CN113707351B - Static uranium removal method for sponge iron filter material - Google Patents
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- CN113707351B CN113707351B CN202011331224.2A CN202011331224A CN113707351B CN 113707351 B CN113707351 B CN 113707351B CN 202011331224 A CN202011331224 A CN 202011331224A CN 113707351 B CN113707351 B CN 113707351B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 269
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 153
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 151
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 123
- 239000000463 material Substances 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 50
- 230000003068 static effect Effects 0.000 title claims abstract description 7
- 238000011282 treatment Methods 0.000 claims abstract description 93
- 239000002351 wastewater Substances 0.000 claims abstract description 83
- 230000008569 process Effects 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 22
- 238000011221 initial treatment Methods 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 5
- 238000007781 pre-processing Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 45
- 230000000694 effects Effects 0.000 abstract description 37
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 27
- 230000035484 reaction time Effects 0.000 description 15
- 238000001179 sorption measurement Methods 0.000 description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 238000000227 grinding Methods 0.000 description 9
- 239000003344 environmental pollutant Substances 0.000 description 8
- 231100000719 pollutant Toxicity 0.000 description 8
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 238000005189 flocculation Methods 0.000 description 5
- 238000012423 maintenance Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 230000005465 channeling Effects 0.000 description 4
- 230000016615 flocculation Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000033116 oxidation-reduction process Effects 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- -1 uranium ions Chemical class 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 235000014413 iron hydroxide Nutrition 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000002354 radioactive wastewater Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010786 composite waste Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical class [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036647 reaction Effects 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/10—Processing by flocculation
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/20—Disposal of liquid waste
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Environmental & Geological Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a static uranium removal method for a sponge iron filter material. The sponge iron filter material has multiple synergistic effects in the treatment of uranium-containing wastewater, has obvious treatment effect, wide sources of reaction materials and low cost, adopts graded treatment in the treatment process, obviously improves the uranium removal effect, has simple process and is more suitable for industrial application compared with the prior art.
Description
Technical Field
The invention belongs to the technical field of radioactive wastewater treatment, and particularly relates to a method for treating uranium-containing wastewater by using a sponge iron filter material.
Background
Uranium is the most main nuclear fuel in the current nuclear energy utilization, and along with the rapid development of nuclear energy, the increase of uranium resource demand and the scale expansion of uranium mining and smelting will produce more low-concentration uranium polluted wastewater.
Uranium mining and dressing will produce a large amount of wastewater at low radioactivity levels. These include pit waste water, tailings water, leaching weathered waste water, which can form composite waste water, and in addition to containing radioactive elements, also toxic and harmful substances such as cadmium, manganese, zinc, chromium, lead, sulfate radical, etc. Once the wastewater enters soil and underground water, the wastewater can pollute the soil, water resources and ecological environment in the tailing pond area and the surrounding area, and seriously endanger human health. Therefore, the treatment of uranium-containing wastewater is particularly important, and is receiving a great deal of attention. The traditional methods mainly comprise chemical precipitation, ion exchange, membrane method, oxidation-reduction method, evaporation concentration and adsorption method, and the methods have the defects of different degrees in the actual operation process, such as long treatment period, low removal efficiency, high cost, large secondary waste amount and the like.
In the new technology developed in recent years, the diffusion of pollutants can be fundamentally prevented by directly constructing treatment engineering in the underground aquifer of the reservoir zone leakage zone to treat the leakage water in situ. In this respect, the Permeable Reactive Barrier (PRB) treatment technology can continuously treat pollutants in situ for a long time, has the advantages of multiple components, good treatment effect, relatively low cost, small influence on ecological environment, strong practicability and very good application prospect in industry.
In practical application, the wall body reaction material has a direct influence on the treatment effect of wastewater, so that the reaction material is a key of the treatment effect of pollutants by the carburization reaction wall. The factors such as the adsorption or degradation capacity of the reaction material to pollutants, stability, hydraulic conductivity, environmental compatibility and price are considered when the PRB reaction medium is selected.
Among them, zero-valent iron is the most commonly used permeable reactive barrier reaction material, and has good effects on pollutants such as radionuclide uranium and harmful heavy metals. The zero-valent iron is cheap and easy to obtain, is environment-friendly, can remove various heavy metals in water through mechanisms such as adsorption, reduction, precipitation and the like, and is particularly suitable for the advanced treatment of low-concentration radioactive wastewater. However, in the current practical application process, substances such as iron oxide, indissoluble salt and the like are precipitated in the pores of the reaction wall body and on the surface of the zero-valent iron, so that the reaction wall body is blocked, channeling is generated, the treatment efficiency and effect are reduced, the activity of the zero-valent iron is reduced, and the service life of the zero-valent iron is shortened.
Therefore, there is a strong need for a uranium-containing wastewater treatment method, in which the reaction material has stable reactivity and a wide source, and uranium in the wastewater can be stably removed for a long period of time by using the method.
Disclosure of Invention
In order to solve the problems, the inventor has conducted intensive studies and provides a method for treating uranium-containing wastewater by using an active sponge iron filter material, which reduces uranium ions by using sponge iron, and micro-electrolyzes, adsorbs and precipitates uranium-containing substances by using iron hydroxide and the like cooperatively produced by a special structure of the sponge iron, thereby greatly reducing the content of uranium in the wastewater. The concentration of the uranium in the wastewater treated by the method can meet the wastewater discharge requirement. Moreover, the sponge iron is used as a reaction material to treat wastewater, so that the activity is stable, the service life is long, and the requirements of actual industry can be met.
