CN114807456B - Sucrose decoloring method and system - Google Patents
Sucrose decoloring method and system Download PDFInfo
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- CN114807456B CN114807456B CN202210745626.XA CN202210745626A CN114807456B CN 114807456 B CN114807456 B CN 114807456B CN 202210745626 A CN202210745626 A CN 202210745626A CN 114807456 B CN114807456 B CN 114807456B
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- 238000000034 method Methods 0.000 title claims abstract description 109
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 title claims abstract description 60
- 229930006000 Sucrose Natural products 0.000 title claims abstract description 60
- 239000005720 sucrose Substances 0.000 title claims abstract description 57
- 239000011347 resin Substances 0.000 claims abstract description 298
- 229920005989 resin Polymers 0.000 claims abstract description 298
- 238000011069 regeneration method Methods 0.000 claims abstract description 91
- 230000008929 regeneration Effects 0.000 claims abstract description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000011001 backwashing Methods 0.000 claims abstract description 53
- 238000002386 leaching Methods 0.000 claims abstract description 52
- 238000004042 decolorization Methods 0.000 claims abstract description 49
- -1 styrene anion Chemical class 0.000 claims description 144
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 112
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 48
- 239000007788 liquid Substances 0.000 claims description 46
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 31
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 21
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 230000001172 regenerating effect Effects 0.000 claims description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 229960004793 sucrose Drugs 0.000 description 44
- 230000000052 comparative effect Effects 0.000 description 22
- 239000000463 material Substances 0.000 description 11
- 150000001450 anions Chemical class 0.000 description 10
- 239000010865 sewage Substances 0.000 description 9
- 229910001415 sodium ion Inorganic materials 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000012267 brine Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 6
- 235000009508 confectionery Nutrition 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 5
- 239000012492 regenerant Substances 0.000 description 5
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 4
- 230000000737 periodic effect Effects 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 238000011021 bench scale process Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/14—Purification of sugar juices using ion-exchange materials
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/14—Purification of sugar juices using ion-exchange materials
- C13B20/146—Purification of sugar juices using ion-exchange materials using only anionic ion-exchange material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
- B01J49/57—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for anionic exchangers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/60—Cleaning or rinsing ion-exchange beds
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
- C13B20/00—Purification of sugar juices
- C13B20/14—Purification of sugar juices using ion-exchange materials
- C13B20/144—Purification of sugar juices using ion-exchange materials using only cationic ion-exchange material
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
-
- C—CHEMISTRY; METALLURGY
- C13—SUGAR INDUSTRY
- C13K—SACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
- C13K13/00—Sugars not otherwise provided for in this class
- C13K13/002—Xylose
Abstract
The invention discloses a sucrose decoloring method and a sucrose decoloring system, wherein the method comprises the following steps: (1) a decoloring step: (2) a water sugar-lifting procedure; (3) a backwashing step; (4) a regeneration step; and (5) a rinsing process. 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 decolorization method and the sucrose decolorization system fully utilize the advantages of two different resins to achieve better decolorization effect, the color value after decolorization is reduced to below 150IU from 1200IU before decolorization, the decolorization rate is up to more than 85%, and meanwhile, the resin utilization rate is high, and the resin dosage can be saved.
