CN109433169A - A kind of ameliorative way and device of old calcium type chromatography resin separating capacity - Google Patents
A kind of ameliorative way and device of old calcium type chromatography resin separating capacity Download PDFInfo
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- CN109433169A CN109433169A CN201811411304.1A CN201811411304A CN109433169A CN 109433169 A CN109433169 A CN 109433169A CN 201811411304 A CN201811411304 A CN 201811411304A CN 109433169 A CN109433169 A CN 109433169A
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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
- B01J20/281—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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- 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
- B01J20/3425—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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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention discloses a kind of ameliorative way of old calcium type chromatography resin separating capacity, includes the following steps: (1), water top resin；(2), resin regeneration: resin is immersed in certain time in calcium chloride solution；(3), resin backwash；(4), calcium type rate detects；(5), resin shifts；(6), resin uses: during normal production, preparing calcium chloride solution and is added in chromatographic system.The invention also discloses a kind of improvement devices of old calcium type chromatography resin separating capacity.The present invention can effectively improve the separating capacity of old calcium type chromatography resin by impregnating the online addition calcium ion of joint.Invention additionally discloses a kind of improvement devices that old calcium type chromatography resin separating capacity is improved using the ameliorative way.Present invention regeneration is more continuous, regeneration is more thorough, effect duration is longer, can efficiently reduce disposable regenerated number, guarantee the operation of production continuous-stable, can be with industrial application.
Description
Technical field
The present invention relates to resin regeneration technical fields, and in particular to a kind of improvement side of old calcium type chromatography resin separating capacity
Method and device.
Background technique
Resin built in chromatographic column is calcium type macroporous absorbent resin, a kind of to combine with adsorptivity and screening property principle
The material of porosity characteristic.With the extension of service life, the centrifugation of resin can gradually weaken.Calcium type chromatographic isolation resin is again
Life is presently mainly first rinsed with water resin, then uses salt acid soak, is impregnated with calcium salt soln with after pure water rinsing, finally used again
Pure water rinsing, to improve the separating capacity of resin.The patent of Publication No. CN102247900A discloses a kind of calcium type chromatography point
Regeneration method from resin, this method utilize hydrochloric acid desalination, calcium salt regeneration, pH detection control regeneration terminal.This method exist with
Lower problem: first is that regenerating for disposable calcium salt, being unable to cyclic regeneration, un-cleared albumen and lipid matter remained in material, after
The continuous separating capacity for influencing resin, the effect duration for improving resin separating capacity are short；Second is that being only applicable to small test rank
The improvement of the chromatography resin separating capacity of section, may not apply to industrialization production.
Summary of the invention
The object of the present invention is to provide the ameliorative ways and device of a kind of old calcium type chromatography resin separating capacity, existing to solve
Have in technology that resin regeneration is discontinuous, regeneration is not thorough, effect duration is short, is unable to the problems such as industrial application.
The invention adopts the following technical scheme:
A kind of ameliorative way of old calcium type chromatography resin separating capacity, includes the following steps:
(1), water top resin
Old resin in chromatographic column is pushed up by the way that hot pure water is counter into resin backwashing tower, and water is drained；
(2), resin regeneration
Calcium chloride solution is prepared with hot pure water, is added in the backwashing tower of step (1) emptied of water, resin is immersed in calcium chloride solution
Middle certain time, is impregnated by high concentration calcium ion, the other ions adsorbed on permutation function group, completes resin regeneration, it
Soak is drained into sewage plant afterwards；
(3), resin backwash
Backwash is carried out to the resin after regeneration with hot pure water, removes extra calcium chloride, shredded resin and part insoluble protein,
Into cleaning solution, calcium ion content is 0 and cleaning solution is clarified；
(4), calcium type rate detects
The detection of resin calcium type rate is carried out to the resin in step (3), reaching standard is qualification, unqualified to repeat step (2) extremely
(3)；
(5), resin shifts
Chromatography resin qualified in step (4) is transferred to chromatographic column；
(6), resin uses
The chromatographic column of step (5) is come into operation, during normal production, calcium chloride solution is prepared and is added in chromatographic system: is first
In use, being added in eluent by metering pump, the calcium ion of eluent is made to reach a certain concentration, the resin after regeneration is carried out
On-line maintenance prevents the calcium ion on functional group to be replaced；The eluent of recycling is contained using preceding its calcium ion of detection
Amount, supplementing calcium ion by metering pump makes its concentration maintain above-mentioned concentration.
Further, step (1), (2), the hot pure water that (3) hot pure water is 75 ± 2 DEG C.
