CN114606348A - Sucrose decoloring method and system - Google Patents

Sucrose decoloring method and system Download PDF

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Publication number
CN114606348A
CN114606348A CN202210240595.2A CN202210240595A CN114606348A CN 114606348 A CN114606348 A CN 114606348A CN 202210240595 A CN202210240595 A CN 202210240595A CN 114606348 A CN114606348 A CN 114606348A
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Prior art keywords
anion resin
zone
resin column
water
column
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Inventor
张天惕
苏鑫
唐海静
高建国
王圣昶
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Aoshangyuan Tianjin Co ltd
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Aoshangyuan Tianjin Co ltd
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Priority to CN202210240595.2A priority Critical patent/CN114606348A/en
Publication of CN114606348A publication Critical patent/CN114606348A/en
Priority to CN202210745626.XA priority patent/CN114807456B/en
Priority to PCT/CN2023/076190 priority patent/WO2023169166A1/en
Priority to LU505449A priority patent/LU505449B1/en
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    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00Purification of sugar juices
    • C13B20/14Purification of sugar juices using ion-exchange materials
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00Purification of sugar juices
    • C13B20/14Purification of sugar juices using ion-exchange materials
    • C13B20/146Purification of sugar juices using ion-exchange materials using only anionic ion-exchange material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/50Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
    • B01J49/57Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for anionic exchangers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/60Cleaning or rinsing ion-exchange beds
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00Purification of sugar juices
    • C13B20/14Purification of sugar juices using ion-exchange materials
    • C13B20/144Purification of sugar juices using ion-exchange materials using only cationic ion-exchange material
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K13/00Sugars not otherwise provided for in this class
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K13/00Sugars not otherwise provided for in this class
    • C13K13/002Xylose

Abstract

The invention discloses a sucrose decoloring method and a system, wherein the method comprises the following steps: (1) and (3) a decoloring procedure: (2) carrying out water sugar-lifting process; (3) a backwashing process; (4) a regeneration step; (5) and (5) leaching. The sucrose decolorizing system comprises a decolorizing zone, a water-top sugar zone, a backwashing zone, a regeneration zone and a leaching zone. The sucrose decoloring method and the sucrose decoloring system fully utilize the advantages of two different resins to achieve better decoloring effect, the color value after decoloring is reduced from 1200IU before decoloring to below 150IU, the decoloring rate is up to more than 85 percent, and meanwhile, the resin utilization rate is high, and the resin consumption can be saved.

Description

Sucrose decoloring method and system
Technical Field
The invention relates to a sucrose processing technology, in particular to a sucrose decoloring method and a sucrose decoloring system.
Background
In the refining production process of cane sugar taking cane as raw materials at present, in order to improve the yield, the mother liquor of crystallization separation can be repeatedly returned to the recycling before full filling, and then the color value of the material before crystallization is higher and higher, and the color quality of the crystallized product is seriously influenced. The traditional production process for decoloring the sucrose generally adopts the steps of adding activated carbon after full filling, decoloring and filtering to remove pigments, but the color value of the material is high due to high pigments in mother liquor and repeated reuse, so that the decoloring effect of the activated carbon is poor, the decoloring rate can only reach 50-60%, and the color value of the material is still as high as about 1200IU after the activated carbon is used for decoloring. Some manufacturers adopt fixed bed resin for decolorization, but the resin dosage is large, the utilization rate is low, and the decolorization rate is not ideal.
Disclosure of Invention
In order to solve the problem of poor sucrose decoloring effect in the prior art, the invention adopts a multi-unit continuous decoloring process to perform two-stage decoloring, thereby achieving better decoloring effect.
The invention provides a sucrose decoloring method, which comprises the following steps:
(1) and (3) a decoloring procedure: after the sucrose solution enters a plurality of acrylic acid anion resin columns which are formed in parallel, the effluent enters a plurality of styrene anion resin columns which are formed in parallel for two-stage decolorization;
(2) a water sugar-lifting procedure: performing water jacking on the acrylic acid anion resin column and the styrene anion resin column switched from the decoloring procedure by adopting water, and recovering the jacked materials;
(3) and (3) backwashing: backwashing the acrylic acid anion resin column and the styrene anion resin column switched by the water-based sugar-lifting process by using water;
(4) a regeneration procedure: regenerating an acrylic acid anion resin column and a styrene anion resin column which are switched out in a backwashing process by using a regeneration liquid, wherein the regeneration liquid is a mixed solution of NaCL and NaOH;
(5) leaching: leaching the acrylic acid anion resin column and the styrene anion resin column which are switched out in the regeneration process by adopting water;
and the acrylic acid anion resin column and the styrene anion resin column in the decoloring procedure, the water sugar-pushing procedure, the backwashing procedure, the regenerating procedure and the leaching procedure are switched according to the sequence of the procedures.
