CN107999149A - A kind of method for resuscitation and recovery medicament of the cation exchange resin of organic basifier pollution - Google Patents
A kind of method for resuscitation and recovery medicament of the cation exchange resin of organic basifier pollution Download PDFInfo
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- CN107999149A CN107999149A CN201711334038.2A CN201711334038A CN107999149A CN 107999149 A CN107999149 A CN 107999149A CN 201711334038 A CN201711334038 A CN 201711334038A CN 107999149 A CN107999149 A CN 107999149A
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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
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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
- B01J49/60—Cleaning or rinsing ion-exchange beds
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Abstract
The method for resuscitation and recovery medicament of the cation exchange resin of organic basifier pollution, it is related to the method for resuscitation and recovery medicament of the cation exchange resin of organic pollution, organic basifier is polluted the invention solves existing method for resuscitation more serious, substitute effective functional group inside cation exchange resin, when recovery elutes the problem of effect is bad and existing recovery reagent combination cannot increase cation exchange groups quantity.The method for resuscitation of the cation exchange resin of organic basifier pollution is implemented by the following steps in the present invention：First, the transition of positive resin；2nd, rinse；3rd, remove positive resin organic pollution and make its recovery；4th, rinse.Recovery medicament in the present invention used in the method for resuscitation of the cation exchange resin of organic pollution, is made of NaCl, NaOH, organic additive and water.
Description
Technical field
The present invention relates to the method for resuscitation and recovery medicament of a kind of cation exchange resin of basifier pollution.
Background technology
At present in the in-service nuclear power generating sets in China, the secondary circuit of most nuclear power generating sets is using full volatilization (AVT) water chemistry
Treatment technology, i.e., by adding ammonia (NH3) and diamine (N2H4) to control the pH value of secondary coolant circuit system and oxygen content respectively.But
Be ammonia gas-liquid distribution factor it is higher, most of ammonia are present in vapour phase during high temperature, and ammonia content is seriously relatively low in liquid phase, makes liquid phase
PH values are relatively low, easily cause the generation for flowing accelerated corrosion (FAC).
In order to reduce FAC, the U.S., France propose using the relatively low organic amine of gas-liquid partition coefficient (such as monoethanolamine,
Quinoline etc.) substitute technical solution of the ammonia as secondary circuit basifier.Domestic and international nuclear power station the actual running results show：Organic aqueous amine
Chemical technology can effectively slow down the flowing accelerated corrosion at the position such as secondary circuit draining system and biphase gas and liquid flow system, lower hydrophobic
Iron concentration in system (such as separator is hydrophobic), and then reduce migration of the iron ion into steam generator
And its deposition of oxide.The U.S. uses morpholine water condition since the eighties, starts the nineties in last century to use monoethanolamine
（ETA）Water condition, the later stage nineties use advanced amine such as aminoanisole（MPA）, dimethylamine（DMA）Deng organic amine as alkalization
Agent, the nuclear power station application ETA for having more than 60% in the world now replaces ammonia to adjust feedwater pH value, and also there is part nuclear power in the country
Station has carried out the trial operation of ETA operating modes.
Many power plant are required to use precision processing device of condensation water, and ion exchange resin generally is used for condensate polishing treatment
System.Precision processing system is eventually entered for the pH amine adjusted, is ion exchanged Resin Absorbent immediately.Although resin can be used
In system water purification, but its selection exchangeability for amine is not strong, regeneration or replacement Treatment is needed after efficiency lost resin, to maintain system
Normal operation.Foreign study found that the addition of secondary circuit basifier can shorten the secondary circuit condensate polishing treatment mixed bed cycle of operation,
Increase mixed bed regeneration times and soda acid consumption, and the power of regeneration for thering is certain probability to exceed resin, cause permanent failure.Resin streak
During ammonia, ion can be caused to reveal, and finally concentrated in a vapor generator, cause equipment damage.
