CN106732832B - EDTA metal complex is recycled using metal salt solution and regenerates the method for Chioro-anion exchange resin - Google Patents
EDTA metal complex is recycled using metal salt solution and regenerates the method for Chioro-anion exchange resin Download PDFInfo
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- CN106732832B CN106732832B CN201710057865.5A CN201710057865A CN106732832B CN 106732832 B CN106732832 B CN 106732832B CN 201710057865 A CN201710057865 A CN 201710057865A CN 106732832 B CN106732832 B CN 106732832B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—Separation; Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- Organic Chemistry (AREA)
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- Environmental & Geological Engineering (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
A method of EDTA cadmium metal complex compound and regeneration Chioro-anion exchange resin are recycled using metal salt solution, it adsorbs EDTA cadmium metal complex compound using chlorine type resin anion (R.A.), again using the Chioro-anion exchange resin after load EDTA cadmium metal complex compound as process object, select metal salt solution as regenerative agent, dynamic regeneration is carried out to the chlorine type resin anion (R.A.) after absorption, then regenerated liquid is handled, recycles EDTA and cadmium metal.After processed by the invention, EDTA cadmium metal complex compound in complex solution can effectively be recycled, and resin passes through after recycling several times, resin still has preferable adsorption effect, it provides convenience for large-scale experiment from now on, certain processing time and cost are reduced, and EDTA metal complex solution can be reduced to secondary pollution caused by environment.
Description
Technical field
It the present invention relates to the use of metal salt solution recycling EDTA metal complex and regenerate Chioro-anion exchange resin
Method.
Background technique
Ion exchange resin has many advantages, such as that good chemical stability, high mechanical strength, exchange capacity are big, thus uses in boiler
Water process and demineralized water, pure water production in be widely used.In use, but it is continuous ejected wash water often occur
Phenomena such as increase, effluent quality is poor, and periodical water production constantly declines, and darkens, and resin exchange capacity constantly declines.According to
The above phenomenon can regard as resin and be contaminated.If take reasonable measure makes its regeneration not in time, resin mistake will result in
Effect, or even scrap, it influences normally to produce.
Currently, regeneration of ion-exchange resin technology mainly has NaCl method of reproduction, soda acid again in softening and desalination process
It thinks of a way, CO2Regenerant ions exchange process, electrically regenerative method, ultrasound desorption etc., wherein NaCl method of reproduction, acid-alkali regeneration technology are own passes through
To being widely applied, these regeneration treatments technical matters, in terms of respectively have feature.Such as: NaCl method of reproduction
It is mainly used in ion exchange softening water process, ion exchange softening water process is using commutative in cation exchange resin
Cation (such as from Na+、H+), the calcium and magnesium ion that obtains contained in water is cemented out, for the exchange energy for restoring ion exchange resin
Power generallys use industrial table salt solution (8%-10%) and is regenerated.Regeneration for strong acid positive resin generally uses HCl
And H2SO4Make regenerative agent, the regeneration of strong basicity negative resin generally cooks regenerative agent using NaOH.Use CO2Regenerate Subacidity cation
Exchanger resin is mainly reflected in the CARIX technique proposed by Karlsruhe Nuclear research centre, West Germany, and the technique is by means of freedom
The weak acid positive resin and HCO of sour form3 -The anionite of type, so that the salt dissolved in water is carbonated substitution, in reaction
Release carbon dioxide.Under pressure, carbon dioxide is dissolved in water generation carbonic acid, it can regenerate cation and anion exchange simultaneously
Agent.For electrically regenerative method, due to the effect of electric field force, on the boundary that anion exchange resin and cation exchange resin particle contact
On face, by H2The H of O ionization and generation3O+And OH-Ion, which respectively enters, sets positive and negative ion inside cationic, anionic exchange resin
It swaps out and.Positive and negative ion passes through cation-exchange membrane respectively and enters dope room drains as concentrate.
A large number of studies show that EDTA can be with gold being carried out in lessivation with chelating agent EDTA to heavy-metal contaminated soil
Belong to ion and form stable complex state anion, if the direct emission for generating a large amount of EDTA metal complex solutions can be to environment
Secondary pollution is caused, in addition costly in view of EDTA price, when handling a large amount of polluted soils, required higher cost.?