Description
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 existing cane sugar refining production process taking cane sugar as a raw material, in order to improve the yield, mother liquor separated by crystallization can be repeatedly recycled before full filling, so that the color value of a material before crystallization is higher and higher, and the color and quality of a crystallized product are seriously influenced. The sucrose decolorization in the traditional production process generally adopts the steps of adding activated carbon after saturation, decolorizing and filtering to remove pigments, but because the pigments in the mother liquor are high and the color value of the material is higher due to repeated recycling, the decolorization effect of the activated carbon is poor, the decolorization rate can only reach 50-60%, and the color value of the material is still as high as about 1200IU after the activated carbon decolorization. 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: carrying out 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 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 procedure: regenerating an acrylic acid anion resin column and a styrene anion resin column which are switched out in a backwashing procedure 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 procedure by adopting water;
and the acrylic acid anion resin column and the styrene anion resin column in the decoloring procedure, the water sugar-lifting procedure, the backwashing procedure, the regeneration 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 this arrangement, the number of the resin columns in the decoloring step, the water-sugar-lifting step, the backwashing step, the regenerating step, and the rinsing step is 2 or more, and each step 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-lifting procedure, the backwashing procedure, the regeneration procedure and the leaching procedure are arranged at intervals, and are switched 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, when the first resin column of the decoloring procedure is switched to be the acrylic anion resin column, the acrylic anion resin column is switched to the water sugar-lifting procedure after the switching, the adjacent styrene anion resin column is switched to be the first process position, and when the switching is performed again, the styrene anion resin column is switched to be 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 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 solution of NaCl solution with the mass percent concentration of 8-10% and NaOH solution with the mass percent 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 percent concentration of the cane sugar in the liquid outlet is less than 25%, the liquid outlet returns 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 decoloration system, which comprises:
a decolorization area: the decoloring 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 out 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.
Two or more resin columns are arranged in the decolorizing zone, the water-carrying sugar zone, the regenerating zone and the leaching zone, and one or more resin columns are arranged in the backwashing zone.
Adjacent arranging is acrylic acid class anion resin post unit between the acrylic acid class anion resin post in decoloration district, water overhead sugar district, backwash district, regeneration zone and the leaching district, and styrene class anion resin post adjacent arranging is styrene class anion resin post unit, and water overhead sugar district, backwash district, regeneration zone and the leaching district's acrylic acid class anion resin post unit and styrene class anion resin post unit set up side by side, and the same kind of resin post corresponds the switching 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 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 sequence of the process positions 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 area, the types of the resin columns in the backwashing area are changed according to the switching period interval.
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 kind of 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-1400mm. 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 pigment exchange capacity of acrylic resin and wide pigment adsorption selection range of styrene resin) are fully utilized to achieve better decoloring effect, 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 1 and example 3.
FIG. 8 is a plot of the periodic discharge color values of comparative example 1 and example 3.
FIG. 9 is a cycle bleed pH profile for comparative example 2 and example 3.
FIG. 10 is a plot of the periodic discharge color values of comparative example 2 and example 3.
In the figure, an acrylic anion resin column is abbreviated as propane, and a styrene anion resin column is abbreviated as benzene.
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 150IU; the next procedure can be carried out after the material is discharged from the tank after being decolored;
a water sugar-lifting procedure: carrying out 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, the effluent returns to the decoloring feeding tank; when the mass percent concentration of the sucrose in the effluent liquid is less than 25%, the effluent liquid returns to the sweet water tank, and the sweet water in the sweet water tank can be used for the sucrose decalcification process;
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; the backwash effluent can be recycled to a sugar dissolving water tank for the sugar dissolving process;
a regeneration procedure: regenerating an acrylic acid anion resin column and a styrene anion resin column which are switched out in a backwashing procedure by using a regeneration liquid, wherein the regeneration liquid is a mixed solution of 8-10% of NaCl solution and 0.5-1.0% of NaOH solution in percentage by mass; 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 procedure 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-lifting procedure, the backwashing procedure, the regeneration procedure and the leaching procedure are switched according to the sequence of the procedures.
Example 1 a sucrose decolorization system comprising:
a decolorization zone: 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 mixed solution of NaCl and NaOH;
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.
As shown in fig. 2, the acrylic anion resin column and the styrene anion resin column in the decoloring region, the water headspace region, the backwashing region, the regeneration region and the leaching region are arranged separately to form an independent acrylic anion resin column unit and an independent 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 region are switched to the next region simultaneously during continuous switching. The acrylic acid anion resin column unit and the styrene anion resin column unit in the water headspace area, the backwashing area, the regeneration area and the leaching area 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 comprises 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.
The sucrose decolorization system in the embodiment can totally share 1-20# acrylic anion resin column and 1-20# styrene anion resin column, and the number of the acrylic anion resin column and the styrene anion resin column distributed in each zone can be determined according to the sucrose treatment capacity.
