CN109433169B - Method and device for improving separating capacity of old calcium type chromatographic resin - Google Patents
Method and device for improving separating capacity of old calcium type chromatographic resin Download PDFInfo
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- CN109433169B CN109433169B CN201811411304.1A CN201811411304A CN109433169B CN 109433169 B CN109433169 B CN 109433169B CN 201811411304 A CN201811411304 A CN 201811411304A CN 109433169 B CN109433169 B CN 109433169B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/282—Porous sorbents
- B01J20/285—Porous sorbents based on polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/265—Adsorption chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
- B01D15/426—Specific type of solvent
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3425—Regenerating or reactivating of sorbents or filter aids comprising organic materials
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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Abstract
The invention discloses a method for improving the separating capacity of old calcium type chromatographic resin, which comprises the following steps: (1) water top resin; (2) and resin regeneration: soaking the resin in calcium chloride solution for a certain time; (3) backwashing the resin; (4) detecting the calcium type rate; (5) resin transfer; (6) and the resin is used: during normal production, a calcium chloride solution is prepared and added into the chromatographic system. The invention also discloses a device for improving the separating capacity of the old calcium type chromatographic resin. The method can effectively improve the separation capability of the old calcium type chromatographic resin by combining soaking and online calcium ion addition. The invention also discloses an improvement device for improving the separation capacity of the old calcium type chromatographic resin by using the improvement method. The invention has more continuous regeneration, more thorough regeneration and longer effect duration, can effectively reduce the one-time regeneration times, ensures continuous and stable operation of production and can be applied industrially.
Description
Technical Field
The invention relates to the technical field of resin regeneration, in particular to a method and a device for improving the separating capacity of old calcium type chromatographic resin.
Background
The chromatographic column built-in resin is calcium type macroporous adsorption resin, and is a material with porous characteristic combining the adsorption and screening principles. The separation of the resin gradually decreases with the increase of the service life. At present, the regeneration of the calcium type chromatographic separation resin mainly comprises the steps of washing the resin with water, soaking the resin with hydrochloric acid, washing the resin with pure water, soaking the resin with a calcium salt solution, and finally washing the resin with the pure water so as to improve the separation capacity of the resin. Patent publication No. CN102247900A discloses a regeneration method of calcium-type chromatographic separation resin, which utilizes hydrochloric acid desalination, calcium salt regeneration, and pH detection to control the regeneration end point. This method has the following problems: firstly, the regeneration is carried out on the disposable calcium salt, the regeneration cannot be carried out continuously, protein and lipid substances which are not completely removed remain in the materials, the separation capacity of the resin is continuously influenced, and the effect duration time for improving the separation capacity of the resin is short; and secondly, the method is only suitable for improving the separation capacity of the chromatographic resin in a small experimental stage and cannot be applied to industrial production.
Disclosure of Invention
The invention aims to provide a method and a device for improving the separating capacity of old calcium type chromatographic resin, which aim to solve the problems of discontinuous resin regeneration, incomplete regeneration, short effect duration, incapability of industrialized application and the like in the prior art.
The invention adopts the following technical scheme:
a method for improving the separating capacity of an old calcium-type chromatographic resin comprises the following steps:
(1) water top resins
Ejecting the old resin in the chromatographic column to a resin backwashing tower through hot pure water, and draining water;
(2) regeneration of resin
Preparing a calcium chloride solution by using hot pure water, adding the calcium chloride solution into the backwashing tower for draining water in the step (1), soaking the resin in the calcium chloride solution for a certain time, replacing other ions adsorbed on the functional groups by soaking the resin in high-concentration calcium ions to complete resin regeneration, and then discharging the soaking solution to a sewage station;
(3) resin backwash
Backwashing the regenerated resin by using hot pure water to remove redundant calcium chloride, broken resin and partial insoluble protein until the content of calcium ions in the cleaning solution is 0 and the cleaning solution is clear;
(4) calcium type rate detection
Performing resin calcium type rate detection on the resin in the step (3), wherein the resin is qualified when reaching the standard, and the steps (2) to (3) are repeated when the resin is unqualified;
(5) resin transfer
Transferring the qualified chromatographic resin in the step (4) to a chromatographic column;
(6) and use of the resin
Putting the chromatographic column in the step (5) into use, and during normal production, preparing a calcium chloride solution and adding the calcium chloride solution into a chromatographic system: when the resin is used for the first time, the resin is added into eluent by a metering pump, so that the calcium ions of the eluent reach a certain concentration, and the regenerated resin is maintained on line to prevent the calcium ions on the functional groups from being replaced; the calcium ion content of the eluent which is recycled is detected before use, and the calcium ion is supplemented by a metering pump to maintain the concentration at the concentration.