It is general to select anion exchange resin to the EDTA in waste liquid in research with ion-exchange processing EDTA metal complex waste liquid
Metal complex anions are handled, but if regenerating not in time to resin after absorption, will lead to efficiency lost resin and report
It is useless, in addition, also needing to recycle EDTA metal complex in resin, elution cost can be saved, reduces secondary pollution.Therefore,
It is high to select EDTA metal complex recovery efficiency in some pairs of EDTA metal complex solution, it is easy to operate, and to resin regeneration
Effect is good, and is the key that resin treatment heavy metal waste liquid to the lower regenerative agent of subsequent concentration treatment cost of waste liquor.
Summary of the invention
It is negative using metal salt solution recycling EDTA cadmium metal complex compound and regeneration chlorine type that the object of the present invention is to provide a kind of
The method of ion exchange resin, with solve present in existing ion exchange technique it is low to EDTA metal complex recovery efficiency,
The problems such as resin regeneration effect is poor, subsequent concentration liquid waste processing is difficult.
To achieve the goals above, the technical solution adopted by the present invention are as follows: a kind of to recycle EDTA cadmium using metal salt solution
Metal complex and the method for regenerating Chioro-anion exchange resin comprising following steps:
(1) diameter height is chosen than the glass chromatography column for 2.5-15, and precision weighs quantitative Chioro-anion exchange resin, then
It is fitted into glass chromatography column；
(2) it is pumped into glass chromatography column, and makes using constant flow pump using EDTA cadmium metal complex solution as adsorption liquid
EDTA cadmium metal complex solution passes downwardly through glass chromatography column at the top of glass chromatography column, realizes dynamic upper prop, when chlorine type yin
The mass volume ratio of ion exchange resin and EDTA cadmium metal complex solution stops sample introduction after reaching 1:325；
(3) it chooses metal active and is better than the metal salt solution of cadmium as regenerative agent, using constant flow pump according to 0.5-2L/min
Flow velocity metal salt solution is pumped into respectively through step (2) obtain load EDTA cadmium metal complex compound chlorine type anion exchange
Resin, and metal salt solution is made to pass downwardly through glass chromatography column at the top of glass chromatography column, until in unit volume regenerated liquid
EDTA cadmium metal complex compound content is lower than 0.021mg/L；
(4) regenerated liquid containing EDTA cadmium metal complex compound in collection step (3), is added quality into the regenerated liquid of collection
Concentration be 5% calcium oxide solution, adjust pH to 9~10, be stirred to react 2 hours, be centrifuged, filtering, recycling heavy metal precipitation with
EDTA-Ca solution.
It is 0.5-50mmol/L that EDTA cadmium metal complex solution, which is by cadmium pollution soil and concentration, in the step (2)
Ca-EDTA solution, which is mixed, to be made.
The metal salt solution is calcium chloride, and magnesium sulfate, ferrum sulfuricum oxydatum solutum, concentration is 0.5-2.5mol/L, wherein sulphur
Sour ferrous solution is best.The ferrum sulfuricum oxydatum solutum can connect the Chioro-anion exchange resin of load EDTA cadmium metal complex compound
Continue five absorption regenerations.
The present invention prepares EDTA cadmium metal complex solution using Ca-EDTA solution and cadmium pollution soil, then utilizes chlorine
Type resin anion (R.A.) adsorb EDTA cadmium metal complex compound, then by load EDTA cadmium metal complex compound after chlorine type anion exchange tree
Rouge selects metal salt solution as regenerative agent as process object, carries out dynamic regeneration to the chlorine type resin anion (R.A.) after absorption,
Then regenerated liquid is handled, recycles EDTA and cadmium metal.
In addition, resin carries out continuous absorption regeneration experiment several times after adsorbable；Merge absorption stream finally by measurement
Liquid and cadmium ion content in regeneration efflux and filtrate out, can calculate regenerative agent and imitate to the recycling of EDTA cadmium metal complex compound
The adsorption efficiency and cadmium ion removal efficiency of rate and Chioro-anion exchange resin.Continuous absorption regeneration experiment number are as follows: 5 times
More than.
EDTA calcium salt of the invention is the metal salt chelate of EDTA, and the principle of complexing heavy metal is consistent with EDTA, only
It is the H on carboxyl+By Ca2+It is replaced；During soil extracts, EDTA and retardance Metal Ions Cd are formed negatively charged
Metal complex, can be with active group Cl in Chioro-anion exchange resin functional group-Exchange reaction, final cadmium ion occurs
It is mainly fixed in the form of anion in resin phase；In fact, ion exchange process is a reversible process, therefore,
Anion (Cl during anion regeneration, in regenerant solution-, SO4 2-) in the case that concentration has comparative advantage, it can be with
Exchange reaction occurs for anion in resin phase, to make resin be regenerated, therefore metal salt solution is to EDTA metal complex
The rate of recovery is high, and reduces certain processing to the favorable regeneration effect of resin to carry out providing convenience from now in large-scale experiment
Time and cost.
