CN102631955B - Restoration method for removing iron pollution of anion exchange resin and restoration drug formula - Google Patents
Restoration method for removing iron pollution of anion exchange resin and restoration drug formula Download PDFInfo
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- CN102631955B CN102631955B CN201210136938.7A CN201210136938A CN102631955B CN 102631955 B CN102631955 B CN 102631955B CN 201210136938 A CN201210136938 A CN 201210136938A CN 102631955 B CN102631955 B CN 102631955B
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- exchange resin
- anion exchange
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- resuscitation
- iron pollution
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Abstract
The invention discloses a restoration method for removing iron pollution of an anion exchange resin and a restoration drug formula, which can be used for solving the problem that the environment is polluted and an anion exchange resin tank is corroded because the use of sodium sulfite and concentrated hydrochloric acid in the original restoration formula and restoration drug formula of the anion exchange resin can cause toxic gas SO2. The restoration method comprises the following steps: 1. transforming the anion resin; 2. washing; 3. removing the iron pollution of the anion resin to lead the anion resin to restore; 4. washing; and 5. regenerating. The restoration drug formula consists of hydrochloric acid, sodium chloride, hydroxylamine hydrochloride and water, wherein the weight percent of the above components in water are as follows: 2-6% of hydrochloric acid, 4-8% of sodium chloride and 1-5% of hydroxylamine hydrochloride. The restoration method is suitable for restoration of the iron pollution of the anion resin and is effective in removing the iron pollution of a cation resin.
Description
Technical field
The present invention relates to remove method for resuscitation and the analeptic agent prescription of anion exchange resin iron pollution.
Background technology
Iron pollution anion exchange resin surface is two kinds of forms: the first, cover anion exchange resin surface; The second, be deposited in anion exchange resin duct.Because the iron-holder of regeneration alkali lye is too high, or misoperation, iron exists with the form of complex compound and oxide, the relative anion exchange resin of its volume duct is larger, cannot enter anion exchange resin duct, under anion exchange resin surface deposits rapidly, then cover its particle surface.The contaminated rear color of anion exchange resin becomes brown even black, and exchange capacity sharply declines.On Industrial Boiler, for reducing the anion exchange resin ubiquity of feed-water hardness, " iron poisoning " phenomenon at present.Remove the operation of iron in anion exchange resin and be called " recovery " or " removing toxic substances ".Iron to the pollution of anion exchange resin have multiple may, for the oxide of iron ion, hydroxide, sulfide, carbonate, phosphate etc. are imperceptible, be suspended the pollution that particle adheres to or adsorb, comparatively traditional method is employing hydrochloric acid infusion method.In actual production, conventional method for resuscitation is to soak anion exchange resin with concentrated hydrochloric acid, but this method exists an outstanding problem, Here it is, and resuscitation effect is not ideal enough, after each recovery, in anion exchange resin, iron content reaches 200～300mg/kg, and also can corrode anion exchange resin tank.
Summary of the invention
The present invention is the method that will solve existing concentrated hydrochloric acid immersion anion exchange resin, the problem that its resuscitation effect is poor and the existence of original recovery formula is corroded anion exchange resin tank, and a kind of method for resuscitation and analeptic agent prescription of removing anion exchange resin iron pollution is provided.
In the present invention, a kind of method for resuscitation of removing anion exchange resin iron pollution is realized by following steps: one, the transition of anion exchange resin: the saline solution that is 8%～10% by weight percent concentration carries out circulation immersion to anion exchange resin, temperature is 18～22 ℃, rate of circulating flow is 2～3m/h, adopt upper entering and lower leaving mode to circulate, after circulation immersion 6～10 hours, complete transition.Two, rinse: after transition, the waste liquid of draining, carries out back flush to anion exchange resin with desalted water, and washing time is 1.5～2.5h, and irrigation flow rate is 18～22m/h.Three, remove anion exchange resin iron pollution and make its recovery: chemical tank and circulating pump are set, recovery medicament are squeezed into anion exchange resin tank and carry out recycling elution.Resuscitation fluid cumulative volume is to treat 3～4 times of recovery resin volume.For strengthening resuscitation effect, take the mode of gradation recovery, carry out altogether 3～4 times, recovery bolus volume each time with treat that recovery anion exchange resin volume is identical, each elution time is 2～2.5h, rate of circulating flow is 2～3m/h at every turn.Each recovery finishes the rear desalted water back flush anion exchange resin of using, and washing time is 18～22min, and back flush flow velocity is 9～11m/h, and during wash-out anion exchange resin, whole recovery process temperature is 35～39 ℃.Four, rinse: the anion exchange resin after recovery carries out back flush with desalted water, and washing time is 2.5～3.5h, and back flush flow velocity is 9～11m/h.Five, regeneration: after resin recovery, carry out the regeneration of resin with standby.
