CN102502913A - Method for removing anion pollutants from water - Google Patents
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- CN102502913A CN102502913A CN2011103438762A CN201110343876A CN102502913A CN 102502913 A CN102502913 A CN 102502913A CN 2011103438762 A CN2011103438762 A CN 2011103438762A CN 201110343876 A CN201110343876 A CN 201110343876A CN 102502913 A CN102502913 A CN 102502913A
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Abstract
The invention belongs to the technical field of purification treatment, and relates to a method for removing anion pollutants from water. The method comprises the following steps of: (1) adding an adsorbent into a water body polluted by anion pollutants and undergoing an adsorption reaction at a certain temperature; and (2) after adsorption is completed, intercepting, separating and treating the adsorbent in water. The anion pollutants in drinking water are adsorbed by using the structure recovery function of a stratified bimetal hydroxide. The adsorbent has the advantages of mild preparation conditions, readily-available raw materials, low production cost, high adsorption efficiency, recyclability, removing rate of over 80 percent on common anion pollutants and good application prospect.
Description
Technical field
The invention belongs to the purification treatment technology field, relate to a kind of method of removing anionic pollutent in the water.
Background technology
In recent years, along with the increase of expanding economy and population, industry, sewage constantly increase, and water environment pollution is serious day by day, and wherein the anionic pollutent is a big main body pollutent of water environment pollution.Wherein, F
-, Cl
-, NO
3 --N and SO
4 2-Be traditional anionic pollutant, and ClO
4 -, BrO
3 -, ClO
3 -Deng being recent emerging anionic pollutant.Fluorine belongs to high toxic material, and the Gamma Magnitude fluorine can suppress the activity of enzyme in organ such as bone, tooth, cardiovascular, kidney, neural system and the tissue.Chloride content in the water is too high, can damage metallic conduit and buildings, and hinders plant-growth.The final product that nitrate nitrogen decomposes for the organic nitrogen compound nitration oxidation is if the too high levels of nitrate nitrogen in the tap water can cause the baby to suffer from conversion property oxyphorase disease.Vitriol is the main existence form of sulphur in water, and the content of vitriol causes the effect of rushing down during greater than 250mg/L.Micro-perchlorate can disturb Tiroidina normally to secrete thyroxine in the water, is identified as international novel endocrine disrupter.The EPA and the World Health Organization are placed on bromate in " possible carcinogens " classification.
To present above-mentioned anionic pollutant, main removal technology is absorption method and ion exchange method, absorption method remove negatively charged ion often adopt activated alumina, clay, etc. material, but be generally disposable input, not can be recycled.Gac is relatively poor to its adsorption effect, and the charcoal absorption effect after modification is slightly good still to exist shortcomings such as Financial cost height, material modified easy desorption, can't ensure drinking water safety.And common Financial cost of ion exchange method and operation cost be all than higher, and dope also needs further to handle.
Layered double hydroxide can utilize the instead effect exchange of interlayer anion to remove some anionic pollutants in the water body, but because ion-exchange capacity is different, some anionic pollutant such as perchlorate are difficult to remove through displacement.The inventive method is intended through the high-temperature roasting layered double hydroxide, makes it lose interlayer anion, and employing to be subject to the pyrolysated carbonate be interlayer anion, the CO that overflows after the roasting
2Can also form micropore at adsorbent surface, increase adsorption surface area.In addition, main body laminate iron compound oxide also can form complex compound with some anionic pollutant, increases loading capacity.
Summary of the invention
The objective of the invention is to provides a kind of method of removing anionic pollutant in the water to the defective of prior art.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of method of removing anionic pollutant in the water, it comprises following steps:
(1) with the sorbent material input by in the water body of anionic contaminants, carry out absorption reaction at a certain temperature;
(2) after absorption reaction is accomplished, the sorbent material in the water is held back separating treatment.
Sorbent material is selected from magnesium iron layered bi-metal oxide M g in the described step (1)
6Fe
2O
9
Negatively charged ion pollutes and is ClO in the described step (1)
4 -, BrO
3 -, ClO
3 -, NO
3 -Or F
-Deng in one or more.
