing into the C liquid tank is raffinate, the solution flowing into the S liquid tank is pigment and impurity ion liquid, and the solution flowing into the X liquid tank is dilute liquid.

The components in the drawings are as follows: the device comprises an isolating valve I1, a chromatographic column I2, a connecting pipe I3, a material valve I VFF, an eluent valve I VWW, a flow meter I55, a booster pump I41, a feeding valve VFS, an impurity valve VS, an impurity pipe 15, a conductivity meter I71, a flow meter I51, a flow regulating valve I61, an impurity main valve VS1, an impurity branch I34 and a dilute liquid branch 35;

the device comprises a second isolating valve 21, a second chromatographic column 22, a second connecting pipe 23, a main eluent pipe 11, a main material pipe 12, a feeding pipe 121, second material valves VF 1-VF 4, second eluent valves VW 1-VW 4, a second booster pump 42, extracting liquid valves VN 1-VN 4, an extracting liquid pipe 14, a third flow meter 53, a third flow regulating valve 63, an extracting liquid branch 31 and a fourth flow meter 54;

raffinate valve VM 1-VM 4, raffinate pipe 13, second conductivity meter 72, second flow meter 52, second flow control valve 62, raffinate main valve VC, raffinate branch 32, impurity main valve VS2 and impurity branch 33.

FIG. 2 is a seven step procedural diagram of a cycle one run. F is a feed; w is an eluent; b is extracted liquid; c is raffinate; s is a pigment and impurity ionic liquid; x is a dilute solution; the black body in the column indicates that there is flow through.

Detailed Description

The apparatus of the present invention will be described in further detail with reference to the accompanying drawings.

Example 1

A device for decoloring, deionizing and separating mixture comprises a 1 st group of chromatographic systems and a 2 nd group of chromatographic systems, as shown in figure 1, the 1 st group of chromatographic systems consists of 1 chromatographic column, and an outlet and an inlet of the first chromatographic column 2 are connected through a booster pump 41, a block valve 1, a connecting pipe 3 and a flow meter 54; an inlet of the first chromatographic column 2 is connected with an eluent valve VWW and a material valve VFF; the eluent valve I VWW and the material valve I VFF are respectively connected with the eluent main pipe 11 and the material main pipe 12; an outlet of the chromatographic column I2 is connected with an impurity valve VS and a feeding valve VFS; the feeding valve VFS is connected to a feeding pipe 121 and then is connected with the first feeding valves VF 1-VF 4 of the 2 nd group of chromatographic systems; the impurity valve VS is connected with an impurity pipe 15; a first conductivity meter 71 is arranged on the impurity tube 15 and is used for detecting the conductivity of the effluent liquid; the impurity pipe 15 is also provided with a first flowmeter 51 and a first flow regulating valve 61 for detecting and regulating flow; the impurity pipe 15 is divided into two branches after passing through a first flow regulating valve 61: the first impurity branch 34 is connected with the S liquid tank after passing through a first impurity main valve VS 1; and the dilute liquid branch is connected with the X liquid tank after passing through a dilute liquid main valve VX.

The 2 nd group of chromatographic systems are formed by connecting 4 chromatographic columns in series, and a booster pump II 42, a closing valve II 21 and a connecting pipe II 23 are arranged among the chromatographic columns; an eluent valve II VW 1-VW 4 and a material valve II VF 1-VF 4 are connected to the inlet of each chromatographic column of the 2 nd group of chromatographic systems; the eluent valve and the material valve are respectively connected with the eluent main pipe 11 and the feeding pipe 121; the outlet of each chromatographic column of the 2 nd group of chromatographic systems is connected with raffinate valves VM 1-VM 4 and extract valves VN 1-VN 4; the raffinate valves VM 1-VM 4 are connected with a raffinate pipe 13, and the extract liquid valves VN 1-VN 4 are connected with an extract liquid pipe 14; a second conductivity meter 72 is arranged on the raffinate pipe 13 and is used for detecting the conductivity of the effluent; the raffinate pipe 13 is also provided with a second flowmeter 52 and a second flow regulating valve 62 for detecting and regulating flow; the residual liquid extracting pipe 13 is divided into two branches after passing through a second flow regulating valve 62: the second impurity branch 33 is connected with the S liquid tank after passing through an impurity main valve VS 2; the raffinate branch 32 is connected with a liquid C tank after passing through a liquid C main valve VC; and a third flow meter 53 and a third flow regulating valve 63 are arranged on the extracting liquid pipe 14 and are used for detecting and regulating the flow, and then the extracting liquid pipe is connected with the B liquid tank after passing through the extracting liquid branch 31.