Further, the hot pure water in the steps (1), (2) and (3) is hot pure water with the temperature of 75 +/-2 ℃.
Further, the concentration of the calcium chloride solution in the step (2) is 6 +/-1 wt%.
Further, the step (2) utilizes compressed air for back blowing to ensure that all the resin is soaked in the solution.
Further, the resin in the step (2) is soaked in calcium chloride solution for 24-48 hours.
Furthermore, the qualified standard of the step (4) is that the resin calcium type rate is more than 90%.
Further, the concentration of the calcium chloride solution in the step (6) is 0.1 +/-0.01 wt%.
Further, the calcium ion concentration of the eluent in the step (6) reaches 2-50 ppm.
An improvement device for improving the separation capacity of old calcium type chromatographic resin by utilizing the improvement method for the separation capacity of old calcium type chromatographic resin comprises a calcium preparation barrel and a metering pump, wherein the calcium preparation barrel is connected with a chromatographic eluent tank through the metering pump; the calcium preparation barrel is used for preparing a calcium chloride solution, and the calcium chloride solution is added into the eluent in the chromatographic eluent tank through the metering pump, so that calcium ions in the eluent reach a certain concentration, and the regenerated resin is maintained on line.
Further, the calcium preparation barrel is provided with a stirring motor.
The invention has the beneficial effects that:
the method can effectively improve the separation capability of the old calcium type chromatographic resin by combining soaking and online calcium ion addition, and can obviously improve the content of maltitol in a chromatographic extracting solution and greatly reduce the content of maltitol in a raffinate (mainly polyol and sorbitol) if the method is applied to the production of maltitol. Compared with the prior art, the regeneration method has the advantages of more continuous regeneration, more thorough regeneration and longer effect duration, can effectively reduce the frequency of one-time regeneration, ensures continuous and stable operation of production, can be industrially applied, and can generate direct economic benefit of 50 ten thousand yuan/year when being applied to the production of maltitol and producing 1 ten thousand tons of crystal maltitol.
Drawings
FIG. 1 shows the change in the maltitol content of the extract of example 1.
FIG. 2 shows the variation of maltitol content in the polyol component of example 1.
FIG. 3 is a graph showing the variation of the maltitol content in the sorbitol component of example 1.
FIG. 4 is a schematic view showing the structure of an apparatus for improving the separating ability of an old calcium-type chromatography resin.
Detailed Description
The invention is explained in more detail below with reference to exemplary embodiments and the accompanying drawings. The following examples are provided only for illustrating the present invention and are not intended to limit the scope of the present invention.
A method for improving the separating capacity of an old calcium-type chromatographic resin comprises the following steps:
(1) water top resins
Ejecting old resin in a chromatographic column into a resin backwashing tower through hot pure water at 75 +/-2 ℃, and draining the water to prevent regenerated liquid from being diluted or mixed unevenly to influence the regeneration effect;
(2) regeneration of resin
Preparing a 6 +/-1 wt% calcium chloride solution by using hot pure water at 75 +/-2 ℃, adding the calcium chloride solution into the backwashing tower for draining water in the step (1), carrying out reverse blowing by using compressed air, soaking all resins in the calcium chloride solution for 24-48 hours, replacing other ions adsorbed on functional groups by soaking with high-concentration calcium ions to complete resin regeneration, and then discharging a soaking solution to a sewage station;
(3) resin backwash
Backwashing the regenerated resin by using hot pure water at 75 +/-2 ℃ to remove redundant calcium chloride, crushed resin and partial insoluble protein until the content of calcium ions in the cleaning solution is 0 and the cleaning solution is clear;
(4) calcium type rate detection
Performing resin calcium type rate detection on the resin in the step (3), wherein the resin is qualified when the resin reaches more than 90% (the calcium type rate is 90% which is a more economic critical value), and repeating the steps (2) to (3) if the resin is unqualified;
(5) resin transfer
Transferring the qualified chromatographic resin in the step (4) to a chromatographic column;
(6) and use of the resin
Putting the chromatographic column of the step (5) into use; because the crosslinking degree of the used resin is reduced, calcium ions on functional groups of the regenerated resin are easily replaced by other ions again in the running process, so that the separation capability is reduced, and therefore, in normal production, 0.1 +/-0.01 wt% calcium chloride solution (avoiding introducing other anions) is prepared and added into a chromatographic system: when the resin is used for the first time, the resin is added into eluent by a metering pump, so that the calcium ion of the eluent reaches 2-50ppm, and the regenerated resin is maintained on line to prevent the calcium ion on the functional group from being replaced; the recycled eluent is used for detecting the calcium ion content before use, and the calcium ion is supplemented by a metering pump to maintain the concentration of the eluent at 2-50 ppm.