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 out 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 mixed solution of NaCl and NaOH; is a mixed solution of NaCl solution with the mass percent concentration of 8-10 percent and NaOH solution with the mass percent concentration of 0.5-1.0 percent;
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 and 4, the acrylic anion resin columns and the styrene anion resin columns in the decolorization zone, the water-topped sugar zone, the backwashing zone, the regeneration zone and the leaching zone are arranged at intervals, the acrylic 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 decolorization zone is the acrylic anion resin column, the adjacent column No. 5 is the styrene anion resin column, and after switching, as shown in fig. 4, 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. One cycle is completed for each resin column switch.
The water-topped sugar zone comprises a plurality of resin columns which are connected in series, the acrylic anion resin columns and the styrene anion resin columns are arranged at intervals and connected in series, the water-topped sugar zone comprises a No. 1 column (styrene anion resin column), a No. 2 column (acrylic anion resin column) and a No. 3 column (styrene anion resin column) as shown in figure 3, 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 zone, so that different types of resin columns are used in different cycles, as shown in fig. 3, and the resin column in the backwash zone is a No. 20 column (acrylic acid anion resin column) in cycle 1. 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, as shown in figure 3, the regeneration 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), the No. 17 column and the No. 19 column are connected in series, and regeneration liquid sequentially flows through the No. 17 column and the No. 19 column. After switching, as shown in fig. 4, the regeneration zone includes column No. 18 (acrylic anion resin column), column No. 19 (styrene anion resin column) and column No. 20 (acrylic anion resin column), the column No. 18 (acrylic anion resin column) and column No. 20 (acrylic anion resin column) are connected in series, and the regeneration liquid flows through column No. 18 and column No. 20 in sequence.
The leaching zone comprises a plurality of resin columns, acrylic anion resin columns and styrene anion resin columns are arranged at intervals, the same resin columns are connected in series, as shown in figure 3, the leaching zone comprises a 14 # column (acrylic anion resin column), a 15 # column (styrene anion resin column) and a 16 # column (acrylic anion resin column), the 14 # column and the 16 # column are connected in series, water sequentially flows through the 14 # column and the 16 # column, 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 elution includes No. 15 column (styrene-based anion resin column), no. 16 column (acrylic anion resin column) and No. 17 column (styrene-based anion resin column), and No. 17 column (styrene-based anion resin column) and 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 per bench scale, again 20 columns, 10 columns each)
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 1165 ICUMSA, according to the arrow direction of the figure into the resin column, the feed rate is 30L. And collecting the discharged material to detect pH value and color value. The adsorption resins used in the resin column are shown in table 1. Fig. 3 shows a resin column arrangement in a cycle, and when the column No. 4 shown in fig. 3 is saturated, the column is switched to the next cycle, i.e., the resin column arrangement shown in fig. 4, and the material entering in other areas will be described below with reference to fig. 4.
The water-top sugar zone, as shown in fig. 4, enters 400ml of pure water from the top of column 2, as shown in fig. 4, is connected to column 3 and column 4 once, and water is discharged from the bottom of column 4. 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 4, is fed with water from the bottom and discharged from the top to backwash the resin.
The regeneration zone adopts the series column for regeneration, and the regeneration series column is formed by two single column series single columns which are adjacent to each other as a group of regeneration because the resin columns are filled with two different types of resins at intervals; two adjacent double-column strings are used as another group for regeneration; only one group is regenerated in each period, and the two groups are regenerated alternately in turn. As shown in FIG. 4, 10% NaCl and 0.5% NaOH were injected from the top of column 18, and the mixture was mixed with 400ml as a regenerant, which was discharged from the bottom of column 18, passed through column 20, and discharged from the bottom of column 20, the first 160ml was discharged to the wastewater neutralization tank, and the second 240ml was discharged to the brine recovery tank.
A leaching area, 1, leaching slowly, 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 from the bottom of the No. 19 column, discharging 200ml of pure water to a brine recovery tank, and then discharging 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 repeatedly regenerated for 20 times (20 cycles), 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 cycles are detected, and the detection data are shown in a table 2; the exchange performance analysis data of the resin after 20 cycles are shown in table 3.