It is different from general organic pollution negative resin, water-soluble preferable pollution of the basifier to cation exchange resin
Bigger.Studies have found that absorption of the cation exchange resin to basifier is more sensitive, and the pollution of anion exchange resin is
Due to caused by the pollution degraded of positive resin.Cation exchange resin can adsorb organic basifier in water inlet, and occur at the same time
The suction-operated of ion exchange and Van der Waals force, unhydrolysed small molecule organic amine Molecular Adsorption are hydrolyzed on resin matrix
Then with resin ion exchange occurs for the organic cation of positively charged afterwards, and two kinds of effects are carried out at the same time, and cause positive resin to pollute.Close
In remove the organic pollution of cation exchange resin the problem of, it is classical that the scientific and technical personnel in water treatment field have developed some
Method for resuscitation.It is more widely with traditional dynamic acid-alkali regeneration, the salting liquid of also useful higher concentration（Generally 10% or
Person is more）Organic matter in cation exchange resin is regenerated.The former method for resuscitation step is comparatively laborious, and cost compared with
High effect is simultaneously unstable.Elution effect of the latter to organic matter tends not to satisfactory.It is positive caused by this organic basifier
Resin stain passes through traditional renovation process, and regeneration degree is not high, and resin life shortens so that cost of water treatment rises.
The content of the invention
The present invention is to solve existing method for resuscitation to organic basifier to cation exchange resin the problem of, and provide
A kind of method for resuscitation and recovery medicament of the cation exchange resin of basifier pollution.
Wherein basifier can be monoethanolamine（ETA）, morpholine（MPH）, 3- METHOXY PROPYL AMINEs (MPA), dimethylamine
(DMA) or 5- aminopentanols (5-AP).
The method for resuscitation of the cation exchange resin of organic basifier pollution is through the following steps that realize in the present invention：
First, the transition of cation exchange resin：Cation exchange resin is circulated with the hydrochloric acid that mass fraction is 4% ~ 8%
Immersion, temperature are 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, is circulated using upper entering and lower leaving mode, when circulation immersion 6 ~ 10 is small
Afterwards, it is H-type by ion exchange resin conversion.
2nd, wash：After transition, waste liquid is exhausted, back flush is carried out to cation exchange resin with desalted water, is rinsed
Time is 1.5 ~ 2.5h, and irrigation flow rate is 18 ~ 22m/h.
3rd, organic solvent recovery lye rinses：The cumulative volume of recovery medicament is treat recovery cation exchange resin volume 4
Times.The percentage by weight composition of recovery medicament is respectively the organic additive of 8 ~ 15%NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%；During elution
Between control in the range of 6 ~ 12h.Resuscitation process temperature control is in the range of 36 ~ 42 DEG C, whole process recovery medicament rate of circulating flow
Control is in 3.5 ~ 4.5m/h.
4th, rinse：After elution, cation exchange resin rinses 20 ~ 32min with demineralized water, and flow control is in 8 ~ 12m/h
In the range of, pH is controlled 7.0 ~ 7.5.Resin is spare after the completion of flushing.
A kind of recovery reagent combination for removing cation exchange resin pollution in the present invention, by NaCl, NaOH, organic additive
Formed with water, the weight percent concentration in water of wherein NaCl, NaOH and organic additive are respectively 1 ~ 15%, 0.5 ~ 4% He
0.1~10%。
Organic additive is ethanol, isopropanol, glycerine, sulfonic acid or benzene sulfonic acid.
Beneficial effects of the present invention：
1st, by NaCl, NaOH and organic additive solution composition in recovery medicament, compared with conventional method, resuscitation fluid is inside resin
Ion exchange and unpolarizing occurs at the same time, the organic matter cation exchange that ion exchange occurs, which is got off, to enter carries machine aided
Agent solution.Meanwhile resin, when changing into Na types by H-type, volume expands, can be by organic basifier small molecule inside resin
Wash out, be more advantageous to the elution of organic matter.It is easy to operate, save the time.
2nd, degree of percent regeneration of resin is high, can preferably recover the operating capacity of resin, reduces the environment that waste resin is brought
Pollution, while the utilization rate of resin is improved, without regenerating transition after the completion of recovery, reduce cost.
Embodiment
With reference to embodiments, the present invention will be further described.