The number of the resin columns in the decoloring procedure, the water sugar-pushing procedure, the regeneration procedure and the leaching procedure is two or more, and the number of the resin columns in the backwashing procedure is one or more.
Acrylic acid anion resin columns in the decoloring procedure, the water-jet sugar procedure, the backwashing procedure, the regeneration procedure and the leaching procedure are adjacently arranged to form acrylic acid anion resin column units, styrene anion resin columns are adjacently arranged to form styrene anion resin column units, the acrylic acid anion resin column units and the styrene anion resin column units in the water-jet sugar procedure, the backwashing procedure, the regeneration procedure and the leaching procedure are arranged in parallel, and the same resin columns are correspondingly switched during switching. That is, the acrylic anion resin column of the previous step is switched to the acrylic anion resin column unit of the next step, and the styrene anion resin column of the previous step is switched to the styrene anion resin column unit of the next step. In the arrangement, the number of the resin columns in the decoloring procedure, the water sugar-pushing procedure, the backwashing procedure, the regenerating procedure and the leaching procedure is 2 or more than 2, and each procedure has two kinds of resin columns at the same time.
Acrylic acid anion resin columns and styrene anion resin columns in the decoloring procedure, the water sugar-pushing procedure, the backwashing procedure, the regeneration procedure and the leaching procedure are arranged at intervals, and switching is carried out according to the sequence of the process positions of the resin columns during switching. Because the two resin columns are arranged at intervals, taking the process of switching the decoloring procedure to the water sugar-lifting procedure as an example, the first of the decoloring procedure is the acrylic anion resin column during switching, the acrylic anion resin column is switched to the water sugar-lifting procedure after switching, the adjacent styrene anion resin column is switched to the first process position, and when switching again, the styrene anion resin column is switched to the water sugar-lifting procedure. In this arrangement, the resin columns in the decoloring step, the water-jet-saccharification step, the regeneration step and the rinsing step are two or more, and two or more resin columns are provided, while the backwashing step may be one resin column or more than one resin column, and when only one resin column is provided, the resin columns in each switching period are different in type.
In the regeneration process, in the arrangement of the resin columns which are arranged at intervals, in one switching period, the regeneration liquid only regenerates one resin column, and in the next switching period, the regeneration liquid regenerates the other resin column.
The temperature of the sucrose solution in the decolorization process is 70-80 ℃, and the mass percentage concentration of the sucrose is 50-55%.
The regeneration liquid is a mixed liquid of NaCl solution with the mass concentration of 8-10% and NaOH solution with the mass concentration of 0.5-1.0%.
When the mass percentage concentration of the sucrose in the effluent of the water-sugar-lifting procedure is more than or equal to 25 percent, returning the effluent to the feeding tank; and when the mass percentage concentration of the cane sugar in the liquid outlet is less than 25%, returning the liquid outlet to the sweet water tank.
And (4) performing sewage treatment when the sodium ion concentration of the effluent of the regeneration process is less than 2%, and recovering when the sodium ion concentration is more than or equal to 2%.
Recycling when the concentration of sodium ions in the effluent of the leaching process is more than or equal to 2 percent, and treating sewage when the concentration of the sodium ions is less than 2 percent.
The invention provides a sucrose decolorizing system, comprising:
a decolorization area: the device comprises an acrylic anion resin column unit and a styrene anion resin column unit, wherein the acrylic anion resin column unit and the styrene anion resin column unit are connected in series, the acrylic anion resin column unit comprises a plurality of acrylic anion resin columns connected in parallel, the styrene anion resin column unit comprises a plurality of styrene anion resin columns connected in parallel, and the liquid inlet of a decoloring area is a sucrose solution;
water-sugar-over-water region: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a decoloring area, and the feed liquid of a water and sugar-lifting area is water;
a backwashing area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a water-topped sugar zone, and the feed liquid of a backwashing zone is water;
a regeneration zone: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a backwashing area, and the feed liquid of a regeneration area is a NaCL and NaOH mixed solution;
a showering area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a regeneration zone, and the liquid inlet of a leaching zone is water;
acrylic acid anion resin columns and styrene anion resin columns in the decolorization zone, the water-top sugar zone, the backwashing zone, the regeneration zone and the leaching zone are switched according to the sequence of working procedures.
