CN114522743B - Method for preparing sodium iso-vitamin C and decalcification method and system thereof - Google Patents
Method for preparing sodium iso-vitamin C and decalcification method and system thereof Download PDFInfo
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- CN114522743B CN114522743B CN202210233751.2A CN202210233751A CN114522743B CN 114522743 B CN114522743 B CN 114522743B CN 202210233751 A CN202210233751 A CN 202210233751A CN 114522743 B CN114522743 B CN 114522743B
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- 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
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/02—Column or bed processes
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- 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
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/10—Ion-exchange processes in general; Apparatus therefor with moving ion-exchange material; with ion-exchange material in suspension or in fluidised-bed form
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- 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
- B01J49/53—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for cationic exchangers
Abstract
The invention provides a decalcification method for preparing sodium iso-vitamin C, which comprises the following steps: decalcification is carried out on the reaction liquid to be decalcified by adopting a simulated moving bed, wherein the simulated moving bed comprises a water top acid zone, an ion exchange zone, a leaching zone, a regeneration zone and a backwashing zone which are connected in sequence. The invention also provides a decalcification system for preparing sodium iso-vitamin C and a method for preparing sodium iso-vitamin C. The decalcification method for preparing sodium iso-vitamin C has the advantages of high resin utilization rate, small resin consumption, high calcium ion removal rate and low acid and water consumption.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for preparing sodium iso-vitamin C and a decalcification method thereof.
Background
Sodium erythorbate, also known as sodium erythorbate and sodium D-erythorbate, is a preservative for food preservation, color assisting, and antioxidant. The production process of the sodium iso-vitamin C mainly comprises the following steps: glucose is used as a raw material for fermentation, calcium carbonate is added to produce calcium diketopyrrolopyrroate, sulfuric acid is added after the fermentation is completed, the calcium diketopolybutoxide is converted into diketopolybutoxide, the diketopolybutoxide is esterified by methanol, and sodium methoxide is used for conversion to obtain sodium iso-vitamin C.
In the process of converting the calcium diketopyrrolopyonate into the diketopolygluconate, calcium ions and sulfate radicals are combined to produce precipitate calcium sulfate, and the precipitate can be removed by plate and frame filtration, but the filtrate still has a lot of free calcium ions, if not removed, which can cause serious scaling of an evaporator in the subsequent working procedure. The method for removing the calcium ions adopts an ion exchange method at present, and the traditional process decalcification adopts two-stage ion exchange of a common bed, but the process has the defects of low resin utilization rate, large resin consumption, easy leakage of the calcium ions and high consumption of acid and water.
Disclosure of Invention
The invention aims to solve the technical problems of low resin utilization rate, large resin consumption, easy leakage of calcium ions and high consumption of acid and water of decalcification in the process for preparing sodium iso-vitamin C in the prior art.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a decalcification process for the preparation of sodium iso-vitamin C comprising the steps of:
decalcification is carried out on the reaction liquid to be decalcified by adopting a simulated moving bed, wherein the simulated moving bed comprises a water top acid zone, an ion exchange zone, a leaching zone, a regeneration zone and a backwashing zone which are connected in sequence.
Preferably, the water acid-pushing area is formed by connecting a plurality of resin columns in series; the leaching area is formed by connecting a plurality of resin columns in series; the regeneration zone is formed by connecting a plurality of resin columns in series; the ion exchange areas are multi-stage ion exchange, and the ion exchange areas of all stages are sequentially connected in series.
Preferably, the ion exchange area is three-stage ion exchange, and comprises a primary ion exchange area, a secondary ion exchange area and a tertiary ion exchange area which are sequentially connected in series;
the primary ion exchange area, the secondary ion exchange area and the tertiary ion exchange area are all formed by connecting a plurality of resin columns in parallel.