In the present invention, a kind of analeptic agent prescription of removing anion exchange resin iron pollution, is comprised of hydrochloric acid, sodium chloride, hydroxylamine hydrochloride and water, and wherein hydrochloric acid, sodium chloride and the hydroxylamine hydrochloride weight percent concentration in water is respectively 2～6%, 4～8% and 1～5%.
Beneficial effect of the present invention:
1, the reducing agent NHOHHCl in recovery medicament is reduced to ferrous ion (because of easier oxide or the hydroxide that again forms iron of ferric ion by the ferric ion eluting, their some anion or organic matter complexings easily and in water, form new anion complex or organic matter and recontamination anion exchange resin), thus de-ironing efficiency greatly improved.
2, recovery medicament is greatly reduced the consumption of the concentrated hydrochloric acid in conventional method by hydrochloric acid, sodium chloride and hydroxylamine hydrochloride solution composition, efficiently solves the etching problem of concentrated hydrochloric acid to resin container.
3, in the recovery medicament using in method for resuscitation, contain reducing agent NHOHHCl, efficiently solve traditional reducing agent sodium sulfite and in application, easily produce toxic gas SO
2problem.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: in present embodiment, a kind of method for resuscitation of removing anion exchange resin iron pollution carries out according to the following steps:
One, the transition of anion exchange resin: the saline solution that is 8%～10% by weight percent concentration carries out circulation immersion to anion exchange resin, temperature is 18～22 ℃, and rate of circulating flow is 2～3m/h, adopts upper entering and lower leaving mode to circulate, after circulation immersion 6～10 hours, complete transition.Two, rinse: after transition, the waste liquid of draining, carries out back flush to anion exchange resin with desalted water, and washing time is 1.5～2.5h, and irrigation flow rate is 18～22m/h.Three, remove anion exchange resin iron pollution and make its recovery: chemical tank and circulating pump are set, recovery medicament are squeezed into anion exchange resin tank and carry out recycling elution.Resuscitation fluid cumulative volume is to treat 3～4 times of recovery resin volume.For strengthening resuscitation effect, take the mode of gradation recovery, carry out altogether 3～4 times, recovery bolus volume each time with treat that recovery anion exchange resin volume is identical, each elution time is 2～2.5h, rate of circulating flow is 2～3m/h at every turn.Each recovery finishes the rear desalted water back flush anion exchange resin of using, and washing time is 18～22min, and back flush flow velocity is 9～11m/h, and during wash-out anion exchange resin, whole recovery process temperature is 35～39 ℃.Four, rinse: the anion exchange resin after recovery carries out back flush with desalted water, and washing time is 2.5～3.5h, and back flush flow velocity is 9～11m/h.Five, regeneration: after resin recovery, carry out the regeneration of resin with standby.
Beneficial effect of the present invention:
1, the reducing agent NHOHHCl in recovery medicament is reduced to ferrous ion (because of easier oxide or the hydroxide that again forms iron of ferric ion by the ferric ion eluting, their some anion or organic matter complexings easily and in water, form new anion complex or organic matter and recontamination anion exchange resin), thus de-ironing efficiency greatly improved.
2, recovery medicament is greatly reduced the consumption of the concentrated hydrochloric acid in conventional method by hydrochloric acid, sodium chloride and hydroxylamine hydrochloride solution composition, efficiently solves the etching problem of concentrated hydrochloric acid to resin container.
3, in the recovery medicament using in method for resuscitation, contain reducing agent NHOHHCl, efficiently solve traditional reducing agent sodium sulfite and in application, easily produce toxic gas SO
2problem.
The specific embodiment two: present embodiment is different from the specific embodiment one: the saline solution that in step 1, anion exchange resin transition is 8.5%～9.5% by weight percent concentration carries out circulation immersion to anion exchange resin, temperature is 19～21 ℃, rate of circulating flow is 2.2～2.8m/h, adopt upper entering and lower leaving mode to circulate, the time of circulation immersion is 7～9 hours.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from the specific embodiment one: the saline solution that in step 1, anion exchange resin transition is 9% by weight percent concentration carries out circulation immersion to anion exchange resin, temperature is 20 ℃, rate of circulating flow is 2.5m/h, adopt upper entering and lower leaving mode to circulate, the time of circulation immersion is 8 hours.Other step and parameter are identical with the specific embodiment one.
The specific embodiment four: present embodiment is different from the specific embodiment one: be 1.8～2.2h with desalted water washing time in step 2, irrigation flow rate is 19～21m/h.Other step and parameter are identical with the specific embodiment one.