Two or more resin columns are arranged in the decolorizing zone, the water-topped sugar zone, the regeneration zone and the leaching zone, and one or more resin columns are arranged in the backwashing zone.
Acrylic acid anion resin columns in the decolorizing zone, the water-bearing zone, the backwashing zone, the regeneration zone and the leaching zone are adjacently arranged to form an acrylic acid anion resin column unit, the styrene anion resin columns are adjacently arranged to form a styrene anion resin column unit, the acrylic acid anion resin column units and the styrene anion resin column units in the water-bearing zone, the backwashing zone, the regeneration zone and the leaching zone are arranged side by side, and the same type of resin columns are correspondingly switched during switching. The decolorizing zone, the water-overhead-sugar zone, the backwashing zone, the regeneration zone and the leaching zone are provided with two or more resin columns, and each zone is provided with two resin columns.
Acrylic acid anion resin columns and styrene anion resin columns in the decolorizing zone, the water-top sugar zone, the backwashing zone, the regeneration zone and the leaching zone are arranged at intervals, and are switched according to the process position sequence of the resin columns during switching. The decolorizing zone, the water-topped sugar zone, the regeneration zone and the leaching zone are provided with two or more resin columns, and each zone is provided with two resin columns. When one resin column is arranged in the backwashing region, the types of the resin columns in the backwashing region are changed at intervals according to the switching period.
In one switching period, only one resin column in the regeneration area is communicated with the regeneration liquid inlet pipe, and in the next switching period, the other resin column in the regeneration area is communicated with the regeneration liquid inlet pipe.
The last resin column of the leaching area is connected with the same resin column of the regeneration area in series.
The acrylic acid anion resin column and the styrene anion resin column in the sucrose decolorizing system are small columns, and the diameter of the columns is 800mm-1400 mm. The column diameter ranges for large production grades.
Has the advantages that:
1. the resin utilization rate is high, and the resin consumption is saved;
2. the advantages of two different resins (large exchange capacity of acrylic pigments and wide adsorption selection range of styrene pigments) are fully utilized, a good decoloring effect is achieved, the color value is reduced from 1200IU before decoloring to below 150IU after decoloring, and the decoloring rate is up to more than 85%.
3. The column-string mode is adopted for water sugar-ejecting, leaching and regeneration, the water consumption and the consumption of the regenerant are low, and the water consumption is saved by more than 50 percent;
4. brine (waste liquid containing salt discharged by regeneration) is recycled during regeneration, and is recycled after membrane filtration treatment, so that the regenerant is saved by over 70%;
5. the leaching and regeneration are processed by the same type of resin columns in series, so that the mutual pollution is reduced, and the processing effect is improved;
6. the sweet water is used for washing the column in the sucrose decalcification process; the backwashing effluent is recycled to the sugar dissolving process, so that the discharge of sewage is greatly reduced.
7. The sucrose decolorization system can continuously feed and discharge materials, continuously elute and continuously regenerate, can fully automatically operate and does not need to be operated by personnel.
Drawings
FIG. 1 is a schematic flow diagram of a sucrose decolorization process according to the present invention.
Figure 2 is a process flow diagram of the sucrose decolorization process of example 1.
Figure 3 is a process flow diagram of the sucrose decolorization process of example 2 (showing cycle 1).
Figure 4 is a process flow diagram of the sucrose decolorization process of example 2 (showing cycle 2 after switching).
FIG. 5 is a schematic diagram showing the structure of a decoloring operation group in comparative example 2.
FIG. 6 is a schematic diagram showing the structure of a decoloring reserved group in comparative example 2.
FIG. 7 is a cycle bleed pH profile for comparative example 2 and example 3.
FIG. 8 is a plot of the periodic discharge color values of comparative example 2 and example 3.
In the figure, an acrylic acid anion resin column is referred to as an acrylic acid column for short, and a styrene anion resin column is referred to as a styrene column for short.
Detailed Description
The present invention will be described in detail with reference to examples.