Preferably, the sum of the resin columns of the water top acid zone, the ion exchange zone, the leaching zone, the regeneration zone and the backwashing zone is more than or equal to 17; the number of the resin columns in the primary ion exchange area and the secondary ion exchange area is n, and the number of the resin columns in the tertiary ion exchange area is n+1. 1. The number of the ion exchange resin columns in the secondary ion exchange area is set to be the same, and the number is designed according to the content of calcium ions in materials, the flow rate of passing materials and the resin filling amount of the ion exchange columns. The third ion exchange area is the last stage of ion exchange area, and one more ion exchange resin column is arranged, namely n+1 ion exchange resin columns are arranged, so that decalcification effect can be ensured, and calcium ions are prevented from leaking to the final discharging.
Preferably, the water acid-pushing zone adopts a mode of three columns connected in series; three resin columns connected in series are adopted in the water acid-pushing zone, and are sequentially cut out after the primary ion exchange zone is failed; and/or the number of the groups of groups,
the ion exchange zone adopts strong acid cation resin, in particular macroporous strong acid styrene cation exchange resin with the particle size of 0.45-1.25 mm; and/or the number of the groups of groups,
the leaching area adopts a mode of three columns connected in series; three resin columns connected in series are adopted in the leaching zone and are regenerated resin columns sequentially cut out of the regeneration zone; and/or the number of the groups of groups,
the regeneration zone adopts a mode of three columns connected in series; three resin columns connected in series are adopted in the regeneration zone and are all backwashed resin columns which are sequentially cut out by the backwashing zone; and/or the number of the groups of groups,
the backwashing area adopts a single column backwashing mode; and one resin column adopted by the backwashing zone is a resin column cut after the water acid jacking zone is jacked.
Preferably, the water acid-propping zone adopts a mode of forward water inflow, water enters from the top of a first resin column of the water acid-propping zone, and flows into a second resin column and a third resin column in sequence, and low-unit feed liquid is discharged from the bottom of the third resin column;
the leaching area adopts a desalted water concurrent flow mode, water is fed from the top of a first resin column of the leaching area, the water is sequentially connected to a second resin column and a third resin column in series, and desalted feed liquid is discharged from the bottom of the third resin column;
the regeneration zone adopts a concurrent mode, acid liquor enters from a first resin column of the regeneration zone and is sequentially connected to a second resin column and a third resin column in series, and regenerated feed liquid is discharged from the bottom of the third resin column; wherein the acid liquor is formed by mixing hydrochloric acid with the concentration of 30% with desalted feed liquid discharged from the leaching area, and the hydrochloric acid concentration of the acid liquor is 4.5-5.0%;
the backwashing zone adopts a countercurrent water inlet mode, water is fed from the bottom of the resin column, and liquid after backwashing is discharged from the top of the resin column.
Preferably, the water inflow rate of the water top acid zone is 2-3 times of the resin volume/hour, and the concentration of the material in the material liquid at the bottom outlet of the first resin column of the water top acid zone is 0;
the water inflow rate of the leaching area is 6-8 times of the resin volume/hour, and the pH value of the feed liquid at the bottom outlet of the first resin column of the leaching area is 3.5-4.0;
the acid inlet flow rate of the regeneration zone is 1-1.5 times of the resin volume per hour, and the pH value of the feed liquid at the bottom outlet of the third resin column of the regeneration zone is less than 2.0;
the water inflow of the backwashing zone is 8-10 times of the resin volume/hour, and the liquid at the top outlet of the resin column of the backwashing zone is clarified.
The invention also provides a decalcification system for preparing sodium iso-vitamin C, which is used for realizing the decalcification method for preparing sodium iso-vitamin C.
