CN103578593B - A kind of method utilizing graphene-supported nano zero-valence iron composite material to remove radiocobalt - Google Patents
A kind of method utilizing graphene-supported nano zero-valence iron composite material to remove radiocobalt Download PDFInfo
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- CN103578593B CN103578593B CN201310488509.0A CN201310488509A CN103578593B CN 103578593 B CN103578593 B CN 103578593B CN 201310488509 A CN201310488509 A CN 201310488509A CN 103578593 B CN103578593 B CN 103578593B
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Abstract
The invention discloses a kind of method utilizing graphene-supported nano zero-valence iron composite material to remove radiocobalt belonging to Radwastes treatment technical field.The method, by adding graphene-supported nano zero-valence iron composite material in the water sample containing radioactive nuclide Co, then constant temperature oscillation, removes radioactive nuclide cobalt after certain hour.In the present invention, graphene-supported nano zero-valence iron composite material has adsorptive selectivity to nucleic, its adsorption capacity greatly, not easily desorption, particle after absorption has magnetic, easily recovery, volume is little, convenience is temporary, and experiment condition is gentle, in the nucleic cobalt in removal radioactive wastewater, there is advantage.The maximum equilibrium adsorption capacities of graphene-supported nano zero-valence iron composite material of the present invention to Co is 114.08mg/g.
Description
Technical field
The invention belongs to Radwastes treatment technical field, particularly a kind of method utilizing graphene-supported nano zero-valence iron composite material to remove radiocobalt.
Background technology
It is one of great environmental problem of facing of the world today that the safe handling of radioactive waste is disposed.Wherein, radioactive nuclide
60co is the neutron activation product in nuclear reaction device, is again medical gamma ray radiator, can be applicable to radiation treatment and chemotherapy.
60co has the features such as toxicity is comparatively large, half life period longer (5.27), energy of γ ray high (average 1.25MeV), conducts oneself well to put cause great impact by environment and human health as improper.
The main treatment technology of current radioactive wastewater has chemical precipitation method, evaporation concentration method, ion exchange process, soil filtration, membrane processing method, absorption method, oxidation-reduction method, biotechnology, phytoremediation etc.Wherein, absorption method treatment effeciency is higher, and process is comparatively thorough, and economic benefit is higher.Adopt novel graphite alkene material to receive as adsorbent in recent years to pay close attention to widely.Graphene is a kind of New Two Dimensional material with carbon element, is made up of the planar structure of carbon atom hexatomic ring, has very large theoretical specific surface area (2630m
2/ g); There is the oxy radicals such as a large amount of epoxide groups, hydroxyl, carboxyl in its surface, have adsorption capacity large, adsorb the features such as rapid.The people such as Romanchuk (Physicalchemistrychemicalphysics:PCCP, 15th volume the 2321st page in 2013) report graphene oxide (GO) and remove the radioactive isotope such as actinide and lanthanide series, comprise Am (III), Th (IV), Pu (IV), Np (V), U (VI), Sr (II), Eu (III) and Tc (VII).But because the surface energy of graphene oxide is higher, easily reunite, and be scattered in after in water and be difficult to separate from aqueous solution, be therefore necessary to carry out surface modification to it.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing graphene-supported nano zero-valence iron composite material to remove radiocobalt.
Nano zero valence iron has the advantages such as magnetic, particle size is little, specific surface area is large, surfactivity is large, reducing power is strong, can out be deposited on its surface, thus reach the object removing pollutant by arranging in metal activity series table in metal replacement thereafter.By nano zero valence iron load at graphenic surface, the reunion of nano material can be stoped, keep the reactivity of each component in compound substance, thus promote that material is to the removal ability of radioactive nuclide.Be applied in radionuclide contamination water body treating by graphene-supported nano zero-valence iron composite material, both efficiently can remove nucleic fast, available magnetic separation method is reclaimed again, has shown huge application potential.