An improvement device for improving the separation capacity of old calcium type chromatographic resin by utilizing the method for improving the separation capacity of old calcium type chromatographic resin as shown in the figure 4 comprises a calcium preparation barrel 1 and a metering pump 2, wherein the calcium preparation barrel 1 is connected with a chromatographic eluent tank 3 through the metering pump 2; the calcium preparation barrel 1 is used for preparing calcium chloride solution, calcium chloride raw materials enter the calcium preparation barrel 1 through the dosing port 4, the calcium chloride raw materials are uniformly stirred through the stirring motor 5, eluent is added into the chromatographic eluent tank 3 through the metering pump 2, calcium ions in the eluent reach certain concentration, and the eluent enters the chromatographic column 6, so that the aim of maintaining regenerated resin on line is fulfilled.
Example 1
(1) Water top resins
A set of old chromatographic system (total 8 chromatographic columns) with the calcium type rate of 82% is tested (the calcium type rate of new resin is more than or equal to 95%), the resin in the chromatographic 1# column is reversely jacked into a resin backwashing tower through hot pure water at 75 ℃, and the water is drained, so that the regeneration liquid is prevented from being diluted or unevenly mixed to influence the regeneration effect.
(2) Resin regeneration
Dissolving calcium chloride into 6wt% solution by using hot purified water at 75 ℃, adding the solution into a backwashing tower for draining water in the step (1), carrying out reverse blowing by using compressed air, soaking all resins in the calcium chloride solution for 24 hours, carrying out high-concentration calcium ion soaking to replace other ions adsorbed on functional groups, completing resin regeneration, and then discharging the soaking solution to a sewage station.
(3) Resin backwash
And (3) backwashing the regenerated resin by using hot pure water at 75 ℃ to remove redundant calcium chloride, broken resin and part of insoluble protein until the content of calcium ions in the cleaning solution is 0 and the cleaning solution is clear.
(4) Calcium type rate detection
And (4) detecting the calcium type rate of the resin in the step (3), wherein the calcium type rate is 92.3 percent and reaches more than 90 percent, and the resin is qualified.
(5) Resin transfer
Transferring the qualified chromatographic resin in the step (4) to a chromatographic column # 1, and repeating the steps (1) - (4) to complete the regeneration work of the remaining 7 chromatographic columns.
(6) Resin use (maltitol extraction)
Putting the chromatographic column in the step (5) into use, and separating the raw material with the maltitol content of 84 +/-0.5 percent and the refraction of 50 +/-2 percent by utilizing a chromatographic system in a workshop according to an operation specification. The feeding flow is 3.3 +/-0.1 m for carrying out the downward cultivation, the eluent flow is 9.0 +/-0.5 m for carrying out the downward cultivation, and the eluent temperature is 75 +/-2 ℃ (being beneficial to improving the separation effect). After stable operation for 2-3 cycles, 50ml of each fraction was collected, and the maltitol content of each fraction was measured by liquid chromatography.
As the crosslinking degree of the resin used is reduced, calcium ions on functional groups of the regenerated resin are easily replaced by other ions again during the operation process, so that the separation capability is reduced. Thus, in normal production, a calcium chloride solution is prepared at a concentration of 0.1 ± 0.01wt% (avoiding the introduction of other anions) and added to the chromatographic system: when the resin is used for the first time, the resin is added into eluent by a metering pump, so that the calcium ion concentration of the eluent reaches 2-50ppm, and the regenerated resin is maintained on line to prevent the calcium ions on the functional groups from being replaced; the eluent is recycled and enters an eluent tank for recycling through membrane concentration, the calcium ion content is detected before use, and the calcium ion is supplemented through a metering pump to maintain the concentration of the calcium ion at 2-50 ppm.
(7) Detection of
Collecting chromatographic operation data of 8 months before and after calcium supplement, drawing a trend graph, and evaluating the calcium supplement effect.
(8) Evaluation of
The chromatographic resin starts to normally run, and calcium ions are gradually exposed and replaced by other ions in the material along with the aging of the resin, the reduction of the crosslinking degree and the loosening of functional groups, so that the separation capacity of the chromatographic resin is reduced, the yield of maltitol in an extracting solution is reduced, and the content of maltitol in a raffinate is improved;
in month 2, the content of maltitol in the extract gradually decreased from 89.9% to 89.0%, and the content of maltitol in the raffinate sorbitol increased from 43.4% to 51.0%;
in the 3 rd month, the soaking and the online addition of calcium ions are started, so that the calcium ions in the chromatographic resin are supplemented, and the calcium ions on the functional groups are prevented from being replaced, so that the separation capacity of the resin is continuously recovered and improved, the content of maltitol in the extracting solution is improved, and the content of maltitol in the raffinate is reduced;
at month 6, the yield of maltitol in the extracting solution is continuously improved to 89.9 percent and gradually increased to 91.7 percent, the content of maltitol in the raffinate polyol is gradually reduced to 27.5 percent from 41.2 percent, and the content of maltitol in the raffinate sorbitol is gradually reduced to 39.3 percent from 43.4 percent;
after 6 months, the maltitol content of the extract and of the raffinate was substantially smooth.