The sucrose decoloring method comprises the following steps of:
and (3) a decoloring procedure: the mass percentage concentration is 50-55%, the temperature is 70-80 ℃, the sucrose solution with the color value less than 1200IU enters a plurality of acrylic acid anion resin columns which are formed in parallel, the effluent enters a plurality of styrene anion resin columns which are formed in parallel for two-stage decolorization, and the flow rate is 3BV (3 times of the volume of the resin); checking whether the color value of the effluent is less than or equal to 150 IU;
a water sugar-lifting procedure: performing water jacking on the acrylic acid anion resin column and the styrene anion resin column switched from the decoloring procedure by adopting water, and recovering the jacked materials; when the mass percentage concentration of the sucrose in the effluent is more than or equal to 25 percent, returning the effluent to the feeding tank; when the mass percentage concentration of the sucrose in the effluent is less than 25%, returning the effluent to the sweet water tank, wherein the sweet water in the sweet water tank can be used for the sucrose decalcification procedure;
and (3) backwashing: backwashing the acrylic acid anion resin column and the styrene anion resin column switched by the water-based sugar-lifting process by using water; the backwash effluent can be recycled to a sugar dissolving water tank for the sugar dissolving process;
a regeneration process: regenerating the acrylic acid anion resin column and the styrene anion resin column which are switched out in the backwashing procedure by using a regeneration liquid, wherein the regeneration liquid is a mixed solution of a NaCl solution with the mass concentration of 8-10% and a NaOH solution with the mass concentration of 0.5-1.0%; when the concentration of sodium ions in the effluent of the regeneration process is less than 2%, the effluent enters a sewage neutralization tank for sewage treatment, and when the concentration of sodium ions is more than or equal to 2%, the effluent is recovered to a brine recovery tank;
leaching: leaching the acrylic acid anion resin column and the styrene anion resin column which are switched out in the regeneration process by adopting water; when the sodium ion concentration of the effluent of the leaching process is more than or equal to 2 percent, the effluent is recycled to a brine recycling tank, and when the sodium ion concentration is less than 2 percent, the effluent enters a sewage neutralization tank for sewage treatment; the liquid in the brine recovery tank can be filtered by a membrane, the filtrate can return to the regenerant tank, and the concentrated slag is treated as waste liquid;
and the acrylic acid anion resin column and the styrene anion resin column in the decoloring procedure, the water sugar-pushing procedure, the backwashing procedure, the regenerating procedure and the leaching procedure are switched according to the sequence of the procedures.
Example 1 a sucrose decolorization system includes:
a decolorization area: the device comprises an acrylic anion resin column unit and a styrene anion resin column unit, wherein the acrylic anion resin column unit and the styrene anion resin column unit are connected in series, the acrylic anion resin column unit comprises a plurality of acrylic anion resin columns connected in parallel, the styrene anion resin column unit comprises a plurality of styrene anion resin columns connected in parallel, and the liquid inlet of a decoloring area is a sucrose solution;
water-sugar-over-water region: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a decoloring area, and the feed liquid of a water and sugar-lifting area is water;
a backwashing area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a water-topped sugar zone, and the feed liquid of a backwashing zone is water;
a regeneration zone: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a backwashing area, and the feed liquid of a regeneration area is a NaCL and NaOH mixed solution;
a showering area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a regeneration zone, and the feed liquid of a leaching zone is water;
acrylic acid anion resin columns and styrene anion resin columns in the decolorization zone, the water-top sugar zone, the backwashing zone, the regeneration zone and the leaching zone are switched according to the sequence of working procedures.
As shown in figure 2, the acrylic anion resin column and the styrene anion resin column in the decoloring area, the water-top sugar area, the backwashing area, the regeneration area and the leaching area are separately arranged to form an independent acrylic anion resin column unit and a styrene anion resin column unit, and the resin columns in the acrylic anion resin column unit and the styrene anion resin column unit in the former area are simultaneously switched to the next area during continuous switching. The acrylic acid anion resin column unit and the styrene anion resin column unit in the water overhead sugar zone, the backwashing zone, the regeneration zone and the leaching zone are arranged in parallel.
A plurality of resin columns are arranged in the acrylic acid anion resin column units of the water-topped sugar area, the regeneration area and the leaching area and are connected in series; the styrene anion resin column unit has a plurality of resin columns which are connected in series. The back washing area is two resin columns, one of which is an acrylic acid anion resin column, and the other is a styrene anion resin column.
The last acrylic acid anion resin column in the leaching area is connected with the first acrylic acid anion resin column in the regeneration area in series; the last styrene-based anion resin column in the leaching zone is connected with the first styrene-based anion resin column in the regeneration zone in series.