Preferably, the decalcification system for preparing sodium iso-vitamin C comprises a water top acid zone, an ion exchange zone, a leaching zone, a regeneration zone and a backwashing zone which are connected in sequence; wherein, a water top material inlet valve is arranged at the water inlet of the water top acid area; a primary feed valve is arranged at the feed inlet of the primary ion exchange zone of the ion exchange zone, a secondary feed valve is arranged at the feed inlet of the secondary ion exchange zone, and a tertiary feed valve is arranged at the feed inlet of the tertiary ion exchange zone; a leaching valve is arranged at the water inlet of the leaching area; an acid inlet valve is arranged at the acid inlet of the regeneration zone; a backwash valve is arranged at the discharge outlet of the backwash area;
a light acid outlet valve is arranged at the outlet of the water acid jacking area; a primary discharge valve is arranged at the discharge port of the primary ion exchange area; a secondary discharge valve is arranged at the discharge port of the secondary ion exchange area; a third discharge valve is arranged at the discharge port of the third ion exchange area; a drain valve is arranged at the discharge outlet of the leaching area; a discharge valve is arranged at the discharge port of the regeneration zone; a backwash inlet valve is arranged at the water inlet of the backwash zone;
and a serial column valve is arranged at the bottom outlet of each resin column in series, and the serial column valve is positioned between the valve at the discharge outlet of each functional area and the bottom outlet of the resin column.
The invention also provides a method for preparing sodium iso-vitamin C, which adopts the decalcification method for preparing sodium iso-vitamin C to decalcifie.
The scheme of the invention at least comprises the following beneficial effects:
(1) The decalcification method for preparing sodium iso-vitamin C adopts a simulated moving bed continuous ion exchange technology, adopts a mode of combining parallel-serial connection with multistage series connection in a water acid-pushing zone, an ion exchange zone, a leaching zone, a regeneration zone and a backwashing zone, and realizes automatic and continuous operation of the system. Compared with the common sheet root resin column, the decalcification method has the advantages of small diameter, less resin filling amount, high resin utilization rate and 40 percent of resin saving amount; the acid and water consumption is low, the consumption of the regenerant hydrochloric acid can be saved by 50% in the string column regeneration zone, the consumption of water can be saved by about 30% in the string column water top acid zone and the string column leaching zone, and meanwhile, compared with the common bed ion exchange zone, the sewage discharge can be reduced by more than 50%.
(2) According to the decalcification method for preparing sodium iso-vitamin C, the ion exchange area is three-stage ion exchange, so that the high removal rate of discharged calcium ions can be ensured, 2000ppm of calcium ions are fed into the ion exchange area, the discharge calcium ions are less than 5ppm after three-stage ion exchange, and the removal rate of calcium ions reaches 99.8%.
(3) The decalcification system for preparing sodium iso-vitamin C provided by the invention adopts multiple valves to realize function switching and realizes automatic control in the whole process.
Drawings
FIG. 1 is a schematic diagram of a decalcification process for the preparation of sodium iso-vitamin C according to the present invention;
FIG. 2 is a schematic diagram of the structure of the water top acid zone of the decalcification system for preparing sodium iso-vitamin C of the present invention.
Wherein, 1, water acid-pushing area; 101. water acid pushing valve; 102. a first string valve; 103. a second string valve; 104. a fade acid outlet valve; 105. a return valve; 2. a primary ion exchange zone; 3. a secondary ion exchange zone; 4. a tertiary ion exchange zone; 5. a rinsing zone; 6. a regeneration zone; 7. and (5) backwashing the area.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
Example 1
The embodiment of the invention provides a decalcification method for preparing sodium iso-vitamin C, which comprises the following steps:
the reaction liquid to be decalcified is decalcified by adopting a simulated moving bed, as shown in figure 1, wherein the simulated moving bed comprises a water top acid zone 1, an ion exchange zone, a leaching zone 5, a regeneration zone 6 and a backwashing zone 7 which are connected in sequence. Wherein the water acid jacking area 1 is formed by connecting a plurality of resin columns in series; the leaching area 2 is formed by connecting a plurality of resin columns in series; the regeneration zone 3 is formed by connecting a plurality of resin columns in series; the ion exchange areas are multi-stage ion exchange, and the ion exchange areas of all stages are sequentially connected in series.