Distributing devices for uniformly distributing materials are arranged above and below the chromatographic columns in the chromatographic systems of the 1 st group and the chromatographic systems of the 2 nd group, so that the materials form columnar flow in the columns.

Further, the columns of group 1 chromatography systems are packed with adsorbent. The adsorbent media is selected according to the nature of the ions contained in the feed to be treated and the nature of the mixture. The adsorption medium is strong acid cation adsorption resin, or weak base anion adsorption resin, or acrylic acid anion adsorption resin, or cation molecular sieve. The chromatographic column of the 1 st group of chromatographic systems is connected with a feeding valve besides an impurity valve, and the feeding valve is connected to a feeding pipe; when the feed valve is opened, the feed liquid flows out, and the feed liquid flows to the 2 nd group of chromatographic systems through the feed pipe to be used as the feed of the 2 nd group of chromatographic systems. In the group 1 chromatography system, since the adsorbent packed in the column has a weak adsorption ability for the dye and impurity ions and a strong adsorption ability for the substances such as sugars and alcohols, the dye and impurity ions are separated from the substances such as sugars and alcohols and are discharged from the system one after another. The feed liquid flowing into the impurity tank is rich in pigment and impurity ions.

Further, the eluent is pure water, methanol water solution, ethanol water solution, organic acid solution or inorganic acid solution.

Besides, the conventional auxiliary facilities such as a feeding system, an eluent inlet system, a discharge storage tank, pressure measurement, flow measurement and the like are provided.

The feed, elution, and circulation sections of group 1 chromatography system were all completed in 1 column. And (3) feeding the feed liquid containing the pigment, the impurity ions and the mixture into a chromatographic column, flowing through the chromatographic column, removing the pigment and the impurity ions from the mixture, flowing out from the lower part of the chromatographic column, and flowing to the 2 nd group of chromatographic system to be used as the feed of the 2 nd group of chromatographic system.

In the chromatographic system of group 1, the adsorption resin has no adsorption force or weak adsorption force on the pigment and impurity ions, so that the pigment, impurity ions and sugar alcohols have different migration speeds in the adsorption medium, the pigment and impurity ions have high migration speeds, the sugar alcohols have low migration speeds, and the pigment, impurity ions and sugar alcohols are gradually separated during feeding, elution and internal circulation.

Example 2

A decolours and removes the operation method of the ion and separation mixture apparatus, the apparatus runs periodically, four cycles make up a cycle, after the cycle one finishes, run cycle two, then run cycle three, cycle four, after cycle four finishes, return to cycle one, go on circularly; in each cycle, the chromatographic column of the chromatographic system of the 1 st group is a Y1 area; the 4 columns of the chromatography system of group 2 were zone Z1, zone Z2, zone Z3 and zone Z4 and moved forward with increasing number of cycles.

Each cycle consists of seven steps. The three processes of feeding, elution and internal circulation are contained in seven steps. Fig. 2 shows a seven-step procedural diagram of a cycle-by-cycle operating process. Seven steps per cycle are as follows:

step 1: in the 1 st group of chromatographic systems, Y1 is fed, Y1 is discharged, and the feed is a mixture to be separated from saccharides, alcohols and chiral substances, and is collectively called a mixture; the mixture from Y1 was fed to group 2 chromatography system via feed line 121. In the group 2 chromatographic system, eluent enters Z1, an extracting solution exits Z1, and the extracting solution is discharged into a liquid tank B through an extracting solution pipe (14), a flow meter III 53, a flow regulating valve III 63 and an extracting solution branch 31; feeding Z3, discharging pigment and impurity ionic liquid from Z3, discharging the pigment and impurity ionic liquid into an S liquid tank through a raffinate pipe 13, a second conductivity meter 72, a second flow meter 52, a second flow regulating valve 62, a second impurity main valve VS2 and a second impurity branch 33;