Example 2 a sucrose decolorization system includes:
a decolorization area: the device comprises an acrylic anion resin column unit and a styrene anion resin column unit, wherein the acrylic anion resin column unit and the styrene anion resin column unit are connected in series, the acrylic anion resin column unit comprises a plurality of acrylic anion resin columns connected in parallel, the styrene anion resin column unit comprises a plurality of styrene anion resin columns connected in parallel, and the liquid inlet of a decoloring area is a sucrose solution;
water-sugar-over-water region: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a decoloring area, and the feed liquid of a water and sugar-lifting area is water;
a backwashing area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a water-topped sugar zone, and the feed liquid of a backwashing zone is water;
a regeneration zone: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a backwashing area, and the feed liquid of a regeneration area is a NaCL and NaOH mixed solution; is a mixed solution of NaCl solution with the mass concentration of 8-10% and NaOH solution with the mass concentration of 0.5-1.0%;
a showering area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a regeneration zone, and the feed liquid of a leaching zone is water;
acrylic acid anion resin columns and styrene anion resin columns in the decolorization zone, the water-top sugar zone, the backwashing zone, the regeneration zone and the leaching zone are switched according to the sequence of working procedures.
As shown in fig. 3-4, the acrylic acid anion resin columns and the styrene anion resin columns of the decolorizing zone, the water-topped sugar zone, the backwashing zone, the regeneration zone and the leaching zone are arranged at intervals, the acrylic acid anion resin columns and the styrene anion resin columns are sequentially switched to the next zone during continuous switching, one resin column is switched each time, as shown in fig. 3, the column No. 4 in the decolorizing zone is the acrylic acid anion resin column, the adjacent column No. 5 is the styrene anion resin column, as shown in fig. 4 after switching, the column No. 4 is switched to the water-topped sugar zone, and the column No. 5 is switched to the original column No. 4 process position.
The water-topped sugar zone comprises a plurality of resin columns which are connected in series, the acrylic acid anion resin columns and the styrene anion resin columns are arranged at intervals and connected in series, as shown in figure 3, the water-topped sugar zone comprises a No. 1 column (styrene anion resin column), a No. 2 column (acrylic acid anion resin column) and a No. 3 column (styrene anion resin column), the 3 columns are connected in series, and water flows through the No. 1 column, the No. 2 column and the No. 3 column in sequence. After switching, as shown in fig. 4, the water headspace includes column No. 2 (acrylic anion resin column), column No. 3 (styrene anion resin column) and column No. 4 (acrylic anion resin column), and column No. 2, column No. 3 and column No. 4 are connected in series as well.
The backwash zone comprises a resin column and the resin column in the backwash zone is switched from the water overhead so that different types of resin columns are used in different cycles, as shown in figure 3, and the resin column in the backwash zone in cycle 1 is column No. 20 (acrylic acid anion resin column). After the switching, as shown in FIG. 4, the resin column in the backwash zone was a No. 1 column (styrene-based anionic resin column).
The regeneration zone comprises a plurality of resin columns, the acrylic anion resin columns and the styrene anion resin columns are arranged at intervals, the same resin columns are connected in series, the water-topped sugar zone comprises a No. 17 column (styrene anion resin column), a No. 18 column (acrylic anion resin column) and a No. 19 column (styrene anion resin column) as shown in figure 3, the No. 17 column and the No. 19 column are connected in series, and the regeneration liquid flows through the No. 17 column and the No. 19 column in sequence. After switching, as shown in fig. 4, the water-topped sugar region includes a No. 18 column (acrylic acid anion resin column), a No. 19 column (styrene anion resin column) and a No. 20 column (acrylic acid anion resin column), the No. 18 column (acrylic acid anion resin column) and the No. 20 column (acrylic acid anion resin column) are connected in series, and the regeneration liquid flows through the No. 18 column and the No. 20 column in sequence.