Three kinds of multi-valent metal salt solutions are used in the embodiment of the present invention as regenerative agent, to chlorine type anion exchange tree
The recovering effect of EDTA cadmium metal complex compound shows themselves in that Fe in rouge2(SO4)3> MgSO4> CaCl2, wherein needed for three kinds of regenerative agents
Volume is successively are as follows: 60mL, 80mL, 100mL.For Fe2(SO4)3The concentration ratio of solution, EDTA cadmium metal complex solution reaches
1:10.Choose Fe2(SO4)3Subsequent continuous 5 absorption regenerations experiment is carried out, Chioro-anion exchange resin is to EDTA cadmium gold
The absorption adsorption efficiency for belonging to complex compound may remain in 76.64%~93.43%, Fe2(SO4)3Solution is to chlorine type anion exchange
The recovery efficiency of EDTA cadmium metal complex compound may remain in 75.65%~84.19% in resin, additionally, due to Fe2(SO4)3It is molten
Liquid is at acidity, and pH is 4.2 in regenerated liquid, is conducive to subsequent recovery processing.By adding the alkali (calcium oxide that mass concentration is 5%
Solution) processing, 93.87% is reached to cadmium ion removal rate in regenerated liquid.Therefore metal salt solution hands over recycling chlorine type anion
The EDTA metal complex changed in resin is feasible.
Specific embodiment
The invention will be described in further detail With reference to embodiment.But this should not be interpreted as in the present invention
The range for stating theme is only limitted to following implementation columns.
Example one: it tests soil used and is derived from the village Huang Gu, zhuzhou,hunan county downstream farmland, mix and stir with Ca-EDTA solution
EDTA cadmium metal complex solution is obtained after mixing, basic physical and chemical such as table 1:
Physicochemical property and cadmium metal content in 1 waste liquid of table
The specific practice are as follows:
(1) dynamic upper prop adsorbs: precision weighs 2.0g Chioro-anion exchange resin and is packed into diameter height than the glass for 2.5-15
In glass chromatographic column, so that a height of 30mm of resin layer, mineral wool is packed at the top of glass chromatography column, under constant temperature (25 DEG C), by institute
EDTA cadmium metal complex solution is obtained as adsorption liquid, is pumped into glass chromatography column using constant flow pump, from glass chromatography column
Top passes downwardly through glass chromatography column, and flow control collects efflux in 4mL/min, with every 50mL.It is golden in analytical unit volume
Belong to the variation of Cd concentration.
Statistics indicate that effluent volume is before 650mL, in per unit volume in resin dynamic upper prop adsorption process
EDTA cadmium metal complex concentration is maintained at 0.005mg/L hereinafter, after 650mL, measures EDTA cadmium in per unit efflux
Metal complex concentration begins with obvious increase, it is contemplated that EDTA cadmium metal complex compound can be constantly lost in adsorption liquid
Problem, so the volume of absorption EDTA cadmium metal complex solution is 650mL.
(2) elution curve measures: considering metal ion activity and actified solution subsequent processing problem, selects more than three kinds
Valence metal salt solution (Fe2(SO4)3、MgSO4、CaCl2) be used as regenerative agent, under room temperature (25 DEG C), using constant flow pump by three kinds not
Same regenerant solution (i.e. three kinds of multi-valent metal salt solutions: (Fe2(SO4)3、MgSO4、CaCl2) be pumped into obtained by step (1) and bear respectively
The Chioro-anion exchange resin for carrying EDTA cadmium metal complex compound passes downwardly through glass chromatography column from glass chromatography column top, flows
Speed control collects efflux in 2mL/L, with every 10mL.The variation such as table of EDTA cadmium metal complex concentration in analytical unit volume
Shown in 2, elution curve is drawn out, determines the elution volume of three kinds of multi-valent metal salt solutions
EDTA cadmium metal complex compound changes in 2 eluent of table
As known to watch 2: due to regeneration velocity (2mL/L) it is slower than adsorption flow rate (4mL/L) in the case where, can guarantee regenerative agent
It comes into full contact with, can be used effectively with resin, three kinds of multi-valent metal salt solutions all have EDTA cadmium metal complex compound in resin
There are preferable recovering effect, effect are as follows: Fe2(SO4)3> MgSO4> CaCl2.Wherein volume needed for three kinds of regenerative agents is successively are as follows:
60mL, 80mL, 100mL.Fe2(SO4)3Solution is in EDTA cadmium metal complex compound removal process, elution curve peak value highest,
For elution volume in 60mL, EDTA cadmium metal complex compound is lower (0.021mg/L) in unit volume solution, thus choose 60mL compared with
To be suitable, concentration ratio 1:10.