In order to achieve a good decalcification effect, the ion exchange area is three-level ion exchange and comprises a primary ion exchange area 2, a secondary ion exchange area 3 and a tertiary ion exchange area 4 which are sequentially connected in series; the primary ion exchange area 2, the secondary ion exchange area 3 and the tertiary ion exchange area 4 are formed by connecting a plurality of resin columns in parallel.
When the resin columns of each functional area are designed according to the content of calcium ions in the materials, the flow rate of the materials and the resin filling amount of the ion exchange columns, the sum of the resin columns of the water acid ejection area, the ion exchange area, the leaching area, the regeneration area and the backwashing area is more than or equal to 17. The number of the resin columns in the primary ion exchange area and the secondary ion exchange area is n, and the number of the resin columns in the tertiary ion exchange area is n+1. 1. The number of the ion exchange resin columns in the secondary ion exchange area is set to be the same, and the number is designed according to the content of calcium ions in materials, the flow rate of passing materials and the resin filling amount of the ion exchange columns. The third ion exchange area is the last stage of ion exchange area, and one more ion exchange resin column is arranged, namely n+1 ion exchange resin columns are arranged, so that decalcification effect can be ensured, and calcium ions are prevented from leaking to the final discharging. In this embodiment, the number of resin columns in the primary ion exchange area and the secondary ion exchange area is 6, and the number of resin columns in the tertiary ion exchange area is 7. The number of the resin columns in the water acid jacking area 1 is 3; the number of the resin columns in the leaching area 5 is 3; the number of the resin columns of the regeneration zone 6 is 3; the number of resin columns in the backwash zone 7 is 1. Each resin column is numbered in the order of arrangement, as shown in fig. 1, from left to right, respectively 1# column, 2# column to 30# column.
As a preferred implementation manner of this embodiment, the water acid-pushing zone adopts a three-column series connection manner; the three resin columns connected in series are adopted in the water acid-pushing zone, and are sequentially cut out after the primary ion exchange zone is in failure. The water acid-propping zone adopts a forward water inflow mode, water is introduced from the top of a first resin column (namely a 1# column) of the water acid-propping zone, and is sequentially connected to a second resin column (namely a 2# column) and a third resin column (namely a 3# column) in series, and low-unit feed liquid is discharged from the bottom of the third resin column. The water inflow rate of the water acid-pushing zone is 2-3 times of the resin volume/hour, and the concentration of the material in the material liquid at the bottom outlet of the first resin column of the water acid-pushing zone is 0.
The ion exchange zone adopts strong acid cation resin, in this embodiment, macroporous strong acid styrene cation exchange resin with the particle size of 0.45-1.25mm is adopted.
The leaching area adopts a mode of three columns connected in series; and three resin columns connected in series are adopted in the leaching zone, and are regenerated resin columns sequentially cut out in the regeneration zone. The leaching area adopts a desalted water concurrent flow mode, water is fed from the top of a first resin column (namely a 24# column) of the leaching area, and is sequentially connected to a second resin column (namely a 25# column) and a third resin column (namely a 26# column) in series, and desalted feed liquid is discharged from the bottom of the third resin column. The water inflow rate of the leaching area is 6-8 times of the resin volume/hour, and the pH value of the feed liquid at the bottom outlet of the first resin column of the leaching area is 3.5-4.0.
The regeneration zone adopts a mode of three columns connected in series; and three resin columns connected in series are adopted in the regeneration zone, and are backwashed resin columns sequentially cut out by the backwashing zone. The regeneration zone adopts a concurrent mode, acid liquor enters from a first resin column (namely a 27# column) of the regeneration zone and is sequentially connected to a second resin column (namely a 28# column) and a third resin column (namely a 29# column) in series, and regenerated feed liquid is discharged from the bottom of the third resin column; wherein the acid liquor is formed by mixing hydrochloric acid with the concentration of 30% with desalted feed liquid discharged from the leaching area, and the hydrochloric acid concentration of the acid liquor is 4.5-5.0%. The acid inlet flow rate of the regeneration zone is 1-1.5 times of the resin volume/hour, and the pH value of the feed liquid at the bottom outlet of the third resin column of the regeneration zone is less than 2.0.