Utilize graphene-supported nano zero-valence iron composite material to remove a method for radiocobalt, concrete steps are as follows:
(1) first add in reaction vessel by 1 – 2g expansible graphite, add the concentrated sulphuric acid, the mass ratio of the concentrated sulphuric acid and graphite is 70:1 – 200:1, stirs 10 – 30min in ice-water bath; Slowly add potassium permanganate, the mass ratio of potassium permanganate and graphite is 1.5:1 – 6:1, keeps system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 34-36 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, stirs 30 – 60min at 59-61 DEG C, and second time adds 40mL, keeps 30 – 60min at 89-91 DEG C, and third time directly adds 40mL deionized water; Finally add the H of 30wt%
2o
2, H
2o
2be 4.5:1 – 13.5:1 with the mass ratio of graphite, centrifugal 30min under 10000 – 12000r/min while hot, abandoning supernatant is hydrochloric acid and the distilled water centrifuge washing of 1:10 by volume ratio, obtained graphene oxide, and freeze drying is for subsequent use;
(2) graphene oxide that step (1) is obtained is placed in deionized water, ultrasonic disperse; Add FeSO
47H
2o solution, stirs and passes into argon gas and make it to be in anaerobic state; Then KBH is instilled
4solution, KBH
4solution and FeSO
47H
2the volume ratio of O solution is 1:1 – 2.5:1, and concentration ratio scope is 5:1 – 20:1; Blasting argon gas in course of reaction keeps reaction to carry out under anaerobic state; After reacting 1 – 2h, with deionized water and absolute ethanol washing centrifugal, i.e. obtained graphene-supported nano zero-valence iron composite material after vacuum drying, wherein the mass ratio of Zero-valent Iron and graphene oxide is 1:4 – 4:1.
(3) obtained graphene-supported nano zero-valence iron composite material is joined containing radioactive nuclide
60in the waste water of Co, then constant temperature oscillation.
The time of described constant temperature oscillation is 4 – 24h; Temperature is 20 – 30 DEG C.
In waste water
60the concentration of Co is 10 – 407mg/L.
The pH value of waste water is 4 – 9.
The consumption of described graphene-supported nano zero-valence iron composite material is 0.05 – 0.4g/L.
Beneficial effect of the present invention is mainly reflected in: graphene-supported nano zero-valence iron composite material has adsorptive selectivity to Co, its adsorption capacity greatly, not easily desorption, the particle after absorption has magnetic, easily reclaims, volume is little, convenience is temporary; Experiment condition is gentle, in Spent Radioactive water treatment, have advantage; By nano zero valence iron load at graphenic surface, the reunion of nano material can be stoped, keep the reactivity of each component in compound substance, thus promote that material is to the removal ability of radioactive nuclide.Graphene-supported nano zero-valence iron composite material pair
60the maximum equilibrium adsorption capacities of Co is 114.08mg/g.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited in this:
Embodiment 1
First prepare graphene oxide (GO), step is as follows: add in reaction vessel by the 106mL concentrated sulphuric acid and 1.0g expansible graphite, in ice-water bath, stir 30min; Slowly add 5g potassium permanganate, keep system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 35 ± 1 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, at 60 ± 1 DEG C, stir 60min, and second time adds 40mL, at 90 ± 1 DEG C, keep 30min, and third time directly adds 40mL deionized water; Finally add the H of 10mL30wt%
2o
2, centrifugal 30min under 12000r/min while hot, abandoning supernatant, with hydrochloric acid (massfraction 36-38%) and the distilled water centrifuge washing several of volume ratio 1:10, freeze drying is for subsequent use.
Then graphene-supported nano zero valence iron (Fe is prepared
0/ GO) compound substance, step is as follows: take 0.055g graphene oxide and be dissolved in 100mL deionized water, ultrasonic disperse 3h, adds 1.112gFeSO
47H
2o, stirs 3h and passes into argon gas and make it to be in anaerobic state; Then be the KBH of 20mM by concentration
4solution 100mL is with in certain speed instillation reaction vessel; Blasting argon gas in course of reaction keeps reaction to carry out under anaerobic state, keeps stirring to make solution be in Homogeneous phase mixing state; After reaction 1.5h, with deionized water and absolute ethanol washing centrifugal twice, after vacuum drying, namely obtain Fe
0be the Fe of 4:1 with GO duty factor
0/ GO compound substance.