(3) continuous absorption regeneration experiment: under room temperature (25 DEG C), concentration is chosen in 0.5-2.5mol/L Fe2(SO4)3It is molten
Liquid tests resin progress 5 times or more continuous absorption regenerations after absorption EDTA cadmium metal complex compound, after each absorption regeneration
It is cleaned with deionized water；It is total to merge cadmium ion content and efflux in absorption efflux and regeneration efflux finally by measurement
Volume can calculate regenerative agent and imitate to the recovery efficiency of EDTA cadmium metal complex compound and the absorption of Chioro-anion exchange resin
Rate.
Wash cadmium ion Parameters variation after absorption regeneration table 3 continuous 5 times
As shown in Table 3, in 5 absorption and regenerative process, Chioro-anion exchange resin is to EDTA cadmium metal complex compound
Adsorbance constantly reduce, removal rate is maintained at 76.64%~93.43%, and adsorption efficiency has dropped 16.79%, meanwhile, parsing
Amount also has small size decline, and regeneration rate (parsing amount/adsorbance) is maintained at 75.65%~84.19%, in 5 continuous absorption regenerations
Afterwards, Chioro-anion exchange resin is able to maintain higher adsorption rate to EDTA cadmium metal complex compound, meanwhile, Fe2(SO4)3Solution
There can be preferably elution effect to EDTA cadmium metal complex compound, be indicated above Fe2(SO4)3Solution is to Chioro-anion exchange resin
Middle EDTA cadmium metal complex compound has preferable recovering effect, and the Chioro-anion exchange resin after regeneration, which is able to carry out, repeatedly to follow
Ring utilizes, and Fe2(SO4)3PH is 4.2 in regenerated liquid, more advantageous subsequent processing.
(4) regenerated liquid recovery processing test: the regenerated liquid containing EDTA cadmium metal complex compound in (3) is collected, it is carried out
Recovery processing；5% calcium oxide solution is added into regenerated liquid, adjusts pH to 9~10, is stirred to react 2 hours, is centrifuged, filtering,
Recycle heavy metal precipitation and EDTA-Ca solution.
Show to carry out regenerated liquid after adding 5% oxidation Calcium treatment by experimental data, adjusts pH range in 9~10, filtrate
Concentration of cadmium ions 0.069mg/L is dropped to by 1.128mg/L, removal rate reaches 93.87%.It is indicated above that in regenerated liquid
EDTA cadmium metal complex concentration is higher, and metal salt solution solution is to EDTA cadmium metal complex compound in Chioro-anion exchange resin
With preferable recovering effect.
The complex state anion that Chioro-anion exchange resin used in the present invention forms EDTA and cadmium metal has
There is preferable adsorption effect, processing solution amount is larger, and selected multi-valent metal salt solution is to chlorine type anion exchange tree
EDTA metal complex in rouge has preferable recovering effect, and it is higher that waste liquid concentration ratio is complexed.In addition, multivalent metal salt
Solution has preferable power of regeneration to resin, and resin carries out recycled for multiple times after regeneration.For a large-scale soil huge sum of money from now on
Belong to managemental experiment and convenience is provided, reduces certain processing time and cost, EDTA metal complex waste liquid can be reduced to environment institute
Caused by secondary pollution.
Claims (5)
1. a kind of recycle EDTA cadmium metal complex compound using metal salt solution and regenerate the method for Chioro-anion exchange resin,
It is characterized in that including the following steps:
(1) diameter height is chosen than the glass chromatography column for 2.5-15, and precision weighs quantitative Chioro-anion exchange resin, is subsequently filled into
In glass chromatography column；
(2) it is pumped into glass chromatography column using constant flow pump using EDTA cadmium metal complex solution as adsorption liquid, and makes EDTA cadmium
Metal complex solution passes downwardly through glass chromatography column at the top of glass chromatography column, realizes dynamic upper prop, when chlorine type anion is handed over
Change resin and EDTA cadmium metal complex solution mass volume ratio reach 1:325 after stop sample introduction；
(3) it chooses metal active and is better than the metal salt solution of cadmium as regenerative agent, using constant flow pump according to the stream of 0.5-2L/min
Metal salt solution is pumped into the chlorine type anion exchange tree of the load EDTA cadmium metal complex compound obtained through step (2) by speed respectively
Rouge, and metal salt solution is made to pass downwardly through glass chromatography column at the top of glass chromatography column, until unit volume regenerated liquid EDTA cadmium
Metal complex content be lower than 0.021mg/L, wherein the metal salt solution be calcium chloride solution or Adlerika, or
Person's ferrum sulfuricum oxydatum solutum；
(4) regenerated liquid containing EDTA cadmium metal complex compound in collection step (3), is added mass concentration into the regenerated liquid of collection
For 5% calcium oxide solution, pH to 9~10 is adjusted, is stirred to react 2 hours, be centrifuged, heavy metal precipitation and EDTA- are recycled in filtering
Ca solution.