The backwashing area adopts a single column backwashing mode; and one resin column adopted by the backwashing zone is a resin column cut after the water acid jacking zone is jacked. The backwashing zone adopts a countercurrent water inlet mode, water is fed from the bottom of the resin column, and liquid after backwashing is discharged from the top of the resin column. The water inflow of the backwashing zone is 8-10 times of the resin volume/hour, and the liquid at the top outlet of the resin column of the backwashing zone is clarified.
Specifically, in the decalcification method for preparing sodium iso-vitamin C according to this embodiment, water enters from the water inlet of the water top acid zone, is discharged from the discharge outlet, and enters into the ion exchange feed tank and the low unit feed liquid tank respectively according to different concentrations, the feed liquid entering the ion exchange feed tank enters into the primary ion exchange zone again, and at the same time, the reaction liquid to be decalcified (i.e. the acidified filtrate material containing calcium ions) is fed into the primary ion exchange zone through the feed pump, the low unit feed liquid and the acidified filtrate material enter from the top of the parallel resin columns in a concurrent manner, and then are contacted with the resin inside the resin columns to perform ion exchange, the 2-valent calcium ions in the acidified filtrate material are exchanged onto the cationic resin groups, and the H on the resin groups + Is displaced into the acidified filtrate material, and after a single ion exchange, the ions to be decalcified in the material are removed for a substantial portion, but no portion of the calcium ions are removed. Collecting the materials discharged from each resin column in the primary ion exchange zone into a primary discharge pipe, then entering the secondary ion exchange zone, and passing through a secondary ion exchange zoneThe calcium ions in the materials discharged from the tertiary ion exchange area are basically removed completely after the tertiary ion exchange, so that the requirements of the calcium ions can be met<5ppm index requirement.
Next, the resin column cut after the failure of the primary ion exchange zone is replaced to the water top acid zone to conduct water top acid. And replacing the resin column cut after the ejection of the water acid ejection area to the backwashing area, and backwashing. And replacing the resin column cut out after backwashing of the backwashing zone to the regeneration zone for regeneration. And replacing the resin cut out after regeneration in the regeneration zone to the leaching zone for leaching. The resin columns cut out of the ion exchange area are repeatedly utilized through water acid ejection, backwashing, regeneration and leaching, and the resin columns of the three ion exchange areas can be replaced by the resin columns cut out of the secondary ion exchange area after the resin columns of the primary ion exchange area are cut out, the resin columns of the secondary ion exchange area are replaced by the resin columns cut out of the tertiary ion exchange area, and the resin columns of the tertiary ion exchange area are replaced by the leached resin columns.
Example 2
The decalcification system for preparing sodium iso-vitamin C of the embodiment comprises a water top acid zone, an ion exchange zone, a leaching zone, a regeneration zone and a backwashing zone which are connected. Wherein, a water top material inlet valve is arranged at the water inlet of the water top acid area; a primary feed valve is arranged at the feed inlet of the primary ion exchange zone of the ion exchange zone, a secondary feed valve is arranged at the feed inlet of the secondary ion exchange zone, and a tertiary feed valve is arranged at the feed inlet of the tertiary ion exchange zone; a leaching valve is arranged at the water inlet of the leaching area; an acid inlet valve is arranged at the acid inlet of the regeneration zone; a backwash valve is arranged at the discharge outlet of the backwash area;
a light acid outlet valve is arranged at the outlet of the water acid jacking area; a primary discharge valve is arranged at the discharge port of the primary ion exchange area; a secondary discharge valve is arranged at the discharge port of the secondary ion exchange area; a third discharge valve is arranged at the discharge port of the third ion exchange area; a drain valve is arranged at the discharge outlet of the leaching area; a discharge valve is arranged at the discharge port of the regeneration zone; a backwash inlet valve is arranged at the water inlet of the backwash zone;
and a serial column valve is arranged at the bottom outlet of each resin column in series, and the serial column valve is positioned between the valve at the discharge outlet of each functional area and the bottom outlet of the resin column.