By Fe
0/ GO compound substance is used for Adsorption simulated radioactive nuclein Co and Sr, and step is as follows: with 20mL reagent bottle for reactor, and waste water is Co
2+and Sr
2+solution, comprises unitary system and Co
2+and Sr
2+the competitive Adsorption coexisted, pH=6, adds the nucleic aqueous solution of 15mL and the Fe of 0.4g/L in reactor
0/ GO compound substance, reactor sealing be placed in desk-top constant-temperature shaking incubator and react, rotating speed is 150rpm, and temperature is 30 DEG C.Equilibrium adsorption capacity (q after reaction 10h
e) in table 1:
Table 1Fe
0radioactive nuclide Co and Sr removed by/GO compound substance
| System | Element | Initial concentration (mg/L) | Residual concentration (mg/L) | Equilibrium adsorption capacity (mg/g) |
| Single adsorption | Co | 29.41 | 3.65 | 64.40 |
| Single adsorption | Sr | 30.80 | 28.26 | 6.35 |
| Competitive Adsorption | Co | 29.53 | 5.20 | 60.82 |
| Competitive Adsorption | Sr | 29.97 | 29.23 | 1.85 |
Detection method: sample, after the filtering with microporous membrane of 0.22m, adopts atom absorption spectrophotometry instrument (Germany, AAS6Vario) to detect initial and remaining Sr
2+and Co
2+concentration.
It can thus be appreciated that, Fe
0/ GO compound substance has adsorptive selectivity, no matter be unitary system or competition system, its to the adsorption capacity of nucleic Co much larger than Sr.
Embodiment 2
Fe
0the preparation process of/GO compound substance is with embodiment 1.
By Fe
0/ GO compound substance is used for Adsorption simulated radioactive nuclein Co
2+, step is as follows: the Co adding 15mL in reactor
2+the Fe of aqueous solution and 0.05g/L
0/ GO compound substance, reactor sealing be placed in desk-top constant-temperature shaking incubator and react, rotating speed is 150rpm, and temperature is 30 DEG C.Equilibrium adsorption capacity (the q after 7h is reacted under different pH
e) in table 2:
Fe under the different pH of table 2
0nucleic Co removed by/GO compound substance
| pH | Initial concentration (mg/L) | Residual concentration (mg/L) | Equilibrium adsorption capacity (mg/g) |
| 3 | 10 | 5.67 | 21.67 |
| 4 | 10 | 3.66 | 31.69 |
| 5 | 10 | 2.78 | 32.82 |
| 6 | 10 | 2.94 | 35.32 |
| 7 | 10 | 2.94 | 35.32 |
| 8 | 10 | 3.05 | 34.74 |
| 9 | 10 | 2.96 | 35.21 |
Detection method: with embodiment 1.
It can thus be appreciated that, pH in 4 – 9 scopes, Fe
0/ GO compound substance is to nucleic Co
2+equilibrium adsorption capacities comparatively large, be all greater than 30mg/g.
Embodiment 3
Fe
0the preparation process of/GO compound substance is with embodiment 1.
By Fe
0/ GO compound substance is used for Adsorption simulated radioactive nuclein Co
2+, step is as follows: the Co adding 15mL in reactor
2+the Fe of aqueous solution (pH4) and 0.2g/L
0/ GO compound substance, reactor sealing be placed in desk-top constant-temperature shaking incubator and react, rotating speed is 150rpm, and temperature is 30 DEG C.Different Co
2+equilibrium adsorption capacity (the q after 8h is reacted under initial concentration
e) in table 3:
The different Co of table 3
2+fe under initial concentration
0nucleic Co removed by/GO compound substance
| Initial concentration (mg/L) | Residual concentration (mg/L) | Equilibrium adsorption capacity (mg/g) |
| 10.49 | 3.20 | 36.45 |
| 20.26 | 10.21 | 50.25 |
| 40.63 | 28.66 | 59.85 |
| 81.59 | 69.30 | 61.45 |
| 101.80 | 88.54 | 66.31 |
| 193.66 | 177.10 | 82.80 |
| 287.50 | 267.72 | 98.90 |
| 406.73 | 383.92 | 114.08 |
Detection method: with embodiment 1.
It can thus be appreciated that, Fe
0/ GO compound substance is to nucleic Co
2+maximum equilibrium adsorption capacities up to 114.08mg/g.
Embodiment 4
Fe
0the preparation process of/GO compound substance is with embodiment 1, and wherein graphene oxide consumption is 0.22g, Fe in obtained material
0be 1:1 with GO duty factor.
By Fe
0/ GO compound substance is used for Adsorption simulated radioactive nuclein Co
2+, step is as follows: the Co adding 15mL in reactor
2+aqueous solution (pH8) and Fe
0/ GO compound substance, reactor sealing be placed in desk-top constant-temperature shaking incubator and react, rotating speed is 150rpm, and temperature is 25 DEG C.Different Fe
0equilibrium adsorption capacity (the q after 4h is reacted during/GO compound substance consumption
e) in table 4:
The different Fe of table 4
0the removal situation of nucleic Co during/GO compound substance consumption
Detection method: with embodiment 1.