Further, step (2) calcium chloride solution concentration is 6 ± 1wt%.
Further, step (2) utilizes compressed air blowback, guarantees that all resins impregnate in the solution.
Further, step (2) resin is immersed in calcium chloride solution 24-48 hours.
Further, step (4) criterion of acceptability is 90% or more resin calcium type rate.
Further, step (6) calcium chloride solution concentration is 0.1 ± 0.01wt%.
Further, the calcium ion concentration of step (6) eluent reaches 2-50ppm.
A kind of old calcium type chromatography resin of ameliorative way raising using foregoing old calcium type chromatography resin separating capacity
The improvement device of separating capacity, including match calcium bucket, metering pump, it is connected by metering pump with chromatography eluant flow container with calcium bucket；With calcium
Bucket is added to the eluent in chromatography eluant flow container by metering pump for preparing calcium chloride solution, make calcium in eluent from
Son reaches a certain concentration, carries out on-line maintenance to the resin after regeneration.
Further, stirring motor is equipped with calcium bucket.
Beneficial effects of the present invention:
The present invention can effectively improve the separating capacity of old calcium type chromatography resin, such as by impregnating the online addition calcium ion of joint
It applies in the production of maltitol, the content of maltitol in chromatography extracting solution can be obviously improved, it is (main that raffinate is greatly reduced
To be polyalcohol and sorbierite) in maltitol content.Compared with the prior art, present invention regeneration is more continuous, regeneration is more thorough
Bottom, effect duration are longer, can efficiently reduce disposable regenerated number, guarantee the operation of production continuous-stable, can be with
Industrial application, as being applied in the production of maltitol, 10,000 tons of crystal maltose alcohols of every production can produce direct economy
500,000 yuan/year of benefit.
Detailed description of the invention
Fig. 1 is maltitol content variation in 1 extracting solution of embodiment.
Fig. 2 is maltitol content variation in 1 polyol component of embodiment.
Fig. 3 is maltitol content variation in 1 sorb alkoxide component of embodiment.
Fig. 4 is the structural schematic diagram of the improvement device of old calcium type chromatography resin separating capacity.
Specific embodiment
The present invention is done below with reference to embodiment and attached drawing and is further explained.The following example is merely to illustrate this hair
It is bright, but be not used to limit practical range of the invention.
A kind of ameliorative way of old calcium type chromatography resin separating capacity, includes the following steps:
(1), water top resin
Old resin in chromatographic column is pushed up by the way that 75 ± 2 DEG C of hot pure waters are counter into resin backwashing tower, and water is drained, prevents from regenerating
Liquid is diluted or mixes unevenly, influences regeneration effect；
(2), resin regeneration
6 ± 1wt% calcium chloride solution is prepared with 75 ± 2 DEG C of hot pure waters, is added in the backwashing tower of step (1) emptied of water, utilizes pressure
All resins are immersed in calcium chloride solution 24-48 hours, are impregnated by high concentration calcium ion by contracting air blowback, replace function
The other ions adsorbed on energy group, complete resin regeneration, soak are drained into sewage plant later；
(3), resin backwash
Backwash is carried out to the resin after regeneration with 75 ± 2 DEG C of hot pure waters, it is insoluble to remove extra calcium chloride, shredded resin and part
Property albumen, until in cleaning solution calcium ion content be 0 and cleaning solution clarify；
(4), calcium type rate detects
The detection of resin calcium type rate is carried out to the resin in step (3), reaching 90%(calcium type rate 90% is both economical one critical
Value) more than be qualification, it is unqualified repeat step (2) to (3)；
(5), resin shifts
Chromatography resin qualified in step (4) is transferred to chromatographic column；
(6), resin uses
The chromatographic column of step (5) is come into operation；Due to the resin's crosslinkage decline used, the resin after regeneration is in operational process
Calcium ion on middle functional group is easy to be replaced by other ions again, causes separating capacity to decline, therefore during normal production, match
System 0.1 ± 0.01wt% calcium chloride solution (avoiding being introduced into other anion) is added in chromatographic system: when first used, being passed through
Metering pump is added in eluent, and the calcium ion of eluent is made to reach 2-50ppm, carries out on-line maintenance to the resin after regeneration, prevents
Only the calcium ion on functional group is replaced；The eluent of recycling passes through metering pump using preceding its calcium ion content of detection
Supplement calcium ion makes its concentration maintain 2-50ppm.