Embodiment 1：
732 strong-acid cation-exchange resins that 60ml is transformed into Na types are put into ion exchange column, are 0.2g/L's with concentration
Monoethanolamine（ETA）Solution carries out circulation immersion by resin, and coutroi velocity is 1.5 ~ 3.2 m/h, and temperature is 18 ~ 25 DEG C, pollution
2h.Then desalination water rinse resin is used, temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, is followed using upper entering and lower leaving mode
Ring.Pollution resin is recovered according to the following steps：First, the transition of cation exchange resin：With the salt that mass fraction is 4% ~ 8%
Acid carries out cation exchange resin circulation immersion, and temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, under enterprising
Go out mode to circulate, when circulation immersion 6 ~ 10 is small after, be H-type by ion exchange resin conversion.2nd, wash：After transition, waste liquid is exhausted, is used
Demineralized water carries out back flush to cation exchange resin, and washing time is 1.5 ~ 2.5h, and irrigation flow rate is 18 ~ 22m/h.3rd,
Organic solvent recovery lye rinses：The cumulative volume of recovery medicament is treat recovery cation exchange resin volume 4 times.Analeptic
The percentage by weight composition of agent is respectively the organic additive of 8 ~ 15%NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%；Elution time control 6 ~
In the range of 12h.Resuscitation process temperature control in the range of 36 ~ 42 DEG C, the control of whole process recovery medicament rate of circulating flow 3.5 ~
4.5m/h.4th, rinse：After elution, cation exchange resin rinses 20 ~ 32min with demineralized water, and flow control is in 8 ~ 12m/h models
In enclosing, pH is controlled 7.0 ~ 7.5.Resin industry and traffic is measured after the completion of flushing, acquired results insert table 1.
Embodiment 2：
732 strong-acid cation-exchange resins that 60ml is transformed into Na types are put into ion exchange column, are 0.2g/L's with concentration
Dimethylamine（DMA）Solution carries out circulation immersion by resin, and coutroi velocity is 1.5 ~ 3.2 m/h, and temperature is 18 ~ 25 DEG C, pollution
2h.Then desalination water rinse resin is used, temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, is followed using upper entering and lower leaving mode
Ring.Pollution resin is recovered according to the following steps：First, the transition of cation exchange resin：With the salt that mass fraction is 4% ~ 8%
Acid carries out cation exchange resin circulation immersion, and temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, under enterprising
Go out mode to circulate, when circulation immersion 6 ~ 10 is small after, be H-type by ion exchange resin conversion.2nd, wash：After transition, waste liquid is exhausted, is used
Demineralized water carries out back flush to cation exchange resin, and washing time is 1.5 ~ 2.5h, and irrigation flow rate is 18 ~ 22m/h.3rd,
Organic solvent recovery lye rinses：The cumulative volume of recovery medicament is treat recovery cation exchange resin volume 4 times.Analeptic
The percentage by weight composition of agent is respectively the organic additive of 8 ~ 15%NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%；Elution time is controlled 6
In the range of ~ 12h.In the range of 36 ~ 42 DEG C, whole process recovery medicament rate of circulating flow is controlled 3.5 resuscitation process temperature control
~4.5m/h.4th, rinse：After elution, cation exchange resin rinses 20 ~ 32min with demineralized water, and flow control is in 8 ~ 12m/h
In the range of, pH is controlled 7.0 ~ 7.5.Resin industry and traffic is measured after the completion of flushing, acquired results insert table 1.
Embodiment 3：
732 strong-acid cation-exchange resins that 60ml is transformed into Na types are put into ion exchange column, are 0.2g/L's with concentration
3- METHOXY PROPYL AMINEs (MPA) solution carries out circulation immersion by resin, and coutroi velocity be 1.5 ~ 3.2 m/h, and temperature is 18 ~
25 DEG C, pollute 2h.Then desalination water rinse resin is used, temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, and use is enterprising
Under go out mode and circulate.Pollution resin is recovered according to the following steps：First, the transition of cation exchange resin：It is with mass fraction
4% ~ 8% hydrochloric acid carries out cation exchange resin circulation immersion, and temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h,
Circulated using upper entering and lower leaving mode, when circulation immersion 6 ~ 10 is small after, be H-type by ion exchange resin conversion.2nd, wash：After transition, row
Fall waste liquid, back flush carried out to cation exchange resin with demineralized water, washing time is 1.5 ~ 2.5h, irrigation flow rate for 18 ~
22m/h.3rd, organic solvent recovery lye rinses：The cumulative volume of recovery medicament is treat recovery cation exchange resin volume 4
Times.The percentage by weight composition of recovery medicament is respectively the organic additive of 8 ~ 15%NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%；During elution
Between control in the range of 6 ~ 12h.Resuscitation process temperature control is in the range of 36 ~ 42 DEG C, whole process recovery medicament rate of circulating flow
Control is in 3.5 ~ 4.5m/h.4th, rinse：After elution, cation exchange resin rinses 20 ~ 32min with demineralized water, and flow control exists
In the range of 8 ~ 12m/h, pH is controlled 7.0 ~ 7.5.Resin industry and traffic is measured after the completion of flushing, acquired results insert table 1.