Embodiment 5
Fe
0the preparation process of/GO compound substance is with embodiment 1, and wherein graphene oxide consumption is 0.88g, Fe in obtained material
0be 1:4 with GO duty factor.
By Fe
0/ GO compound substance is used for Adsorption simulated radioactive nuclein Co
2+, step is as follows: the Co adding 15mL in reactor
2+the Fe of aqueous solution (pH6) and 0.1g/L
0/ GO compound substance, reactor sealing be placed in desk-top constant-temperature shaking incubator and react, rotating speed is 150rpm, and temperature is 20 DEG C.Adsorbance (the q of differential responses time
t) in table 5:
Table 5Fe
0nucleic Co process removed by/GO compound substance
| Time (min) | Initial concentration (mg/L) | Residual concentration (mg/L) | Adsorbance (mg/g) |
| 10 | 10.49 | 6.43 | 20.30 |
| 30 | 10.49 | 5.06 | 27.14 |
| 60 | 10.49 | 4.34 | 30.74 |
| 240 | 10.49 | 3.20 | 36.46 |
| 480 | 10.49 | 3.09 | 37.00 |
| 720 | 10.49 | 3.21 | 33.94 |
| 1440 | 10.49 | 3.42 | 32.88 |
Detection method: with embodiment 1.
In sum, Fe of the present invention
0/ GO compound substance has adsorptive selectivity, its to the maximum equilibrium adsorption capacities of nucleic Co up to 114.08mg/g, experiment condition is gentle, and the particle after absorption has magnetic, easily recovery, volume is little, convenience is temporary, has broad application prospects in the radioactive nuclide in process water.
Claims (5)
1. utilize graphene-supported nano zero-valence iron composite material to remove a method for radiocobalt, it is characterized in that, concrete steps are as follows:
(1) first add in reaction vessel by 1 – 2g expansible graphite, add the concentrated sulphuric acid, the mass ratio of the concentrated sulphuric acid and graphite is 70:1 – 200:1, stirs 10 – 30min in ice-water bath; Slowly add potassium permanganate, the mass ratio of potassium permanganate and graphite is 1.5:1 – 6:1, keeps system temperature to be no more than 15 DEG C; Withdraw from ice-water bath after completion of the reaction, at temperature 34-36 DEG C, constant temperature stirs 3 days; Then divide three times and add deionized water, first time adds 40mL, stirs 30 – 60min at 59-61 DEG C, and second time adds 40mL, keeps 30 – 60min at 89-91 DEG C, and third time directly adds 40mL deionized water; Finally add the H of 30wt%
2o
2, H
2o
2be 4.5:1 – 13.5:1 with the mass ratio of graphite, centrifugal 30min under 10000 – 12000r/min while hot, abandoning supernatant is hydrochloric acid and the distilled water centrifuge washing of 1:10 by volume ratio, obtained graphene oxide, and freeze drying is for subsequent use;
(2) graphene oxide that step (1) is obtained is placed in deionized water, ultrasonic disperse; Add FeSO
47H
2o solution, stirs and passes into argon gas and make it to be in anaerobic state; Then KBH is instilled
4solution, KBH
4solution and FeSO
47H
2the volume ratio of O solution is 1:1 – 2.5:1, and concentration ratio scope is 5:1 – 20:1; Blasting argon gas in course of reaction keeps reaction to carry out under anaerobic state; After reacting 1 – 2h, with deionized water and absolute ethanol washing centrifugal, i.e. obtained graphene-supported nano zero-valence iron composite material after vacuum drying, wherein the mass ratio of Zero-valent Iron and graphene oxide is 1:4 – 4:1;
(3) obtained graphene-supported nano zero-valence iron composite material is joined containing radioactive nuclide
60in the waste water of Co, then constant temperature oscillation.
2. method according to claim 1, is characterized in that, the time of described constant temperature oscillation is 4 – 24h; Temperature is 20 – 30 DEG C.
3. method according to claim 1, is characterized in that, in waste water
60the concentration of Co is 10 – 407mg/L.
4. method according to claim 1, is characterized in that, the pH value of waste water is 4 – 9.
5. method according to claim 1, is characterized in that, the consumption of described graphene-supported nano zero-valence iron composite material is 0.05 – 0.4g/L.
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