The leaching zone comprises a plurality of resin columns, the acrylic anion resin columns and the styrene anion resin columns are arranged at intervals, the same resin columns are connected in series, the water-topped sugar zone comprises a 14 # column (acrylic anion resin column), a 15 # column (styrene anion resin column) and a 16 # column (acrylic anion resin column) as shown in figure 3, the 14 # column and the 16 # column are connected in series, water flows through the 14 # column and the 16 # column in sequence, meanwhile, the 16 # column is connected in series with the 18 # column of the regeneration zone, and the 16 # column and the 18 # column are the same column. After switching, as shown in fig. 4, the water-topped sugar zone comprises a No. 15 column (styrene-based anion resin column), a No. 16 column (acrylic acid-based anion resin column) and a No. 17 column (styrene-based anion resin column), and the No. 17 column (styrene-based anion resin column) and the No. 19 column (styrene-based anion resin column) of the regeneration zone are connected in series.
Example 3 sucrose decolorization was performed using the system of example 2 (resin amount is on a bench scale, again 20 columns, 10 per column)
The decolorization zone is divided into primary decolorization (a double column filled with acrylic anion resin) and secondary decolorization (a single column filled with styrene anion resin), sucrose solution is injected into the decolorization column in a countercurrent mode (bottom inlet and top outlet) as shown in figure 1, and the feeding conditions are as follows: 6L/h, 70 ℃, Bx 55%, PH 8.51, color value 1165ICUMSA, according to the arrow direction of the figure into the resin column, the feed rate is 30L. And collecting the discharged material, and detecting the pH value and the color value. The adsorption resins used in the resin column of FIG. 1 are shown in Table 1.
And (3) a water-topped sugar area, wherein after the introduction of the sucrose solution is finished, the No. 4 column shown in figure 3 is transferred to the water-topped sugar area to carry out string column water-topped sugar, 400ml of pure water enters from the top of the No. 2 column, and is stringed to the No. 3 column and the No. 4 column once as shown in figure 3, and water is discharged from the bottom of the No. 4 column. After switching of a plurality of periods, the No. 4 column can be sequentially switched to a backwashing area, a regeneration area and a leaching area.
The backwashing area, column 1 shown in figure 3, is fed with water from the bottom and discharged from the top to backwash the resin.
The regeneration zone, shown in fig. 3, adopts the regeneration of the string columns, because the resin columns are filled with two different types of resins at intervals, the regeneration string columns are two single columns adjacent to each other and the single columns are used as a group for regeneration; two adjacent double-column strings are regenerated as another group; only one group is regenerated in each period, and the two groups are regenerated alternately in turn. 400ml of regenerant of a mixed solution of 10 percent NaCL and 0.5 percent NaOH is injected from the top of the No. 18 column, the regenerated solution is connected to the No. 20 column after being discharged from the bottom of the No. 18 column and is discharged from the bottom of the No. 20 column, the first 160ml is discharged to a sewage neutralization tank, and the second 240ml is discharged to a brine collection tank.
A leaching area, 1, slowly leaching, injecting 400ml of pure water from the top of a No. 15 column, discharging water from the bottom, sequentially stringing the columns to No. 17 and No. 19 columns, discharging the water from the bottom of the No. 19 column, discharging the initial 200ml of pure water to a brine collection tank, and discharging the later 400ml of pure water to a sewage neutralization tank; 2. and (3) quickly leaching, injecting pure water from the top of the No. 15 column, discharging from the bottom, washing the residual sodium chloride and sodium hydroxide in the column, and discharging a sewage neutralization tank.
The decolorization system of the sucrose solution is recycled and regenerated for 20 times, the pH value and the color value of the discharged sucrose solution in the 1 st, 5 th, 10 th, 15 th and 20 th periods are detected, and the detection data are shown in the table 2; the analytical data of the exchange resin after 20 cycles are shown in Table 3.
Comparative example 1
The resins in the single-double resin column were all loaded with styrene type strong base anion resin, and the sucrose solution was decolorized and purified in the same manner as in example 3. The resins used in the comparative examples are shown in table 1 below.
The procedure of the decoloring system for water topping, backwashing, regeneration and leaching is the same as that of example 3.
The decolorization system of the sucrose solution is recycled and repeatedly regenerated for 20 times, the pH value and the color value of the discharged sucrose solution in the 1 st, 5 th, 10 th, 15 th and 20 th periods are detected in the same way as in example 3, and the detection data are shown in Table 4; the analytical data of the exchange resin after 20 cycles are shown in Table 5.