The starting point concentration scope of pollutent in water is respectively ClO in the described step (1)
4 -100～5000 μ g/L, BrO
3 -100～5000 μ g/L, ClO
3 -100～5000 μ g/L, NO
3 -100～50000 μ g/L or F
-100～50000 μ g/L.
The mass ratio of sorbing material and water is 1: 100～1: 30000 in the described step (1).
Adsorption temp is 5 ℃～80 ℃ in the described step (1).
Adsorption time is 30min-12h in the described step (1).
Described step (1) is carried out in shaking table or is added whipping appts, and wherein mixing speed or shaking speed are 140-220rpm.
Need not to regulate water pH value (the water pH value scope is usually between 4～10) in the described step (1).
The sorbent material of accomplishing in the described step (2) after adsorbing passes through coagulating sedimentation or membrane filtration process and water sepn.
The renovation process of accomplishing the sorbent material of absorption in the described step (2) is heat regeneration or alkali regeneration.
Described heat is regenerated as magnesium iron layered bi-metal oxide compound that absorption is reached capacity and in retort furnace, behind 400～600 ℃ of following roasting 3～6h, is cooled to room temperature under the nitrogen protection, and vacuum seal is preserved then.
Described alkali is regenerated as magnesium iron layered bi-metal oxide compound that absorption is reached capacity through 5%NaOH and 10%Na
2CO
3The mixed alkali liquor of forming is after soaking 4h under 75 ℃, and suction filtration, drying behind 400～600 ℃ of following roasting 3～6h, are ground the vacuum seal of sieving and preserved.
Absorption 30min can remove the anionic pollutant more than 75%, and clearance can reach more than 90% behind the 6h.
Roasting attitude magnesium iron layered double hydroxide, its ideal structure formula is Mg
6Fe
2O
9Magnesium iron layered double hydroxide, its structure and brucite (Mg (OH)
2) similar, structural formula Mg
6Fe
2(OH)
16CO
34H
2O.Be MgO
6The octahedra limit that is total to each other forms laminate structure, between layer and the layer top is stacked, and interlayer passes through hydrogen bond association.Mg in the brucite laminate structure
2+To a certain extent by Fe
3+During isomorphous substitution, can cause the surplus of layer last positive charge, these positive charges are positioned at the negatively charged ion (CO of interlayer
3 2-) balance, its complementary space of interlayer is occupied by crystal water, forms magnesium iron layered double hydroxide.After this magnesium iron layered double hydroxide roasting at a certain temperature; Losing between middle water, laminate hydroxyl dehydration and interlayer carbanion is removed; Veneer structure subsides, and forms roasting attitude magnesium iron layered double hydroxide, and magnesium iron double metal composite oxides.
The preparation method of above-mentioned roasting attitude magnesium iron layered double hydroxide may further comprise the steps:
(1) the precursor magnesium iron layered double hydroxide Mg of preparation roasting attitude magnesium iron layered double hydroxide
6Fe
2(OH)
16CO
34H
2O:
Magnesium iron layered double hydroxide, it has following structural: Mg
6Fe
2(OH)
16CO
34H
2O, wherein Mg
2+And Fe
3+Positively charged ion main body laminate, CO
3 2-Be intercalant anion, after co-precipitation, stirring, crystallization, suction filtration, oven dry, prepare corresponding sorbent material precursor.