step 2: the eluent is fed into the chromatographic system of the group 1, the eluent is fed into the chromatographic system of the group Y1, and the discharge is fed into the chromatographic system of the group Y1, and the discharge is a mixture and becomes the feed of the chromatographic system of the group 2 through a feeding pipe 121; feeding the material into a group 2 chromatographic system Z3, discharging pigment and impurity ionic liquid from Z3, and discharging the pigment and the impurity ionic liquid into an S liquid tank through a raffinate pipe 13, a second conductivity meter 72, a second flowmeter 52, a second flow regulating valve 62, a second impurity main valve VS2 and a second impurity branch 33;

and step 3: in the group 1 of chromatographic systems, eluent is fed into Y1, and Y1 is discharged to form a mixed solution of a dilute mixture and pigment impurity ions, and the mixed solution is discharged into an X liquid tank through an impurity pipe 15, a first conductivity meter 71, a first flowmeter 51, a first flow control valve 61, a dilute liquid control valve VX and a dilute liquid branch 35; in the group 2 chromatographic system, eluent is introduced into Z1, raffinate is extracted from Z3 through Z1, Z2 and Z3 and is discharged into a liquid C tank through a raffinate pipe 13, a second conductivity meter 72, a second flow meter 52, a second flow regulating valve 62, a main liquid C valve VC and a raffinate branch 32;

and 4, step 4: group 1 chromatography system, no feed nor discharge of Y1, internal recycle of Y1; in the group 2 chromatographic system, eluent is introduced into Z1, raffinate is extracted from Z3 through Z1, Z2 and Z3 and is discharged into a liquid C tank through a raffinate pipe 13, a second conductivity meter 72, a second flow meter 52, a second flow regulating valve 62, a main liquid C valve VC and a raffinate branch 32;

and 5: group 1 chromatography system, no feed nor discharge of Y1, internal recycle of Y1; the 2 nd group of chromatographic systems do not feed materials into or out of the system and carry out internal circulation;

step 6: in the group 1 of chromatographic systems, eluent is fed into Y1, and the material is discharged from Y1, is a liquid rich in pigment and impurity ions and is discharged into an S liquid tank through an impurity pipe 15, a first conductivity meter 71, a first flowmeter 51, a first flow regulating valve 61 and a first impurity valve VS 1; the 2 nd group of chromatographic systems, materials do not enter and exit the system, and carry out internal circulation;

and 7: in the group 1 of chromatographic systems, eluent is fed into Y1, and Y1 is discharged to form a mixed solution of a dilute mixture and pigment impurity ions, and the mixed solution is discharged into an X liquid tank through an impurity pipe 15, a first conductivity meter 71, a first flowmeter 51, a first flow regulating valve 61 and a main dilute liquid valve VX; and 2, in the chromatographic system, materials do not enter and exit the system and are subjected to internal circulation.

Further, after the cycle one is completed, the cycle two is operated, wherein the chromatographic system in the group 1 repeats the step of the cycle one, the chromatographic system in the group 2 also repeats the step of the cycle one, and the four zones Z1, Z2, Z3 and Z4 all advance to the next chromatographic column; after the second period is finished, the third period is operated, at this time, the chromatographic system in the 1 st group repeats the step of the second period, the chromatographic system in the 2 nd group also repeats the step of the second period, and the four zones Z1, Z2, Z3 and Z4 all advance one step to the next chromatographic column; after the cycle three is completed, running a cycle four, wherein the chromatographic system of the group 1 repeats the step of the cycle three, the chromatographic system of the group 2 also repeats the step of the cycle three, and the four zones of Z1, Z2, Z3 and Z4 all advance one step to the next chromatographic column; and after the period four is finished, the operation period I is repeated, and the cycle is repeated.

Example 3

The following example further illustrates the invention in a pilot scale plant using the de-ionizing and separating mixture apparatus shown in FIG. 1.

The chromatographic system of group 1 had a column length of 3.5m and an internal diameter of 0.085 m.

The chromatographic column is filled with adsorption resin. The resin is strong acid cation exchange resin, sodium type, the crosslinking degree is 4.5-7.5%, and the volume total exchange capacity is more than or equal to 1.8 mol/ml. The resin is a uniform particle sphere with a diameter of 0.28 mm. Pure water is selected as the eluent.

Each column of the group 2 chromatography system had a length of 3m and an internal diameter of 0.072 m.