A kind of old calcium type chromatography resin of ameliorative way raising using foregoing old calcium type chromatography resin separating capacity
The improvement device of separating capacity passes through metering pump 2 and chromatography eluant with calcium bucket 1 as shown in figure 4, including matching calcium bucket 1, metering pump 2
Flow container 3 connects；It is entered by ingredients mouth 4 with calcium bucket 1, by stirring with calcium bucket 1 for preparing calcium chloride solution, calcium chloride raw material
It mixes motor 5 to stir evenly, eluent passes through metering pump 2 again and is added in chromatography eluant flow container 3, reaches the calcium ion in eluent
To a certain concentration, eluent enters chromatographic column 6, to achieve the purpose that carry out on-line maintenance to the resin after regeneration.
Embodiment 1
(1) water top resin
The old chromatographic system (totally 8 chromatographic columns) for being 82% to a set of calcium type rate is tested (new resin calcium type rate is >=95%),
Resin in chromatography 1# column is pushed up by the way that 75 DEG C of hot pure waters are counter into resin backwashing tower, and water is drained, prevents regenerated liquid dilute
It releases or mixes unevenly, influence regeneration effect.
(2) resin regeneration
Calcium chloride is dissolved into the solution of 6wt% with 75 DEG C of hot purified waters, is added in the backwashing tower of step (1) emptied of water, is utilized
All resins are immersed in calcium chloride solution 24 hours, are impregnated by high concentration calcium ion, permutation function by compressed air blowback
The other ions adsorbed on group complete resin regeneration, soak are drained into sewage plant later.
(3) resin backwash
Backwash is carried out to the resin after regeneration with 75 DEG C of hot pure waters, it is insoluble to remove extra calcium chloride, shredded resin and part
Albumen, until calcium ion content is 0 in cleaning solution and cleaning solution is clarified.
(4) calcium type rate detects
The detection of resin calcium type rate is carried out to the resin in step (3), is 92.3%, reaches 90% or more, for qualified resin.
(5) resin shifts
Chromatography resin qualified in step (4) is transferred to chromatography 1# column, and repeats step (1)-(4) and completes remaining 7 chromatography
The reproduction operation of column.
(6) resin uses (maltitol extraction)
The chromatographic column of step (5) is come into operation, using the chromatographic system in workshop, according to working specification, to maltitol content
It is 84 ± 0.5%, the raw material that refractive power is 50 ± 2% is separated.Feed rate be 3.3 ± 0.1m3/h, elution flow quantity 9.0 ±
0.5m3/h, 75 ± 2 DEG C of Eluant temperature (are conducive to improve separating effect).After the 2-3 period of stable operation, each separation group is collected
Divide 50ml, with maltitol content in liquid chromatographic detection each component.
Due to the resin's crosslinkage decline used, the calcium ion of resin after regeneration in the process of running on functional group holds
It is easily replaced again by other ions, separating capacity is caused to decline.Therefore during normal production, compound concentration is 0.1 ± 0.01wt%'s
Calcium chloride solution (avoids introducing other anion), is added in chromatographic system: when first used, being added and is eluted by metering pump
In liquid, the calcium ion concentration of eluent is made to reach 2-50ppm, on-line maintenance is carried out to the resin after regeneration, prevents functional group
On calcium ion be replaced；Eluent enters elution flow container by film concentration and recovery and is recycled, and uses preceding its calcium ion of detection
Content, supplementing calcium ion by metering pump makes its concentration maintain 2-50ppm.
(7) it detects
The 8 months chromatographic run data in front and back of replenishing the calcium are collected, tendency chart is drawn, assess effect of supplemented calcium.
(8) it assesses
Chromatography resin starts to operate normally, with the aging of resin, the degree of cross linking decline, functional group loosen, cause calcium ion by
It is gradually exposed, maltitol in extracting solution is reduced so that chromatography resin separating capacity reduces by other ion exchanges in material
Yield, improve the content of maltitol in raffinate；
2nd month, the content of maltitol was gradually lowered to 89.0% by 89.9% in extracting solution, the malt in raffinate sorbierite
The content of sugar alcohol increases to 51.0% by 43.4%；
3rd month, start to impregnate the online addition calcium ion of joint, the calcium ion in chromatography resin is supplemented, while preventing function
Calcium ion on energy group is replaced, so that the separating capacity of resin is constantly restored and improved, to improve wheat in extracting solution
The content of bud sugar alcohol reduces the content of maltitol in raffinate；
6th month, the yield of maltitol was continuously improved 89.9% and gradually increases to 91.7% in extracting solution, in raffinate polyalcohol
Maltitol content is gradually decreased to 27.5% by 41.2%, and the content 43.4% of the maltitol in raffinate sorbierite gradually decreases
To 39.3%；
After 6th month, the maltitol content in extracting solution and raffinate is substantially steady.