The specific embodiment five: present embodiment is different from the specific embodiment one: be 2h with desalted water washing time in step 2, irrigation flow rate is 20m/h.Other step and parameter are identical with the specific embodiment one.
The specific embodiment six: present embodiment is different from the specific embodiment one: in step 3, during wash-out anion exchange resin, whole recovery process temperature is 36～38 ℃.Other step and parameter are identical with the specific embodiment one.
The specific embodiment seven: present embodiment is different from the specific embodiment one: in step 3, during wash-out anion exchange resin, whole recovery process temperature is 37 ℃.Other step and parameter are identical with the specific embodiment one.
The specific embodiment eight: present embodiment is different from the specific embodiment one: in step 4, washing time is 2.5～3.5h, back flush flow velocity is 9～11m/h.Other step and parameter are identical with the specific embodiment one.
The specific embodiment nine: a kind of method for resuscitation analeptic agent prescription used of removing anion exchange resin iron pollution in present embodiment, hydrochloric acid, sodium chloride, hydroxylamine hydrochloride and water, consist of, wherein the weight percent concentration of hydrochloric acid, sodium chloride and hydroxylamine hydrochloride is respectively 2～6%, 4～8% and 1～5%.
The specific embodiment ten: present embodiment is different from the specific embodiment nine: analeptic agent prescription is comprised of hydrochloric acid, sodium chloride, hydroxylamine hydrochloride and water, wherein the weight percent concentration of hydrochloric acid, sodium chloride and hydroxylamine hydrochloride is respectively 4%, 6% and 3%.Other composition and parameter are identical with the specific embodiment nine.
For verifying beneficial effect of the present invention, carried out following experiment (in experiment, the volume of anion exchange resin is 50mL, and anion-exchange resin column volume is 300mL):
Experiment one: a kind of method for resuscitation of removing anion exchange resin iron pollution follows these steps to carry out:
One, the transition of anion exchange resin: anion exchange resin is hydrogen-oxygen type in running, for making it stable, before recovery, must transfer chlorine type to.The saline solution that is 10% by weight percent concentration carries out circulation immersion to ion exchange resin, and temperature is 19.5～20.5 ℃, and rate of circulating flow is 3m/h, adopts upper entering and lower leaving mode to circulate.After circulation immersion 10 hours, complete transition.
Two, rinse: after transition, the waste liquid of draining, carries out backwash to anion exchange resin with desalted water, and washing time is 2h, and flow control is 20m/h.
Three, remove anion exchange resin iron pollution and make its recovery: recovery medicament cumulative volume is 200mL, treats that recovery anion exchange resin volume is 50mL.For strengthening resuscitation effect, take the mode of gradation recovery, carry out altogether 4 times, recovery bolus volume each time with treat that recovery anion exchange resin volume is identical, each elution time is 2.5h, rate of circulating flow is 3m/h at every turn.Each recovery finishes the rear desalted water back flush anion exchange resin of using, and washing time is 20min, and back flush flow velocity is 10m/h, and during wash-out anion exchange resin, whole recovery process temperature is 37 ℃.In analeptic agent prescription, the weight percent concentration of hydrochloric acid, sodium chloride and hydroxylamine hydrochloride is respectively 4%, 6% and 3%.
Four, rinse: the anion exchange resin after recovery carries out back flush with desalted water, and the time is 3h, and back flush flow velocity is 10m/h.
The inventive method of learning from else's experience anion exchange resin 10mL after treatment, in anion exchange resin, iron pollution content is 95mg/kg after testing, and in actual production after conventional concentrated hydrochloric acid immersion process recovery anion exchange resin iron content reach 200～300mg/kg, de-ironing efficiency has had significantly and has improved compared with the latter.
Claims (9)
1. remove a method for resuscitation for anion exchange resin iron pollution, it is characterized in that it realizes by following steps:
One, the transition of anion exchange resin: the saline solution that is 8%～10% by weight percent concentration carries out circulation immersion to anion exchange resin, temperature is 18～22 ℃, and rate of circulating flow is 2～3m/h, adopts upper entering and lower leaving mode to circulate, after circulation immersion 6～10 hours, complete transition; Two, rinse: after transition, the waste liquid of draining, carries out back flush to anion exchange resin with desalted water, and washing time is 1.5～2.5h, and irrigation flow rate is 18～22m/h; Three, remove anion exchange resin iron pollution and make its recovery: chemical tank and circulating pump are set, and recovery medicament is squeezed into anion exchange resin tank carries out recycling elution; Resuscitation fluid cumulative volume is to treat 3～4 times of recovery resin volume; For strengthening resuscitation effect, take the mode of gradation recovery, carry out altogether 3～4 times, recovery bolus volume each time with treat that recovery anion exchange resin volume is identical, each elution time is 2～2.5h, rate of circulating flow is 2～3m/h at every turn; Each recovery finishes the rear desalted water back flush anion exchange resin of using, and washing time is 18～22min, and back flush flow velocity is 9～11m/h, and during wash-out anion exchange resin, whole recovery process temperature is 35～39 ℃; Four, rinse: the anion exchange resin after recovery carries out back flush with desalted water, and washing time is 2.5～3.5h, and back flush flow velocity is 9～11m/h; Five, regeneration: after resin recovery, carry out the regeneration of resin with standby; Wherein analeptic agent prescription described in step 3, is comprised of hydrochloric acid, sodium chloride, hydroxylamine hydrochloride and water, and hydrochloric acid, sodium chloride and the hydroxylamine hydrochloride weight percent concentration in water is respectively 2～6%, 4～8% and 1～5%.