Each chromatographic column is filled with an adsorbent resin. The resin is a strong acid cation exchange resin, calcium type, and the volume total exchange capacity is more than or equal to 1.8 mol/ml. The resin is a uniform particle sphere with the diameter of 0.30 mm.

Pure water is selected as an eluent, the temperature in the column is 60-65 ℃, the pressure in the column is 0.1-0.6 MPa, and the flow speed in the column is 1-5 m/h.

The raw material is bagasse hydrolysate which is prepared by washing bagasse with water, removing ash, pretreating, adding 0.3-0.5% by mass of hydrochloric acid solution, and reacting at 110-126 ℃ for 2-4 h. Filtering the bagasse hydrolysate to remove mechanical impurities, and concentrating to 56.0% by mass. The bagasse hydrolysis concentrated solution has the conductivity of 300000-600000 mu s/cm and is black brown. Table 1 shows the conductivity of the solution before and after the treatment in the apparatus for removing ions and separating the mixture. Table 2 is a table of the composition of the solution before and after treatment in the apparatus for decolorizing, deionizing and separating mixtures.

TABLE 1 conductivity of solution before and after treatment in decolorizing deionization and separation mixtures apparatus

Name(s)	Conductivity,. mu.s/cm
		Concentrate before treatment	300000~600000
Treated xylose-rich liquid	3000~3500
		Treated arabinose-rich liquid	2500~3000

TABLE 2 table of solution components before and after treatment with decolorizing deionization and separation apparatus

The steps of the periodic operation of the pilot scale device, the feeding and discharging amount are as follows:

step 1: 2.0L of bagasse hydrolysis concentrate is input into Y1; 2.0L of feed liquid flows out from Y1 and is input into Z3, and 2.0L of feed liquid flows out from Z3 and is discharged into an S liquid tank; 2.0L of purified water was supplied to Z1, and 2.0L of the extract was discharged from Z1 and discharged into liquid B tank.

Step 2: 0.5L of pure water was fed into Y1, 0.5L of feed liquid was fed into Z3 after flowing out of Y1, and 0.5L of dye impurity ion liquid was fed into S liquid tank after flowing out of Z3.

And step 3: inputting 0.5L of pure water into Y1, and discharging 0.5L of dilute solution from Y1 into an X liquid tank; 0.5L of pure water was fed to Z1, and the raffinate was discharged from Z3 via Z1, Z2 and Z3, and discharged to the C liquid tank.

And 4, step 4: y1 is subjected to internal circulation, and the amount of the internal circulation is 2.0L; 2.0L of pure water was fed to Z1, passed through Z1, Z2 and Z3, and the raffinate was discharged from Z3 to the C tank.

And 5: y1 is subjected to internal circulation, and the amount of the internal circulation is 1.0L; z1, Z2, Z3 and Z4 are subjected to internal circulation, and the amount of the internal circulation is 1.0L.

Step 6: 3.0L of pure water is input into Y1, and 3.0L of pigment impurity ion liquid flows out from Y1 and is discharged into an S liquid tank; z1, Z2, Z3 and Z4 were subjected to internal circulation, and the amount of internal circulation was 3.0L.

And 7: inputting 0.5L of pure water into Y1, and discharging 0.5L of dilute solution from Y1 into an X liquid tank; z1, Z2, Z3 and Z4 were subjected to internal circulation, and the amount of internal circulation was 0.5L.

The respective 7 steps of period two to period four are the same as period one. And after the fourth period is finished, the operation returns to the first repeating period.

The period one to the period four constitute a large period.

After the system runs for 3-5 large cycles, the system reaches a balanced state.

The examples of the present invention are merely illustrative, and not restrictive, of the present invention. The person skilled in the art can carry out various inventive modifications of the method according to the invention, which are protected by patent laws, insofar as they are within the scope of the claims.