Claims (10)
1. a kind of ameliorative way of old calcium type chromatography resin separating capacity, which comprises the steps of:
(1), water top resin
Old resin in chromatographic column is pushed up by the way that hot pure water is counter into resin backwashing tower, and water is drained；
(2), resin regeneration
Calcium chloride solution is prepared with hot pure water, is added in the backwashing tower of step (1) emptied of water, resin is immersed in calcium chloride solution
Middle certain time, is impregnated by high concentration calcium ion, the other ions adsorbed on permutation function group, completes resin regeneration, it
Soak is drained into sewage plant afterwards；
(3), resin backwash
Backwash is carried out to the resin after regeneration with hot pure water, removes extra calcium chloride, shredded resin and part insoluble protein,
Into cleaning solution, calcium ion content is 0 and cleaning solution is clarified；
(4), calcium type rate detects
The detection of resin calcium type rate is carried out to the resin in step (3), reaching standard is qualification, unqualified to repeat step (2) extremely
(3)；
(5), resin shifts
Chromatography resin qualified in step (4) is transferred to chromatographic column；
(6), resin uses
The chromatographic column of step (5) is come into operation, during normal production, calcium chloride solution is prepared and is added in chromatographic system: is first
In use, being added in eluent by metering pump, the calcium ion of eluent is made to reach a certain concentration, the resin after regeneration is carried out
On-line maintenance prevents the calcium ion on functional group to be replaced；The eluent of recycling is contained using preceding its calcium ion of detection
Amount, supplementing calcium ion by metering pump makes its concentration maintain above-mentioned concentration.
2. the ameliorative way of old calcium type chromatography resin separating capacity according to claim 1, which is characterized in that step (1),
(2), the hot pure water that (3) hot pure water is 75 ± 2 DEG C.
3. the ameliorative way of old calcium type chromatography resin separating capacity according to claim 1, which is characterized in that step (2)
Calcium chloride solution concentration is 6 ± 1wt%.
4. the ameliorative way of old calcium type chromatography resin separating capacity according to claim 1, which is characterized in that step (2)
Using compressed air blowback, guarantee that all resins impregnate in the solution.
5. the ameliorative way of old calcium type chromatography resin separating capacity according to claim 1, which is characterized in that step (2)
Resin is immersed in calcium chloride solution 24-48 hours.
6. the ameliorative way of old calcium type chromatography resin separating capacity according to claim 1, which is characterized in that step (4)
Criterion of acceptability is 90% or more resin calcium type rate.
7. the ameliorative way of old calcium type chromatography resin separating capacity according to claim 1, which is characterized in that step (6)
Calcium chloride solution concentration is 0.1 ± 0.01wt%.
8. the ameliorative way of old calcium type chromatography resin separating capacity according to claim 1, which is characterized in that step (6)
The calcium ion concentration of eluent reaches 2-50ppm.
9. a kind of ameliorative way using old calcium type chromatography resin separating capacity as claimed in any of claims 1 to 8 in one of claims
Improve the improvement device of old calcium type chromatography resin separating capacity, which is characterized in that including matching calcium bucket, metering pump, pass through with calcium bucket
Metering pump is connected with chromatography eluant flow container；With calcium bucket for preparing calcium chloride solution, chromatographic eluents are added to by metering pump
Eluent in tank makes the calcium ion in eluent reach a certain concentration, carries out on-line maintenance to the resin after regeneration.
10. the improvement device of old calcium type chromatography resin separating capacity according to claim 9, which is characterized in that match calcium bucket
Equipped with stirring motor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811411304.1A CN109433169B (en) | 2018-11-24 | 2018-11-24 | Method and device for improving separating capacity of old calcium type chromatographic resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811411304.1A CN109433169B (en) | 2018-11-24 | 2018-11-24 | Method and device for improving separating capacity of old calcium type chromatographic resin |
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| CN109433169A true CN109433169A (en) | 2019-03-08 |
| CN109433169B CN109433169B (en) | 2022-03-04 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090008333A1 (en) * | 2004-04-23 | 2009-01-08 | Robert Lewis Clarke | Perchlorate Destruction |
| 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 |
-
2018
- 2018-11-24 CN CN201811411304.1A patent/CN109433169B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090008333A1 (en) * | 2004-04-23 | 2009-01-08 | Robert Lewis Clarke | Perchlorate Destruction |
| 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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| Publication number | Publication date |
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| CN109433169B (en) | 2022-03-04 |
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