(2) preparation magnesium iron layered bi-metal oxide compound:
With the roasting at high temperature of sorbent material precursor magnesium iron layered double hydroxide, cause interlayer CO
3 2-Ion is decomposed into CO fully
2Overflow, obtain required sorbent material---roasting attitude magnesium iron layered double hydroxide (magnesium iron layered bi-metal oxide compound), Mg
6Fe
2O
9
In the described step (1):
Take by weighing [Mg
2+]/[Fe
3+The magnesium salts of]=3: 1, (described magnesium salts is selected from nitrate salt soluble in water, vitriol and muriate to molysite, and described molysite is selected from nitrate salt soluble in water, vitriol and muriate; Preferred magnesium nitrate hexahydrate, nine nitric hydrate iron), pour in the Erlenmeyer flask; Mix, normal temperature and pressure adds deionized water dissolving down, and wherein the mass ratio of deionized water and metal-salt is 0.4～0.8; Stir, consoluet mixed solution is called a after half a hour;
According to (NaOH)/(Mg+Fe) mol ratio is 2 ratio, NaOH/NaCO
3(mol ratio) is 4 ratio, takes by weighing no water sodium hydroxide, soda ash light respectively, pours in another Erlenmeyer flask; Normal temperature and pressure adds deionized water down fast makes its dissolving; Wherein the mass ratio of deionized water and metal-salt is 0.6～1.3, and induction stirring is even, obtains complete solvent soln b;
Get the deionized water of solution a and solution b TV 1/5～1/3, be heated to 75 ℃ and constant;
Solution a and solution b are dropwise also flowed (0.8～1.5mL/min; Be that both splash in the deionized water with identical speed respectively simultaneously) be added drop-wise in above-mentioned 75 ℃ of deionized waters; And constantly stir this mixed solution, keep the pH value of system of the mixed solution of solution a and solution b to maintain 7～8, and continuous stirring (200～350rpm) after solution a dropwises; Add the NaOH solution of 0.1mol/L, the pH value that makes mixed serum is 7～8; Vigorous stirring (30min～the 60min of 300rpm～500rpm) again.
The mixed serum of above-mentioned solution a that obtains and solution b is placed 75 ℃ of crystallization 24～48h in the baking oven; Suction filtration is then with no CO
2Redistilled water repetitive scrubbing filter cake, originally washing speed is slower, and with increasing of washing times, speed is more and more faster, continues washing, is neutral until filtrating pH;
With the filter cake extrusion molding, insert in the vacuum drying oven, 75 ℃ vacuumize dry 24～48h, obtain magnesium iron layered double hydroxide, and molecular formula is Mg
6Fe
2(OH)
12CO
34H
2O;
In the described step (2):
The magnesium iron layered double hydroxide (Mg that step (1) is made
6Fe
2(OH)
16CO
34H
2O) 400～600 ℃ of roasting 3～6h in retort furnace feed nitrogen then and are cooled to room temperature, obtain roasting attitude magnesium iron layered double hydroxide, i.e. magnesium iron layered bi-metal oxide compound (Mg
6Fe
2O
9), vacuum seal bag kept dry.
Magnesium iron layered double hydroxide loses interlayer anion and water molecules under the condition of high-temperature roasting, thereby causing that laminate structure is collapsed forms the sosoloid of MOX, and the reaction formula that take place this moment is:
Mg
6Fe
2(OH)
16CO
3·4H
2O→Mg
6Fe
2O
9+CO
2+12H
2O。
The invention has the advantages that:
The present invention utilizes magnesium salts, molysite to be main raw material, adopts low supersaturation coprecipitation method, through steps such as crystallization, suction filtration, washing, oven dry, forms magnesium iron layered double hydroxide, selects the CO that at high temperature very easily decomposes
3 2-As interlayer anion, the CO that overflows after the roasting
2Not only make interlayer anion disappearance main body laminate be positive polarity and can also form microvoid structure, increase adsorption surface area on magnesium iron double metal composite oxides surface.Utilize the structure recovery function of layered double hydroxide to adsorb the anionic pollutent in the tap water.Preparation condition is gentle, raw material is easy to get, production cost is low, adsorption efficiency is high, and can be recycled, and the clearance of common anionic pollutant is all reached more than 80%, has a good application prospect.
Description of drawings
Fig. 1 is the XRD spectra of the magnesium iron double metal composite oxides behind magnesium iron layered double hydroxide, magnesium iron double metal composite oxides and the absorption perchlorate; Wherein a is a magnesium iron layered double hydroxide; B is magnesium iron double metal composite oxides, and c is the magnesium iron double metal composite oxides behind the absorption perchlorate.