Table 1 comparative table of resins used in example 3 and comparative example 1
Figure BDA0003541008490000081
Table 2 table of discharge parameters of sucrose solution in each period of example 3
Cycle period 1 5 10 15 20
pH 8.44 8.37 8.56 8.38 8.51
Colour value 86 109 127 132 136
Table 3 table of resin exchange performance parameters after 20 cycles of example 3
Figure BDA0003541008490000091
TABLE 4 TABLE 1 TABLE OF DISCHARGE PARAMETERS OF SACCHARE SOLUTION IN COMPARATIVE EXAMPLE 1 FOR THE PERIODIC DISCHARGE
Cycle period 1 5 10 15 20
pH 8.54 8.46 8.37 8.32 8.26
Colour value 106 131 154 186 218
TABLE 5 resin exchange Performance after 20 cycles of comparative example 1 Table
Figure BDA0003541008490000092
As can be seen from comparison of the results in tables 2 and 4, the color value of comparative example 1 was increased by about 38% compared with that of example 1 and the resin exchange capacity was decreased by about 11.6% compared with that of example 1 after the cyclic decolorization was carried out for 20 cycles. Comparative example 1 showed a slight increase in the discharge color value compared to example 3.
As can be seen from the results in tables 3 and 5, the acrylic anion exchange resin in the double column can effectively adsorb macromolecular pigment as a primary decolorizing column, and is not easily polluted by pigment, so that the styrene anion resin in the single column as a secondary decolorizing column can be prevented from being rapidly polluted. Example 3 can effectively suppress the decrease in the total exchange capacity of the styrene-based anion resin as compared with comparative example 1.
Comparative example 2 (bench scale)
The method comprises the following steps of (1) adopting a floating bed ion-exchange two-stage decoloring mode, wherein one column consists of 4 columns, the 1# column is filled with acrylic acid strong base anion resin, the 2# column is filled with styrene strong base anion resin, and the 1# column and the 2# column are connected in series and fed for two-stage decoloring; the 3# and 4# columns are used as regeneration and backup columns as 1# and 2 #. The specific process is shown in FIGS. 5 and 6
And (3) decoloring: the decolorization feed was carried out in the same manner as in example 3, except that it consisted of only 2 floating beds of larger volume. The material enters from the bottom of the No. 1 column in a counter-current manner, is discharged from the top through the resin layer and is stringed to the bottom of the No. 2 column, enters, is adsorbed by the resin layer and is discharged from the top;
the water topping, backwashing, regeneration, and rinsing functions were performed simultaneously as in example 3 with multiple columns, and comparative example 2 was performed sequentially with only one column set.
The resins used in this comparative example are shown in table 6, the cycle of the decolorization system of sucrose solution is divided into 5 periods, the discharge detection is repeated for 3 periods, and the pH and color values of the discharged sucrose solution are shown in table 7, table 8, fig. 7 and fig. 8, which are the same as those of example 3, at 1 st, 2 nd, 3 rd, 4 th and 5 th times.
Table 6 comparative resin table used in example 3 and comparative example 2
Figure BDA0003541008490000093
Figure BDA0003541008490000101
Table 7 table of discharge parameters of sucrose solution in each period of example 3
Cycle period 1 2 3 4 5
pH 8.51 8.42 8.40 8.38 8.36
Colour value 90 105 125 136 139
TABLE 8 TABLE 2 TABLE OF DISCHARGE PARAMETERS OF SACCHARE SOLUTION IN SEPARATES/CYCLES
Cycle period 1 2 3 4 5
pH 8.82 8.76 8.37 8.32 8.16
Colour value 85 106 132 167 220
As can be seen from tables 7 and 8 and the graphs, the detection index of periodic discharge of comparative example 2 has larger fluctuation than that of example 3, the pH and color value are not stable as in example 3, the quality is obviously affected by the large fluctuation of the discharge detection index, and the discharge quality of comparative example 2 is lower than that of example 3. The resin amount of the embodiment 3 is saved by 50% according to the comparison of the resin amounts of the two; meanwhile, as the small column is adopted in the embodiment, the pressure of the feed liquid in the column is small during water sugar jacking, leaching, backwashing and regeneration, the feed liquid is uniformly distributed in the column, and the regenerant and water can be effectively saved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A sucrose decolorization method is characterized by comprising the following steps:
(1) and (3) a decoloring procedure: after the sucrose solution enters a plurality of acrylic acid anion resin columns which are formed in parallel, the effluent enters a plurality of styrene anion resin columns which are formed in parallel for two-stage decolorization;
(2) a water sugar-lifting procedure: performing water jacking on the acrylic anion resin column and the styrene anion resin column switched from the decoloring procedure by adopting water;
(3) and (3) backwashing: backwashing the acrylic anion resin column and the styrene anion resin column which are switched out in the water-based sugar-lifting procedure by using water;
(4) a regeneration process: regenerating an acrylic acid anion resin column and a styrene anion resin column which are switched out in a backwashing process by using a regeneration liquid, wherein the regeneration liquid is a mixed solution of NaCL and NaOH;
(5) leaching: leaching the acrylic acid anion resin column and the styrene anion resin column which are switched out in the regeneration process by adopting water;
and the acrylic acid anion resin column and the styrene anion resin column in the decoloring procedure, the water sugar-pushing procedure, the backwashing procedure, the regenerating procedure and the leaching procedure are switched according to the sequence of the procedures.