In the decalcification system for preparing sodium iso-vitamin C, when the valves and pipelines are designed and arranged, each resin column is provided with a corresponding inlet valve and a corresponding outlet valve in different functional areas, the inlet valve and the outlet valve are connected with a corresponding main pipeline, and when the resin column is in different functional areas to execute the function, the corresponding valves are controlled to be automatically opened through a PLC program, and the corresponding valves are automatically closed after the function is completed, so that the automatic control and the operation are realized. In this embodiment, taking the acid water top zone as an example, when acid water top is performed in the acid water top zone, as shown in fig. 2, the acid water top inlet valve 101 of the first resin column (i.e., column 1), the first string valve 102 of the first resin column, the second string valve 103 of the second resin column (i.e., column 2), the third string valve 104 of the third resin column (i.e., column 3), and the fade-out valve 105 are opened. The method is characterized in that acid is carried out by the water inlet top of a No. 1 column, the water inlet flow is controlled through a regulating valve and a flowmeter on a water inlet pipeline, the water inlet volume is calculated, a No. 1 column serial-column valve is opened to be serial to a No. 2 column inlet, a No. 2 column serial-column valve is opened to be serial to a No. 3 column inlet, a light acid outlet valve of a No. 3 column outlet is opened to discharge light acid, the concentration of materials is 0 in feed liquid at the bottom outlet of a first resin column in the water acid carrying area, and the acid outlet concentration of an initial volume is close to the feed concentration.
As a preferred implementation manner of this embodiment, a reflux valve 106 is further disposed on the main pipeline of the water acid lifting area. The outlet of the water acid jacking area is provided with a low-unit material liquid tank and an ion exchange feeding tank; the low unit feed liquid tank is connected with the weak acid outlet valve 105, and the ion exchange feed tank is connected with the reflux valve 106. When the reflux valve 106 is opened, the feed liquid is discharged to the ion exchange zone feed tank, when the acid concentration of the discharged feed liquid is low, the weak acid outlet valve 105 is opened, the reflux valve 106 is closed, and the discharged feed liquid is switched from the ion exchange feed tank to the low unit feed liquid tank.
As a preferred implementation manner of the embodiment, the decalcification system for preparing sodium iso-vitamin C is further provided with a valve frame, all valves are arranged on the valve frame to form a valve array, and a regulating valve and a flowmeter are arranged at the valve position on the valve array and are controlled by a PLC program. And setting flow and accumulated volume parameters of each functional area, and interlocking a PLC (programmable logic controller) with a flowmeter and a regulating valve, wherein the flow and accumulated volume of each functional area are controlled through parameter setting, so that the automatic conversion and control of each functional area are realized.
The valve frame comprises a first valve frame and a second valve frame, wherein the first valve frame is positioned at the top of the resin column, and is provided with a water jacking water inlet valve, a primary feeding valve, a secondary feeding valve, a tertiary feeding valve, a leaching valve, an acid inlet valve and a backwashing outlet valve. The second valve frame is positioned at the bottom of the resin column and is provided with a light acid outlet valve, a primary outlet valve, a secondary outlet valve, a tertiary outlet valve, a sewage draining valve, a discharge valve, a backwashing inlet valve and a column stringing valve. The arrangement mode is clear in pipeline and convenient for unified maintenance.