Embodiment
Embodiment 1
(1) takes by weighing 192.3075g magnesium nitrate hexahydrate and 101.005g nine nitric hydrate iron; Pour in the 500mL Erlenmeyer flask; Add the 150mL deionized water dissolving after mixing again; If there is fine particle to dissolve, can on magnetic stirrer, stir behind ultrasonic 3～5min, consoluet mixed solution is called a after half a hour.Take by weighing 80.02g respectively and do not have water sodium hydroxide and two kinds of medicines of 52.995g soda ash light; Pour in another 500mL Erlenmeyer flask, add deionized water 150mL fast and make its dissolving, if there is fine particle to dissolve; Induction stirring is even after can ultrasonic 3～5min, obtains complete solvent soln b.
(2) clean two 150mL constant pressure funnel, its stopping property is checked in oven dry, ready after, respectively a, b two solution major parts are transferred in two constant pressure funnel, it is for use to reserve two portions.Clean pH meter, paper towel is dried gently, and calibration repeatedly in the standard acid-base solution, and till the pH meter reading equated basically with the pH value of standard acid-base solution and be stable, calibration finished the back and cleans pH meter once more with zero(ppm) water, cleans for use.
(3) get a 1000mL large beaker, the deionized water of the 150mL that in beaker, packs into places to be heated to 75 ℃ and constant on the magnetic stirrer.Two constant pressure funnel that fill a, b solution are respectively placed on the large beaker, and put into pH meter, place on the agitator and constantly stir; At any time regulate the speed of constant pressure funnel based on the pH value of solution, the pH value of reaction system is remained at about 7.5, and keep suitable rate of titration (1mL/min as far as possible; More slowly mix guaranteeing), when pH value departs from 7.5 when far away accidentally, absorption is on a small quantity from the fraction aqueous slkali of reserving with simple and easy suction pipe; Manually splash into and make pH get back to 7.5 about 1.5h in the beaker to dropwise; Vigorous stirring 0.5h again, and add an amount of NaOH solution, make the pH value about 7.5;
(4) slurries in the beaker are transferred in the filter flask, place in the baking oven 75 ℃ of crystallization 24h after, take out Erlenmeyer flask, the bottom is a white precipitate, top is clear water.Suction filtration is then with no CO
2Redistilled water repetitive scrubbing filter cake, originally washing speed is slower, and with increasing of washing times, speed is more and more faster, continues washing, is neutral until filtrating pH.With the filter cake extrusion molding, insert in the vacuum drying oven, 75 ℃ vacuumize dry 24h, obtain magnesium iron layered double hydroxide Mg
6Fe
2(OH)
16CO
34H
2O;
(5) with the magnesium iron layered double hydroxide (Mg that makes
6Fe
2(OH)
16CO
34H
2O) 550 ℃ of roasting 4h in retort furnace feed nitrogen then and are cooled to room temperature, obtain magnesium iron layered bi-metal oxide M g
6Fe
2O
9, grind under the condition of nitrogen gas and sieve.Vacuum seal bag kept dry;
(6) deionized water configuration starting point concentration is the sodium perchlorate solution of 2000 μ g/L, pipettes 200mL solution in the 250mL port grinding bottle with graduated cylinder;
(7) be that 140 purpose magnesium iron layered bi-metal oxide compound 0.2g put into the above-mentioned deionized water (weight ratio of sorbent material and water is about 1: 1000) that contains sodium perchlorate with particle diameter; Put into shaking table at normal temperatures; Rotating speed 200rpm; Behind vibration 30min, 1h, 2h, 3h, 4h, 5h, 6h, 8h, 12h, the 24h, get the 5mL adsorption liquid respectively and cross 0.45 μ m membrane filtration, through ion chromatography perchlorate's adsorption rate;
(8) the adsorbable perchlorate more than 70% of absorption 30min of ion chromatography survey, clearance is up to more than 90% behind the absorption 12h.Temperature is high more, and adsorption time is short more, and solution need not to regulate the pH value, is not only applicable to tap water, also is applicable to acidity and alkaline perchlorate contaminated water body;
(9) the magnesium iron double metal composite oxides that absorption reached capacity repeating step (6) behind 550 ℃ of roasting 6h in retort furnace, clearance still can reach more than 65% in the 30min, and clearance can reach 87.5% in the 12h, representes this adsorption functional material reusable edible.