Embodiment 4：
732 strong-acid cation-exchange resins that 60ml is transformed into Na types are put into ion exchange column, are 0.2g/L's with concentration
Morpholine（MPH）Solution carries out circulation immersion by resin, and coutroi velocity is 1.5 ~ 3.2 m/h, and temperature is 18 ~ 25 DEG C, pollutes 2h.
Then desalination water rinse resin is used, temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, is circulated using upper entering and lower leaving mode.
Pollution resin is recovered according to the following steps：First, the transition of cation exchange resin：With the hydrochloric acid pair that mass fraction is 4% ~ 8%
Cation exchange resin carries out circulation immersion, and temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, using upper entering and lower leaving side
Formula circulate, when circulation immersion 6 ~ 10 is small after, be H-type by ion exchange resin conversion.2nd, wash：After transition, waste liquid is exhausted, uses desalination
Water carries out back flush to cation exchange resin, and washing time is 1.5 ~ 2.5h, and irrigation flow rate is 18 ~ 22m/h.3rd, it is organic
Solvent recovery lye rinses：The cumulative volume of recovery medicament is treat recovery cation exchange resin volume 4 times.Recovery medicament
Percentage by weight composition is respectively the organic additive of 8 ~ 15%NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%；Elution time is controlled in 6 ~ 12h
In the range of.Resuscitation process temperature control in the range of 36 ~ 42 DEG C, the control of whole process recovery medicament rate of circulating flow 3.5 ~
4.5m/h.4th, rinse：After elution, cation exchange resin rinses 20 ~ 32min with demineralized water, and flow control is in 8 ~ 12m/h models
In enclosing, pH is controlled 7.0 ~ 7.5.Resin industry and traffic is measured after the completion of flushing, acquired results insert table 1.
Embodiment 5：
732 strong-acid cation-exchange resins that 60ml is transformed into Na types are put into ion exchange column, are 0.2g/L's with concentration
5- aminopentanols (5-AP) solution carries out circulation immersion by resin, and coutroi velocity is 1.5 ~ 3.2 m/h, and temperature is 18 ~ 25
DEG C, pollute 2h.Then desalination water rinse resin is used, temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, under enterprising
Go out mode to circulate.Pollution resin is recovered according to the following steps：First, the transition of cation exchange resin：With mass fraction for 4% ~
8% hydrochloric acid carries out cation exchange resin circulation immersion, and temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, is used
Upper entering and lower leaving mode circulates, when circulation immersion 6 ~ 10 is small after, be H-type by ion exchange resin conversion.2nd, wash：After transition, exhaust useless
Liquid, carries out cation exchange resin back flush, washing time is 1.5 ~ 2.5h, and irrigation flow rate is 18 ~ 22m/ with demineralized water
h.3rd, organic solvent recovery lye rinses：The cumulative volume of recovery medicament is treat recovery cation exchange resin volume 4 times.It is multiple
The percentage by weight composition of medicament of reviving is respectively the organic additive of 8 ~ 15%NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%；Elution time control
System is in the range of 6 ~ 12h.Resuscitation process temperature control is in the range of 36 ~ 42 DEG C, the control of whole process recovery medicament rate of circulating flow
In 3.5 ~ 4.5m/h.4th, rinse：After elution, cation exchange resin rinses 20 ~ 32min with demineralized water, flow control 8 ~
In the range of 12m/h, pH is controlled 7.0 ~ 7.5.Resin industry and traffic is measured after the completion of flushing, acquired results insert table 1.
Resin industry and traffic under the conditions of the different recoveries of table 1.
As it can be seen from table 1 cation exchange resin treated by the present method, degree of percent regeneration of resin is than traditional salting liquid regenerating resin
Regeneration degree higher, operating capacity after regeneration is close to fresh resin.