Claims

1. A decoloration deionization and separation mixture device, which consists of a 1 st group of chromatographic systems and a 2 nd group of chromatographic systems, and is characterized in that:

the 1 st group of chromatographic systems consists of m chromatographic columns, and the outlet and the inlet of the first chromatographic column (2) are connected through a booster pump I (41), a block valve I (1), a connecting pipe I (3) and a flow meter V (55); an inlet of the chromatographic column I (2) is connected with an eluent valve VWW and a material valve VFF; the eluent valve I VWW and the material valve I VFF are respectively connected with the eluent main pipe (11) and the material main pipe (12); an outlet of the first chromatographic column (2) is connected with an impurity valve VS and a feeding valve VFS; the feed valve VFS is connected to a feed pipe (121) and is further connected with a feed valve VF 1-VFn of the group 2 chromatographic system; the impurity valve VS is connected with an impurity pipe (15); a first conductivity meter (71) is arranged on the impurity tube (15) and is used for detecting the conductivity of the effluent liquid; the impurity pipe (15) is also provided with a first flowmeter (51) and a first flow regulating valve (61) for detecting and regulating flow; the impurity pipe (15) is divided into two branches after passing through a flow regulating valve I (61): the impurity branch I (34) is connected with the S liquid tank after passing through an impurity main valve I VS 1; the dilute liquid branch is connected with the X liquid tank after passing through a dilute liquid main valve VX; m = 1-2; n = 4-6;

the 2 nd group of chromatographic systems are formed by connecting n chromatographic columns in series, and a booster pump II (42), an isolating valve II (21) and a connecting pipe II (23) are arranged among the chromatographic columns; an eluent valve II VW 1-VWn and a material valve II VF 1-VFn are connected to the inlet of each chromatographic column of the group 2 chromatographic system; the eluent valve and the material valve are respectively connected with the eluent main pipe (11) and the feeding pipe (121); an outlet of each chromatographic column of the 2 nd group of chromatographic systems is connected with raffinate valves VM 1-VMn and extract valves VN 1-VNn; the raffinate valves VM 1-VMn are connected with a raffinate pipe (13), and the extract valves VN 1-VNn are connected with an extract pipe (14); a second conductivity meter (72) is arranged on the raffinate pipe (13) and is used for detecting the conductivity of the effluent; the residual liquid extracting pipe (13) is also provided with a second flowmeter (52) and a second flow regulating valve (62) for detecting and regulating the flow; the raffinate pipe (13) is divided into two branches after passing through a flow regulating valve II (62): the impurity branch II (33) is connected with the S liquid tank after passing through an impurity main valve II VS 2; a raffinate branch (32) is connected with a liquid C tank after passing through a liquid C main valve VC; a third flowmeter (53) and a third flow regulating valve (63) are arranged on the extracting liquid pipe (14) and are used for detecting and regulating the flow, and then the extracting liquid pipe is connected with the liquid tank B after passing through the extracting liquid branch (31);

the upper part and the lower part of the chromatographic column are provided with distributing devices for uniformly distributing materials; the chromatographic column is filled with an adsorption medium, and the adsorption medium is strong-acid cation adsorption resin, or weak-base anion adsorption resin, or acrylic acid anion adsorption resin, or a cation molecular sieve; the separation temperature in the chromatographic column is 20-90 ℃, the pressure in the chromatographic column is 0.1-1 MPa, and the linear velocity of the materials in the chromatographic column is 1-5 m/h; besides, the device also comprises conventional auxiliary facilities for a feeding system, an eluent inlet system, a discharge storage tank, pressure measurement and flow measurement;

the group 1 chromatographic system operation process at least comprises three steps: feeding, eluting and internally circulating; the group 2 chromatographic system operation process at least comprises three steps: feeding, eluting and internally circulating;

said group 1 chromatography system separating the pigment and impurity ions while feeding the group 2 chromatography system; the 2 nd group chromatographic system separates the mixture and also separates part of the pigment and impurity ions.

2. An operation method of a device for decoloring, deionizing and separating a mixture as described in claim 1, wherein the device is operated periodically, four periods constitute a cycle, after the first period is completed, the second period is operated, then the third period and the fourth period are operated, after the fourth period is completed, the first period is returned to and the cycle is performed; in each cycle, the chromatographic column of the chromatographic system of the 1 st group is a Y1 area; the 4 columns of the 2 nd chromatographic system are zone Z1, zone Z2, zone Z3 and zone Z4 and move forward with increasing cycle number;

each cycle consists of seven steps, which are as follows:

step 1: in the 1 st group of chromatographic systems, Y1 is fed, Y1 is discharged, and the feed is a mixture to be separated from saccharides, alcohols and chiral substances, and is collectively called a mixture; the mixture from Y1 is fed to group 2 chromatographic system via feed line (121); in the 2 nd group of chromatographic systems, Z1 enters an eluent, Z1 discharges an extracting solution, and the extracting solution is discharged into a liquid groove B through an extracting solution pipe (14), a flow meter III (53), a flow regulating valve III (63) and an extracting solution branch pipe (31); feeding materials by Z3, discharging pigment and impurity ionic liquid from Z3, discharging the pigment and impurity ionic liquid into an S liquid tank through a raffinate pipe (13), a second conductivity meter (72), a second flow meter (52), a second flow regulating valve (62), a second impurity main valve VS2 and a second impurity branch (33);

step 2: feeding eluent into the chromatographic system of the group 1, feeding eluent into the chromatographic system of the group Y1, and discharging Y1, wherein the discharged material is a mixture and becomes the feed material of the chromatographic system of the group 2 through a feeding pipe (121); feeding by Z3, discharging pigment and impurity ionic liquid by Z3, and discharging the pigment and impurity ionic liquid into an S liquid tank through a raffinate pipe (13), a second conductivity meter (72), a second flowmeter (52), a second flow regulating valve (62), a second impurity main valve VS2 and a second impurity branch (33);

and 3, step 3: in the group 1 of chromatographic systems, eluent is fed into Y1, and Y1 is discharged, wherein the discharged material is a mixed solution of a dilute mixture and pigment impurity ions and is discharged into an X liquid tank through an impurity pipe (15), a first conductivity meter (71), a first flowmeter (51), a first flow regulating valve (61), a dilute liquid control valve VX and a dilute liquid branch (35); in the 2 nd group of chromatographic systems, Z1 enters eluent, raffinate is extracted from Z3 through Z1, Z2 and Z3 and is discharged into a C liquid tank through a raffinate pipe (13), a second conductivity meter (72), a second flow meter (52), a second flow regulating valve (62), a C liquid main valve VC and a raffinate branch pipe (32);

and 4, step 4: group 1 chromatography system, Y1 with no feed nor discharge, Y1 with internal recycle; in the group 2 chromatographic system, eluent is fed into Z1, raffinate is discharged from Z3 through Z1, Z2 and Z3, and is discharged into a liquid C groove through a raffinate pipe (13), a conductivity meter II (72), a flow meter II (52), a flow regulating valve II (62), a liquid C main valve VC and a raffinate branch pipe (32);

step 6: in the group 1 of chromatographic systems, eluent is fed into Y1, and the material is discharged from Y1, is a liquid rich in pigment and impurity ions and is discharged into an S liquid tank through an impurity pipe (15), a conductivity meter I (71), a flow meter I (51), a flow regulating valve I (61) and an impurity main valve VS 1; the 2 nd group of chromatographic systems, materials do not enter and exit the system, and carry out internal circulation;

and 7: in the group 1 of chromatographic systems, eluent is fed into Y1, and Y1 is discharged, wherein the discharged material is a mixed solution of a dilute mixture and pigment impurity ions and is discharged into an X liquid tank through an impurity pipe (15), a first conductivity meter (71), a first flowmeter (51), a first flow regulating valve (61) and a dilute liquid main valve VX; and 2, in the chromatographic system, materials do not enter and exit the system and are subjected to internal circulation.

3. The method of claim 2, wherein the second cycle is performed after the first cycle is completed, wherein the first cycle is repeated by the chromatographic system of group 1, the first cycle is repeated by the chromatographic system of group 2, and the four zones Z1, Z2, Z3 and Z4 are all advanced one step toward the next chromatographic column; after the second period is finished, the third period is operated, at this time, the chromatographic system in the 1 st group repeats the step of the second period, the chromatographic system in the 2 nd group also repeats the step of the second period, and the four zones Z1, Z2, Z3 and Z4 all advance one step to the next chromatographic column; after the cycle three is completed, running the cycle four, wherein the chromatographic system in the 1 st group repeats the step of the cycle three, the chromatographic system in the 2 nd group also repeats the step of the cycle three, and the four zones of Z1, Z2, Z3 and Z4 all advance one step to the next chromatographic column; and returning to the first period after the fourth period is finished, and repeating the cycle.

4. The method of claim 2, wherein the eluent is pure water, aqueous methanol, aqueous ethanol, organic acid solution, or inorganic acid solution.