A is a magnesium iron layered double hydroxide XRD spectra among the figure; Find out that therefrom all peaks are comparatively sharp-pointed and intensity is higher; Each secondary diffraction peak can significantly be observed, and shows that the magnesium iron layered double hydroxide crystalline form of low supersaturation coprecipitation method preparation is complete, is the laminated metal compound; B is magnesium iron double metal composite oxides, and is visible, after roasting, and interlayer anion CO
3 2-Become CO
2Overflow, laminate structure is caved in, and corresponds to magnesium iron double metal composite oxides; C is the magnesium iron double metal composite oxides behind the absorption perchlorate; Visible by figure; The perchlorate of absorption makes magnesium iron double metal composite oxides return to obvious laminate structure as interlayer anion, shows that the removal of perchlorate is owing in the magnesium iron layered double hydroxide laminate structure regenerative process; Perchlorate also is " a structure memory effect " as between the balance anion interposed layer.
Embodiment
In sum, the adsorption functional material of the present invention's preparation can adsorb removal to the perchlorate in the tap water, reaches water quality standard for drinking water.
Embodiment 2
(1) repeats instance 1 step (1)～(5).
(2) deionized water disposes ClO respectively
4 -Concentration 2000 μ g/L, BrO
3 -Concentration 2000
-μ g/L, NO
3 -Concentration 5000 μ g/L, Cl
-Concentration 5000 μ g/L, H
2PO
4 -Concentration 5000 μ g/L, SO
4 2-Concentration 5000 μ g/L, CO
3 2-The solution of concentration 5000 μ g/L.Respectively pipette the 200mL mixing solutions in the 250mL port grinding bottle with graduated cylinder.
(3) be that 140 purpose magnesium iron layered bi-metal oxide compound 0.5g put into the above-mentioned deionized water (weight ratio of sorbent material and water is 1: 400) that contains anionic pollutant with particle diameter; Put into shaking table for 25 ℃ at normal temperatures; Rotating speed 200rpm; Behind the vibration 12h, get the 5mL adsorption liquid respectively and cross 0.45 μ m membrane filtration, through the adsorption rate to each anionic pollutant of ion chromatography sorbent material.
Behind the ion-chromatographic determination absorption 12h, sorbent material is to ClO
4 -, BrO
3 -, NO
3 -, Cl
-, H
2PO
4 -, SO
4 2-,, CO
3 2-Clearance be respectively 91.3%, 88.5%, 87.2%, 83.6%, 84.5%, 88.9% and 91.86%.
Embodiment 3
(1) repeats instance 1 step (1)～(5).
(2) configuration ClO
4 -Starting point concentration is 2000 μ g/L, pH value and is respectively each 200mL of solution of 2,4,6,8,10,12; Drop into 0.5g sorbent material (weight ratio of sorbent material and water is 1: 400) respectively; Put into shaking table at normal temperatures, rotating speed 200rpm is behind the vibration 12h; Get the 5mL adsorption liquid respectively and cross 0.45 μ m membrane filtration, through the removal efficient of ion chromatography sorbent material the perchlorate.
(3) experiment shows, sorbent material is that 2,4,6,8,10,12 perchlorate clearance is respectively 45%, 88.51%, 90.40%, 89.92%, 85.92 and 53.76% to the pH value.
Embodiment 4
(1) repeats instance 1 step (1)～(5).