TABLE 1 resin used in example 3
Table 2 table of discharge parameters of sucrose solution in each period of example 3
Table 3 table of resin exchange performance parameters after 20 cycles of example 3
Comparative example 1
The resins in the single and double resin columns are all filled with styrene type strong base anion resin, and the sucrose solution is decolored and refined by the same method as the embodiment 3. The resins used in the comparative examples are shown in table 4 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 was repeatedly regenerated 20 times (20 cycles), and the pH and color values of the discharged sucrose solution were measured in the same manner as in example 3 in the 1 st, 5 th, 10 th, 15 th and 20 th cycles, and the measurement data are shown in table 5; the analytical data of the exchange resin after 20 cycles are shown in Table 6.
Table 4 resin used in comparative example 1
TABLE 5 TABLE 1 TABLE OF DISCHARGE PARAMETERS OF SACCHARE SOLUTION IN COMPARATIVE EXAMPLE 1 OF PERIODIC CYCLES
TABLE 6 resin exchange Performance after 20 cycles of comparative example 1
The results of comparing example 3 with comparative example 1 can be seen in fig. 7 and fig. 8, and after 20 cycles of cyclic decolorization, the color value of comparative example 1 is increased by about 56.8% compared with that of example 3, and the increase amplitude is larger; the pH was also reduced by a greater extent than in example 3. The pH and color changes are more even for example 3.
As can be seen from the results in tables 3 and 6, the acrylic anion exchange resin in the double column can effectively adsorb macromolecular pigments as a primary decolorizing column, is not easily polluted by pigments and the like, and can avoid rapid pollution of styrene anion resin in the single column as secondary decolorizing. In example 3, the decrease in the total exchange capacity of the styrene-based anion resin can be effectively suppressed as compared with comparative example 1, and the decrease in the resin exchange capacity of comparative example 1 is about 11.8% higher than that of example 3.
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 column # 3 and column # 4 are identical to column # 1 and column # 2, and are used as regeneration and backup columns. 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;
and (3) transferring the saturated 1# and 2# resin columns to water material ejection, backwashing, regeneration and leaching, and simultaneously performing a decoloring procedure on the 3# column and the 4# column until the 3# column and the 4# column are also saturated, wherein the cycle period is.
Example 3 a plurality of columns simultaneously performed different processes, and comparative example 2 only performed decolorization by one column group and the other column group sequentially performed other processes.
The resins used in this comparative example are shown in table 7, the decolorization system of this comparative example is divided into 5 periods in an average cycle, the pH and color values of the discharged sucrose solutions in different periods of time are measured, 3 periods are repeated and averaged, the discharge data of these 5 periods can correspond to the pH and color values of the discharged sucrose solutions in the 1 st, 5 th, 10 th, 15 th and 20 th periods of example 3 (for convenience, the cycle period is written directly as 1, 5 th, 10 th, 15 th and 20 th periods, corresponding to example 3), and the measurement data are shown in table 7, table 8, and fig. 9 and fig. 10.