2. according to claim 1 handed over using metal salt solution recycling EDTA cadmium metal complex compound and regeneration chlorine type anion
The method for changing resin, which is characterized in that EDTA cadmium metal complex solution is by cadmium pollution soil and concentration in the step (2)
It is made for the Ca-EDTA solution mixing of 0.5-50mmol/L.
3. according to claim 1 handed over using metal salt solution recycling EDTA cadmium metal complex compound and regeneration chlorine type anion
The method for changing resin, which is characterized in that the metal salt solution concentration is 0.5-2.5mol/L.
4. according to claim 3 handed over using metal salt solution recycling EDTA cadmium metal complex compound and regeneration chlorine type anion
The method for changing resin, which is characterized in that the metal salt solution is ferrum sulfuricum oxydatum solutum.
5. according to claim 3 handed over using metal salt solution recycling EDTA cadmium metal complex compound and regeneration chlorine type anion
The method for changing resin, which is characterized in that chlorine type anion exchange of the ferrum sulfuricum oxydatum solutum to load EDTA cadmium metal complex compound
Resin carries out continuous five absorption regenerations.
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| CN201710057865.5A CN106732832B (en) | 2017-01-23 | 2017-01-23 | EDTA metal complex is recycled using metal salt solution and regenerates the method for Chioro-anion exchange resin |
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| CN108977669B (en) * | 2018-09-13 | 2020-07-17 | 中南大学 | Method for deeply removing cadmium in high-concentration cobalt sulfate solution and recycling cadmium |
| CN110117043B (en) * | 2019-05-09 | 2022-07-12 | 江苏南大环保科技有限公司 | Method for removing heavy metal ions in wastewater by using ion exchange resin and regeneration method of resin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745521A (en) * | 2008-12-05 | 2010-06-23 | 中国科学院沈阳应用生态研究所 | Method for repairing cadmium-polluted soil by using chelate-enhanced plants |
| WO2011041570A1 (en) * | 2009-10-01 | 2011-04-07 | First Solar, Inc. | Self-remediating photovoltaic module |
| CN105478467A (en) * | 2016-01-25 | 2016-04-13 | 湖南农业大学 | Method for eluting heavy metals Cu, Zn, Pb and Cd in soil by use of EDTA calcium salt |
| CN105618164A (en) * | 2016-03-30 | 2016-06-01 | 伊犁川宁生物技术有限公司 | Regeneration method of decolorizing resin |
| CN105668702A (en) * | 2016-01-25 | 2016-06-15 | 湖南农业大学 | Method for removing Cu, Zn, Pb and Cd from Ca-EDTA soil leacheate by chloro-type anion exchange resin |
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2017
- 2017-01-23 CN CN201710057865.5A patent/CN106732832B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745521A (en) * | 2008-12-05 | 2010-06-23 | 中国科学院沈阳应用生态研究所 | Method for repairing cadmium-polluted soil by using chelate-enhanced plants |
| WO2011041570A1 (en) * | 2009-10-01 | 2011-04-07 | First Solar, Inc. | Self-remediating photovoltaic module |
| CN105478467A (en) * | 2016-01-25 | 2016-04-13 | 湖南农业大学 | Method for eluting heavy metals Cu, Zn, Pb and Cd in soil by use of EDTA calcium salt |
| CN105668702A (en) * | 2016-01-25 | 2016-06-15 | 湖南农业大学 | Method for removing Cu, Zn, Pb and Cd from Ca-EDTA soil leacheate by chloro-type anion exchange resin |
| CN105618164A (en) * | 2016-03-30 | 2016-06-01 | 伊犁川宁生物技术有限公司 | Regeneration method of decolorizing resin |
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