Claims (6)
1. the method for resuscitation of the cation exchange resin of organic basifier pollution, it is characterised in that it is through the following steps that realize
's：First, the transition of cation exchange resin：Circulation leaching is carried out to cation exchange resin with the hydrochloric acid that mass fraction is 4% ~ 8%
Bubble, temperature are 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, is circulated using upper entering and lower leaving mode, when circulation immersion 6 ~ 10 is small
Afterwards, it is H-type by ion exchange resin conversion；2nd, wash：After transition, waste liquid is exhausted, cation exchange resin is carried out instead with demineralized water
To flushing, washing time is 1.5 ~ 2.5h, and irrigation flow rate is 18 ~ 22m/h；3rd, organic solvent recovery lye rinses：Recovery medicament
Cumulative volume be treat recovery cation exchange resin volume 4 times；The percentage by weight composition of recovery medicament is respectively 8 ~ 15%
The organic additive of NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%；Elution time is controlled in the range of 6 ~ 12h；Resuscitation process temperature control
In the range of 36 ~ 42 DEG C, whole process recovery medicament rate of circulating flow is controlled in 3.5 ~ 4.5m/h；4th, rinse：After elution, sun from
Sub-exchange resin rinses 20 ~ 32min with demineralized water, and in the range of 8 ~ 12m/h, pH is controlled 7.0 ~ 7.5 flow control；Rinse
After the completion of resin it is spare.
2. the method for resuscitation of the cation exchange resin of organic basifier pollution as described in claim 1, it is characterised in that step
Cation exchange resin transition follows cation exchange resin with the hydrochloric acid that weight percent concentration is 4% ~ 8% in rapid one
Ring soaks, and temperature is 18 ~ 25 DEG C, and rate of circulating flow is 2.5 ~ 3.5m/h, is circulated using upper entering and lower leaving mode, the time of circulation immersion
For 6 ~ 10 it is small when.
3. the method for resuscitation of the cation exchange resin of organic basifier pollution as described in claim 1, it is characterised in that step
With desalination washing time it is 1.5 ~ 2.5h in rapid two, irrigation flow rate is 18 ~ 22m/h.
4. the method for resuscitation of the cation exchange resin of the organic pollution as described in claim 1, it is characterised in that step 3
The percentage by weight composition of each recovery medicament is respectively the organic additive of 8 ~ 15%NaCl+0.5 ~ 4%NaOH+0.1 ~ 10%, protection
Agent weight percent concentration 0.15% ~ 2.5%, oxidant weight percent concentration are 1% ~ 5%.
5. the method for resuscitation of the cation exchange resin of organic basifier pollution as described in claim 1, it is characterised in that step
Rapid three elution times control is in the range of 6 ~ 12h, and resuscitation process temperature control is in the range of 36 ~ 42 DEG C, recovery medicament recycle stream
Speed control is in 3.5 ~ 4.5m/h.
6. the method for resuscitation of the cation exchange resin of organic basifier pollution as described in claim 1, it is characterised in that step
Cation exchange resin rinses 20 ~ 32min with demineralized water in rapid four, and in the range of 8 ~ 12m/h, pH is controlled 7.0 flow control
~7.5。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111282603A (en) * | 2020-03-27 | 2020-06-16 | 安徽银创生物科技股份有限公司 | Regeneration method of waste cation exchange resin |
| CN113908889A (en) * | 2021-11-22 | 2022-01-11 | 西安热工研究院有限公司 | Ion exchange resin transformation regeneration method and batch processing device |
| CN114689830A (en) * | 2022-05-06 | 2022-07-01 | 华电电力科学研究院有限公司 | Bicarbonate radical exchange capacity detection method and device for anion resin |
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| 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 |
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| CN102658217A (en) * | 2012-05-08 | 2012-09-12 | 哈尔滨工业大学 | Method for recovering anion exchange resin polluted by organic matters and recovery medicine |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111282603A (en) * | 2020-03-27 | 2020-06-16 | 安徽银创生物科技股份有限公司 | Regeneration method of waste cation exchange resin |
| CN111282603B (en) * | 2020-03-27 | 2023-03-24 | 安徽银创生物科技股份有限公司 | Regeneration method of waste cation exchange resin |
| CN113908889A (en) * | 2021-11-22 | 2022-01-11 | 西安热工研究院有限公司 | Ion exchange resin transformation regeneration method and batch processing device |
| CN114689830A (en) * | 2022-05-06 | 2022-07-01 | 华电电力科学研究院有限公司 | Bicarbonate radical exchange capacity detection method and device for anion resin |
| CN114689830B (en) * | 2022-05-06 | 2023-05-26 | 华电电力科学研究院有限公司 | Bicarbonate exchange capacity detection method and device for anion resin |
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Application publication date: 20180508 |