TABLE 7 resins used in comparative example 2
TABLE 8 TABLE 2 TABLE OF DISCHARGE PARAMETERS OF SACCHARE SOLUTION IN SEPARATES/CYCLES
As can be seen from the comparison between tables 7 and 8 and tables 1 and 2 and the graphs 9 and 10, the detection index of the periodic discharge of comparative example 2 has a significantly larger change range than that of example 3, the pH value and the color value are not stable as that of example 3, the quality is significantly affected by the large change range 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 percent according to the comparison of the resin amounts of the two; meanwhile, as the small column is adopted in the embodiment 3, the pressure of the feed liquid in the column is small during water top sugar, leaching, backwashing and regeneration, and the feed liquid is uniformly distributed in the column, so that 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 (4)
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 formed by parallel connection, liquid outlet enters a plurality of styrene anion resin columns formed by parallel connection for two-stage decolorization, wherein the temperature of the sucrose solution in the decolorization process is 70-80 ℃, and the mass percentage concentration of sucrose is 50-55%;
(2) A water sugar-lifting procedure: carrying out 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 procedure by using a regeneration liquid, wherein the regeneration liquid is a mixed solution of 8-10% of NaCl solution and 0.5-1.0% of NaOH solution in percentage by mass;
(5) Leaching: leaching the acrylic acid anion resin column and the styrene anion resin column which are switched out in the regeneration procedure by adopting water;
sequentially switching an acrylic acid anion resin column and a styrene anion resin column in the decoloring procedure, the water sugar-pushing procedure, the backwashing procedure, the regenerating procedure and the leaching procedure;
acrylic acid anion resin columns and styrene anion resin columns in the decoloring procedure, the water-sugar-lifting procedure, the backwashing procedure, the regeneration procedure and the leaching procedure are arranged at intervals, and are switched according to the sequence of the process positions of the resin columns during switching, wherein one resin column is switched every time;
the leaching process and the regeneration process adopt the same type of resin column string column treatment.
2. The method for decoloring sucrose of claim 1, 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.
3. 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, liquid entering a decoloring area is a sucrose solution, the temperature of the sucrose solution is 70-80 ℃, and the mass percentage concentration of the sucrose is 50-55%;
water-sugar-top zone: comprises an acrylic acid anion resin column and a styrene anion resin column which are switched out 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, wherein a regeneration liquid is a mixed solution of 8-10% of NaCl solution and 0.5-1.0% of NaOH solution in percentage by mass;
a shower 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 decolorizing zone, the water-top sugar zone, the backwashing zone, the regeneration zone and the leaching zone are switched according to the sequence of the working procedures;
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, and one resin column is switched every time;
the leaching area and the regeneration area adopt the same type of resin column to process.
4. The sucrose decolorization system according to claim 3, wherein only one resin column of the regeneration zone is connected to the regeneration liquid inlet pipe in one switching cycle, and the other resin column of the regeneration zone is connected to the regeneration liquid inlet pipe in the next switching cycle, and the last resin column of the rinsing zone is connected to the same resin column of the regeneration zone in series.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU505449A LU505449B1 (en) | 2022-03-10 | 2023-02-15 | Sucrose decoloring method and system |
| PCT/CN2023/076190 WO2023169166A1 (en) | 2022-03-10 | 2023-02-15 | Sucrose decoloring method and system |
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| CN202210240595.2A CN114606348A (en) | 2022-03-10 | 2022-03-10 | Sucrose decoloring method and system |
| CN2022102405952 | 2022-03-10 |
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| CN114606348A (en) * | 2022-03-10 | 2022-06-10 | 欧尚元(天津)有限公司 | Sucrose decoloring method and system |
| CN117583038B (en) * | 2024-01-18 | 2024-04-12 | 欧尚元智能装备有限公司 | Sucrose decalcification method and system |
| CN117599860B (en) * | 2024-01-23 | 2024-03-26 | 欧尚元智能装备有限公司 | Cephalosporium decoloring system and process |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114606348A (en) * | 2022-03-10 | 2022-06-10 | 欧尚元(天津)有限公司 | Sucrose decoloring method and system |
-
2022
- 2022-03-10 CN CN202210240595.2A patent/CN114606348A/en active Pending
- 2022-06-29 CN CN202210745626.XA patent/CN114807456B/en active Active
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2023
- 2023-02-15 LU LU505449A patent/LU505449B1/en active IP Right Grant
- 2023-02-15 WO PCT/CN2023/076190 patent/WO2023169166A1/en unknown
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| CN1817195A (en) * | 2006-03-15 | 2006-08-16 | 浙江大学 | Decoloring method for heliangine lixiviation liquid |
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Also Published As
| Publication number | Publication date |
|---|---|
| LU505449A1 (en) | 2023-12-11 |
| CN114606348A (en) | 2022-06-10 |
| CN114807456A (en) | 2022-07-29 |
| WO2023169166A1 (en) | 2023-09-14 |
| LU505449B1 (en) | 2024-03-11 |
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