Example 3
The method for preparing sodium iso-vitamin C of the present embodiment comprises the steps of:
(1) Fermenting glucose as a raw material, and adding calcium carbonate into the glucose to generate fermentation liquor containing the calcium diketopyrrolopyrroate;
(2) Adding sulfuric acid into the fermentation liquor after fermentation in the step (1), converting the calcium diketopyrrolopyrrole into diketopolygluconic acid, combining calcium ions and sulfate radicals in the fermentation liquor to produce precipitate calcium sulfate, filtering and removing the precipitate by adopting a plate frame, taking the obtained filtrate as a reaction liquor to be decalcified, and decalcification by adopting a decalcification method for preparing sodium iso-vitamin C in the embodiment 1;
(3) And (3) taking the decalcified reaction solution obtained in the step (2), esterifying the diketopyrrolopyrrole acid in the decalcified reaction solution by methanol, and then converting the esterified diketopolygluconate acid by sodium methoxide to obtain sodium iso-vitamin C.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (7)
1. A decalcification process for the preparation of sodium iso-vitamin C, comprising the steps of:
decalcification reaction liquid is decalcified by adopting a simulated moving bed, wherein the simulated moving bed comprises a water top acid zone, an ion exchange zone, a leaching zone, a regeneration zone and a backwashing zone which are connected in sequence,
the water acid-pushing area is formed by connecting a plurality of resin columns in series; the leaching area is formed by connecting a plurality of resin columns in series; the regeneration zone is formed by connecting a plurality of resin columns in series; the ion exchange area is three-level ion exchange and comprises a primary ion exchange area, a secondary ion exchange area and a tertiary ion exchange area which are sequentially connected in series; the primary ion exchange area, the secondary ion exchange area and the tertiary ion exchange area are formed by connecting a plurality of resin columns in parallel;
the sum of the resin columns of the water acid-pushing zone, the ion exchange zone, the leaching zone, the regeneration zone and the backwashing zone is more than or equal to 17; the number of the resin columns in the primary ion exchange area and the number of the resin columns in the secondary ion exchange area are the same, and n are adopted; the number of resin columns in the tertiary ion exchange zone is n+1.
2. The decalcification process for preparing sodium iso-vitamin C according to claim 1, wherein said water top acid zone adopts a three column series connection mode; three resin columns connected in series are adopted in the water acid-pushing zone, and are sequentially cut out after the primary ion exchange zone is failed; and/or the number of the groups of groups,
the ion exchange zone adopts macroporous strong-acid styrene cation exchange resin with the particle size of 0.45-1.25 mm; and/or the number of the groups of groups,
the leaching area adopts a mode of three columns connected in series; three resin columns connected in series are adopted in the leaching zone and are regenerated resin columns sequentially cut out of the regeneration zone; and/or the number of the groups of groups,
the regeneration zone adopts a mode of three columns connected in series; three resin columns connected in series are adopted in the regeneration zone and are all backwashed resin columns which are sequentially cut out by the backwashing zone; and/or the number of the groups of groups,
the backwashing area adopts a single column backwashing mode; and one resin column adopted by the backwashing zone is a resin column cut after the water acid jacking zone is jacked.
3. The decalcification method for preparing sodium iso-vitamin C according to claim 2, wherein the water top acid zone adopts a mode of forward flow water inlet, water is fed from the top of the first resin column of the water top acid zone, the water is sequentially connected to the second resin column and the third resin column in series, and low unit feed liquid is discharged from the bottom of the third resin column;
the leaching area adopts a desalted water concurrent flow mode, water is fed from the top of a first resin column of the leaching area, the water is sequentially connected to a second resin column and a third resin column in series, and desalted feed liquid is discharged from the bottom of the third resin column;
the regeneration zone adopts a concurrent mode, acid liquor enters from a first resin column of the regeneration zone and is sequentially connected to a second resin column and a third resin column in series, and regenerated feed liquid is discharged from the bottom of the third resin column; wherein the acid liquor is formed by mixing hydrochloric acid with the concentration of 30% with desalted feed liquid discharged from the leaching area, and the hydrochloric acid concentration of the acid liquor is 4.5-5.0%;
the backwashing zone adopts a countercurrent water inlet mode, water is fed from the bottom of the resin column, and liquid after backwashing is discharged from the top of the resin column.