2. a kind of method for resuscitation of removing anion exchange resin iron pollution as claimed in claim 1, it is characterized in that the saline solution that anion exchange resin in step 1 transition is 8.5%～9.5% by weight percent concentration carries out circulation immersion to anion exchange resin, temperature is 19～21 ℃, rate of circulating flow is 2.8～3m/h, adopt upper entering and lower leaving mode to circulate, the time of circulation immersion is 7～9 hours.
3. a kind of method for resuscitation of removing anion exchange resin iron pollution as claimed in claim 1, it is characterized in that the saline solution that anion exchange resin in step 1 transition is 9% by weight percent concentration carries out circulation immersion to anion exchange resin, temperature is 20 ℃, rate of circulating flow is 3m/h, adopt upper entering and lower leaving mode to circulate, the time of circulation immersion is 8 hours.
4. a kind of method for resuscitation of removing anion exchange resin iron pollution as claimed in claim 1, is characterized in that in step 2 being 1.8～2.2h with desalted water washing time, and irrigation flow rate is 19～21m/h.
5. a kind of method for resuscitation of removing anion exchange resin iron pollution as claimed in claim 1, is characterized in that in step 2 being 2h with desalted water washing time, and irrigation flow rate is controlled at 20m/h.
6. a kind of method for resuscitation of removing anion exchange resin iron pollution as claimed in claim 1, while it is characterized in that in step 3 wash-out resin anion (R.A.), whole recovery process temperature is 36～38 ℃.
7. a kind of method for resuscitation of removing anion exchange resin iron pollution as claimed in claim 1, while it is characterized in that in step 3 wash-out resin anion (R.A.), whole recovery process temperature is 37 ℃.
8. remove the method for resuscitation recovery medicament used of ion exchange resin iron pollution for one kind, it is characterized in that it is comprised of hydrochloric acid, sodium chloride, hydroxylamine hydrochloride and water, wherein hydrochloric acid, sodium chloride and the hydroxylamine hydrochloride weight percent concentration in water is respectively 2～6%, 4～8% and 1～5%.
9. recovery medicament as claimed in claim 8, is characterized in that it is comprised of hydrochloric acid, sodium chloride, hydroxylamine hydrochloride and water, and wherein the weight percent concentration of hydrochloric acid, sodium chloride and hydroxylamine hydrochloride is respectively 4%, 6% and 3%.
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| CN201210136938.7A CN102631955B (en) | 2012-05-04 | 2012-05-04 | Restoration method for removing iron pollution of anion exchange resin and restoration drug formula |
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| CN201210136938.7A CN102631955B (en) | 2012-05-04 | 2012-05-04 | Restoration method for removing iron pollution of anion exchange resin and restoration drug formula |
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| CN102631955B true CN102631955B (en) | 2014-04-23 |
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| CN103464225B (en) * | 2013-09-14 | 2014-12-10 | 大连交通大学 | Recovery method of polluted anion exchange resin |
| CN107442185A (en) * | 2017-09-28 | 2017-12-08 | 荣成市固废综合处理与应用产业园有限公司 | A kind of online recovery device of resin cation iron poisoning and method for resuscitation |
| CN113457750A (en) * | 2021-07-19 | 2021-10-01 | 南通秋之友生物科技有限公司 | Anion exchange resin recovery process applied to biological extraction |
| CN114768889B (en) * | 2022-04-07 | 2023-08-22 | 南京工业大学 | Gel type anion-cation exchange resin recovery device and recovery method |
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| CN1326622C (en) * | 2005-05-27 | 2007-07-18 | 哈尔滨工业大学 | Process for reactivating gel type strong base negative resin of polluted in industrial water treatment |
| CN101791581A (en) * | 2010-04-21 | 2010-08-04 | 陕西电力科学研究院 | Recovery liquid for ion exchange resin polluted by iron |
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