(2) configuration ClO
4 -Starting point concentration is 2000 each 200mL of μ g/L solution; Drop into 0.005,0.02,0.05,0.1,0.2 respectively, 0.5g and 2g sorbent material (weight ratio of sorbent material and water was respectively 1: 30000,1: 10000,1: 4000,1: 2000,1: 1000,1: 400 and 1: 100); Put into shaking table at normal temperatures, rotating speed 200rpm is behind the vibration 12h; Get the 5mL adsorption liquid respectively and cross 0.45 μ m membrane filtration, through the sorbent material of the different dosages of ion chromatography clearance the perchlorate.
(3) experiment shows that the sorbent material dosage is respectively 0.005,0.02,0.05,0.1,0.2, the perchlorate clearance of 0.5g and 2g is respectively 47%, 65%, 71%, 76%, 82%, 92% and 96%.
Embodiment 5
(1) repeats instance 1 step (1)～(5).
(2) configuration ClO
4 -Starting point concentration is 2000 each 200mL of μ g/L solution; Drop into 0.5g sorbent material (weight ratio of sorbent material and water is 1: 400) respectively; Put into shaking table at 5,15,25,35,45 ℃ respectively, rotating speed 200rpm is behind the vibration 12h; Get the 5mL adsorption liquid respectively and cross 0.45 μ m membrane filtration, sorbent material is to perchlorate's clearance under the ion chromatography differing temps.
(3) experiment shows that adsorbent temperature is respectively 5,15,25,35,45 ℃ perchlorate clearance and is respectively 67%, 70%, 92%, 91% and 93%.
Temperature is high more, and adsorption time is short more, and solution need not to regulate the pH value, is not only applicable to tap water, also is applicable to acidity and basic anion polluted-water.
The above-mentioned description to embodiment is can understand and use the present invention for ease of the those of ordinary skill of this technical field.The personnel of skilled obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. method of removing anionic pollutant in the water, it is characterized in that: it comprises following steps:
(1) with the sorbent material input by in the water body of anionic contaminants, carry out absorption reaction at a certain temperature;
(2) after absorption reaction is accomplished, the sorbent material in the water is held back separating treatment.
2. method according to claim 1 is characterized in that: sorbent material is selected from magnesium iron layered bi-metal oxide M g in the described step (1)
6Fe
2O
9
3. method according to claim 1 is characterized in that: negatively charged ion pollutes and is ClO in the described step (1)
4 -, BrO
3 -, ClO
3 -, NO
3 -Or F
-In one or more.
4. method according to claim 1 is characterized in that: the starting point concentration scope of pollutent in water is respectively ClO in the described step (1)
4 -100～5000 μ g/L, BrO
3 -100～5000 μ g/L, ClO
3 -100～5000 μ g/L, NO
3 -100～50000 μ g/L or F
-100～50000 μ g/L.
5. method according to claim 1 is characterized in that: the mass ratio of sorbing material and water is 1: 100～1: 30000 in the described step (1).
6. method according to claim 1 is characterized in that: adsorption temp is 5 ℃～80 ℃ in the described step (1);
Or adsorption time is 30min-12h in the described step (1).
7. method according to claim 1 is characterized in that: described step (1) is carried out in shaking table or is added whipping appts, and wherein mixing speed or shaking speed are 140-220rpm.
8. method according to claim 1 is characterized in that: the sorbent material of accomplishing in the described step (2) after adsorbing passes through coagulating sedimentation or membrane filtration process and water sepn.
9. method according to claim 1 is characterized in that: the renovation process of accomplishing the sorbent material of absorption in the described step (2) is heat regeneration or alkali regeneration.
10. method according to claim 9; It is characterized in that: described heat is regenerated as magnesium iron layered bi-metal oxide compound that absorption is reached capacity in retort furnace behind 400～600 ℃ of following roasting 3～6h; Be cooled to room temperature under the nitrogen protection, vacuum seal is preserved then;
Or described alkali is regenerated as magnesium iron layered bi-metal oxide compound that absorption is reached capacity through 5%NaOH and 10%Na
2CO
3The mixed alkali liquor of forming is after soaking 4h under 75 ℃, and suction filtration, drying behind 400～600 ℃ of following roasting 3～6h, are ground the vacuum seal of sieving and preserved.
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