Claims (3)
1. An application of old calcium type chromatographic resin with improved separation capacity for extracting maltitol is characterized in that the method for improving the separation capacity of the old calcium type chromatographic resin is as follows:
(1) water top resins
Ejecting the old resin in the chromatographic column to a resin backwashing tower through hot pure water, and draining water;
(2) regeneration of resin
Preparing a calcium chloride solution by using hot pure water, adding the calcium chloride solution into the backwashing tower for draining water in the step (1), soaking the resin in the calcium chloride solution for a certain time, replacing other ions adsorbed on the functional groups by soaking the resin in high-concentration calcium ions to complete resin regeneration, and then discharging the soaking solution to a sewage station; the concentration of the calcium chloride solution is 6 +/-1 wt%, and the resin is soaked in the calcium chloride solution for 24-48 hours;
(3) resin backwash
Backwashing the regenerated resin by using hot pure water to remove redundant calcium chloride, broken resin and partial insoluble protein until the content of calcium ions in the cleaning solution is 0 and the cleaning solution is clear;
(4) calcium type rate detection
Performing resin calcium type rate detection on the resin in the step (3), wherein the resin is qualified when reaching the standard, and the steps (2) to (3) are repeated when the resin is unqualified; the qualified standard is that the resin calcium type rate is more than 90%;
(5) resin transfer
Transferring the qualified chromatographic resin in the step (4) to a chromatographic column;
(6) and use of the resin
Putting the chromatographic column in the step (5) into use, and during normal production, preparing a calcium chloride solution and adding the calcium chloride solution into a chromatographic system: when the resin is used for the first time, the resin is added into eluent by a metering pump, so that the calcium ions of the eluent reach a certain concentration, and the regenerated resin is maintained on line to prevent the calcium ions on the functional groups from being replaced; the calcium ion content of the eluent which is recycled is detected before use, and the calcium ion is supplemented by a metering pump to maintain the concentration of the eluent at the above concentration; the concentration of the prepared calcium chloride solution is 0.1 +/-0.01 wt%, and the calcium ion concentration of the eluent reaches 2-50 ppm.
2. Use of the old calcium-based chromatography resin with improved separation ability for maltitol extraction according to claim 1, wherein the hot purified water of steps (1), (2) and (3) is 75 ± 2 ℃.
3. The use of the old calcium-based chromatography resin with improved separation ability for maltitol extraction according to claim 1, wherein the step (2) uses compressed air blowback to ensure that all resins are immersed in the solution.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247900A (en) * | 2011-07-25 | 2011-11-23 | 山东福田药业有限公司 | Process for regenerating calcium type chromatographic separation resin |
| CN102989529A (en) * | 2012-11-28 | 2013-03-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for on-line recovery of ion exchange resin |
| CN204170734U (en) * | 2014-02-21 | 2015-02-25 | 攀钢集团攀枝花钢铁研究院有限公司 | The device that a kind of ion exchange resin is recovered online |
| CN105126937A (en) * | 2015-08-14 | 2015-12-09 | 芜湖融汇化工有限公司 | Chelate resin tower regeneration prolongation process method |
| CN207760087U (en) * | 2017-11-23 | 2018-08-24 | 成都市排水有限责任公司 | Wet method soft water dosing system |
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| US7399725B2 (en) * | 2004-04-23 | 2008-07-15 | Applied Intellectual Capital | Perchlorate destruction |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102247900A (en) * | 2011-07-25 | 2011-11-23 | 山东福田药业有限公司 | Process for regenerating calcium type chromatographic separation resin |
| CN102989529A (en) * | 2012-11-28 | 2013-03-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for on-line recovery of ion exchange resin |
| CN204170734U (en) * | 2014-02-21 | 2015-02-25 | 攀钢集团攀枝花钢铁研究院有限公司 | The device that a kind of ion exchange resin is recovered online |
| CN105126937A (en) * | 2015-08-14 | 2015-12-09 | 芜湖融汇化工有限公司 | Chelate resin tower regeneration prolongation process method |
| CN207760087U (en) * | 2017-11-23 | 2018-08-24 | 成都市排水有限责任公司 | Wet method soft water dosing system |
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