2. The method for decoloring sucrose according to claim 1, wherein the temperature of the sucrose solution in the decoloring process is 70 to 80 ℃ and the concentration of sucrose in percentage by mass is 50 to 55%.
3. The method for decoloring sucrose according to claim 1, wherein the regeneration liquid is a mixture of a NaCl solution with a mass concentration of 8 to 10% and a NaOH solution with a mass concentration of 0.5 to 1.0%.
4. The sucrose decoloring method according to any one of claims 1 to 3, wherein acrylic anion resin columns in the decoloring process, the water-jet sugar process, the backwashing process, the regenerating process and the leaching process are adjacently arranged to form acrylic anion resin column units, styrene anion resin columns are adjacently arranged to form styrene anion resin column units, and the acrylic anion resin column units and the styrene anion resin column units in the water-jet sugar process, the backwashing process, the regenerating process and the leaching process are arranged in parallel, and when switching is performed, the same type of resin columns are correspondingly switched.
5. The sucrose decoloring method according to any one of claims 1 to 3, wherein the acrylic anion resin columns and the styrene anion resin columns in the decoloring step, the water-jet sugar step, the backwashing step, the regenerating step and the rinsing step are arranged at intervals, and are switched according to the process position sequence of the resin columns.
6. The method for decoloring sucrose of claim 5, wherein in the regeneration step, the regeneration liquid is used to regenerate only one type of resin column in one switching cycle, and the other type of resin column is regenerated in the next switching cycle.
7. A sucrose decolorization system, comprising:
a decolorization area: the device comprises an acrylic anion resin column unit and a styrene anion resin column unit, wherein the acrylic anion resin column unit and the styrene anion resin column unit are connected in series, the acrylic anion resin column unit comprises a plurality of acrylic anion resin columns connected in parallel, the styrene anion resin column unit comprises a plurality of styrene anion resin columns connected in parallel, and the liquid inlet of a decoloring area is a sucrose solution;
water-sugar-over-water region: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a decoloring area, and the feed liquid of a water and sugar-lifting area is water;
a backwashing area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a water-topped sugar zone, and the feed liquid of a backwashing zone is water;
a regeneration zone: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a backwashing area, and the feed liquid of a regeneration area is a NaCL and NaOH mixed solution;
a showering area: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched from a regeneration zone, and the feed liquid of a leaching zone is water;
acrylic acid anion resin columns and styrene anion resin columns in the decolorization zone, the water-top sugar zone, the backwashing zone, the regeneration zone and the leaching zone are switched according to the sequence of working procedures.
8. The sucrose decolorization system according to claim 7, wherein acrylic anion resin columns in the decolorization zone, the water acrose zone, the backwashing zone, the regeneration zone and the leaching zone are adjacently arranged to form an acrylic anion resin column unit, styrene anion resin columns are adjacently arranged to form a styrene anion resin column unit, and the acrylic anion resin column units and the styrene anion resin column units in the water acrose zone, the backwashing zone, the regeneration zone and the leaching zone are arranged in parallel, and when switching, the same type of resin columns are correspondingly switched.
9. The sucrose decolorization system of claim 7, wherein the acrylic acid anion resin columns and the styrene anion resin columns in the decolorization zone, the water-top sugar zone, the backwashing zone, the regeneration zone and the leaching zone are arranged at intervals, and are switched according to the process position sequence of the resin columns.
10. The sucrose decolorization system of claim 9, wherein only one resin column of the regeneration zone is in communication with the regeneration liquid inlet pipe during one switching cycle, and wherein another resin column of the regeneration zone is in communication with the regeneration liquid inlet pipe during the next switching cycle, and wherein the last resin column of the rinse zone is in series communication with the same resin column of the regeneration zone.
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