4. The decalcification process for producing sodium iso-vitamin C according to claim 2, wherein the water top acid zone has a water inflow rate of 2 to 3 times the volume of resin per hour and the concentration of the material in the feed liquid at the bottom outlet of the first resin column of the water top acid zone is 0;
the water inflow rate of the leaching area is 6-8 times of the resin volume/hour, and the pH value of the feed liquid at the bottom outlet of the first resin column of the leaching area is 3.5-4.0;
the acid inlet flow rate of the regeneration zone is 1-1.5 times of the resin volume per hour, and the pH value of the feed liquid at the bottom outlet of the third resin column of the regeneration zone is less than 2.0;
the water inflow of the backwashing zone is 8-10 times of the resin volume/hour, and the liquid at the top outlet of the resin column of the backwashing zone is clarified.
5. Decalcification system for the preparation of sodium iso-vitamin C, characterized in that it is used to implement a decalcification process for the preparation of sodium iso-vitamin C according to any one of claims 1-4.
6. The decalcification system for preparing sodium iso-vitamin C according to claim 5, wherein it comprises a water top acid zone, an ion exchange zone, a leaching zone, a regeneration zone, a backwashing zone, which are connected in sequence; wherein, a water top material inlet valve is arranged at the water inlet of the water top acid area; a primary feed valve is arranged at the feed inlet of the primary ion exchange zone of the ion exchange zone, a secondary feed valve is arranged at the feed inlet of the secondary ion exchange zone, and a tertiary feed valve is arranged at the feed inlet of the tertiary ion exchange zone; a leaching valve is arranged at the water inlet of the leaching area; an acid inlet valve is arranged at the acid inlet of the regeneration zone; a backwash valve is arranged at the discharge outlet of the backwash area;
a light acid outlet valve is arranged at the outlet of the water acid jacking area; a primary discharge valve is arranged at the discharge port of the primary ion exchange area; a secondary discharge valve is arranged at the discharge port of the secondary ion exchange area; a third discharge valve is arranged at the discharge port of the third ion exchange area; a drain valve is arranged at the discharge outlet of the leaching area; a discharge valve is arranged at the discharge port of the regeneration zone; a backwash inlet valve is arranged at the water inlet of the backwash zone;
and a serial column valve is arranged at the bottom outlet of each resin column in series, and the serial column valve is positioned between the valve at the discharge outlet of each functional area and the bottom outlet of the resin column.
7. A method for preparing sodium iso-vitamin C, characterized in that decalcification is carried out by using the decalcification method for preparing sodium iso-vitamin C according to any one of claims 1 to 4.
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| JP2002143869A (en) * | 2000-11-13 | 2002-05-21 | Tomita Pharmaceutical Co Ltd | Water cleaner |
| WO2020201411A1 (en) * | 2019-04-05 | 2020-10-08 | Novasep Process | Sugar processing method |
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| US4648976A (en) * | 1985-03-07 | 1987-03-10 | Belco Pollution Control Corporation | Integral water demineralizer system and method |
| CN101835727B (en) * | 2007-08-30 | 2013-08-07 | 埃欧金能源公司 | Process of removing calcium and obtaining sulfate salts from an aqueous sugar solution |
| CN101798327A (en) * | 2009-08-28 | 2010-08-11 | 郑州拓洋生物工程有限公司 | Preparation process of 2-keto-D-glucolactone |
| CN102029202B (en) * | 2010-10-29 | 2012-12-12 | 西安蓝晓科技新材料股份有限公司 | Continuous ion exchange unit for organic acid production |
| JP2015080750A (en) * | 2013-10-22 | 2015-04-27 | 栗田工業株式会社 | Ion exchange resin column |
| CN109850992B (en) * | 2019-03-29 | 2023-09-26 | 中国科学院沈阳应用生态研究所 | Water-fertilizer-salt ion input integrated regulation and control method and device for preventing and controlling secondary salinization of facility agriculture soil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002143869A (en) * | 2000-11-13 | 2002-05-21 | Tomita Pharmaceutical Co Ltd | Water cleaner |
| WO2020201411A1 (en) * | 2019-04-05 | 2020-10-08 | Novasep Process | Sugar processing method |
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