The invention aims to provide a static uranium removal method for a sponge iron filter material, which utilizes the classification treatment of the sponge iron filter material to remove uranium in wastewater.
The method specifically comprises the following steps:
Step 1, preprocessing sponge iron filter materials;
Step 2, regulating the pH value of uranium-containing wastewater to obtain a liquid to be treated;
step 3, adding the sponge iron filter material into the liquid to be treated, and treating to obtain a mixed liquid;
and step 4, filtering the mixed solution to obtain a treatment solution.
Preferably, in the step 3, the uranium-containing wastewater is subjected to classification treatment, which specifically comprises the following steps:
Step 3-1, performing primary treatment to obtain primary treatment liquid;
The primary treatment is deoxidization treatment;
step 3-2, performing secondary treatment on the primary treatment liquid to obtain a mixed liquid;
The secondary treatment is uranium removal treatment.
The invention provides a static uranium removal method for sponge iron filter materials, which has the following beneficial effects:
(1) The invention utilizes the sponge iron to treat uranium-containing wastewater, has various synergistic treatment effects, improves the treatment effect of the wastewater, and reduces the consumption of reaction materials.
(2) The sponge iron in the invention utilizes the self-supporting and porous structure, the surface activity is improved, the ferric hydroxide and the flocculent ferrous hydroxide generated during the treatment of uranium-containing wastewater are enhanced due to the structure of the sponge iron, the adsorption capacity is enhanced, and the functions of micro-electric fields and the like exist in the sponge iron, so that the efficient utilization of the reaction materials is realized.
(3) The uranium-containing wastewater is treated by using sponge iron as a reaction material, so that the problems of blockage, channeling, treatment efficiency and activity reduction and the like caused by using common iron powder and other zero-valent iron can be avoided, the service life of the reaction material is prolonged, and the maintenance cost is reduced.
(4) According to the invention, the uranium-containing wastewater is treated in a grading manner by using the sponge iron, so that dissolved oxygen in the wastewater is removed first, and then uranium is removed, thereby achieving a better removal effect.
(5) The reaction material in the invention has strong practicability in actual uranium-containing wastewater, has better treatment effect in neutral wastewater, has good treatment effect on low-concentration uranium-containing wastewater, and has good application prospect.
Drawings
FIG. 1 shows a graph of the concentration variation of simulated uranium wastewater treated with different initial concentrations in example 2 of the present invention;
FIG. 2 shows a graph of the concentration variation of simulated uranium wastewater treated at different temperatures in example 3 of the present invention;
FIG. 3 is a graph showing the concentration change of simulated uranium wastewater treated with the reaction materials of example 4 according to the present invention at different pH values;
FIG. 4 shows the effect of reactant particle size on treatment of simulated uranium wastewater in example 5 of the present invention.
Detailed Description
The features and advantages of the present invention will become more apparent and evident from the following detailed description of the invention.
According to the invention, the uranium in the wastewater is removed by utilizing the sponge iron filter material, hexavalent uranium U (VI) in the uranium-containing wastewater can be reduced, and the sponge iron has a special spongy porous structure, is in a soft flocculent state in the solution, adsorbs uranium-containing substances, and has a good uranium removal effect. The process method is simple and easy to implement, the sponge iron is used as a reaction material, the performance can be kept stable, the influence of sediment is weakened, the service life is long, and the uranium removal effect is obvious.
The invention provides a static uranium removal method for a sponge iron filter material, which utilizes the classification treatment of the sponge iron filter material and specifically comprises the following steps:
Step 1, preprocessing sponge iron filter materials;
at present, in practical application, the infiltration reaction wall system is easy to cause the activity reduction of the reaction material and even cause wall blockage due to long-term operation and deposition of attachments in the pores of the reaction wall and on the surface of the reaction material. The zero-valent iron in the existing reaction materials is more in application, for example, common iron powder is used, in the practical application process, the oxide, calcium carbonate and sulfide of the iron are easy to deposit on the surface of the zero-valent iron, even organic matters can be deposited, the effectiveness and activity of the zero-valent iron are greatly reduced, and the service life of the zero-valent iron is short. The common zero-valent iron is used for constructing the permeable reactive barrier, frequent maintenance is needed, continuous treatment of uranium-containing wastewater can not be realized, and the maintenance cost is high.
The sponge iron filter material is prepared from concentrated ore powder and ferric oxide through grinding, magnetic separation, high-temperature sintering, cooling, washing, crushing, magnetic separation again and screening to obtain low-cost porous granular material, which is black and bright in appearance, is in a loose sponge shape and is an alloy consisting of iron, carbon and other impurities (Mn, cr, ni, caO, mgO and the like). The sponge iron filter material is internally provided with a large number of micro-pores, is similar to a sponge when observed under a microscope, can keep the reactivity in a quite long time when being used as a reaction material, keeps the dredging property, and avoids the problems of poor treatment effect, reduced treatment water quantity, frequent maintenance, high cost, incapability of continuous treatment and the like caused by the phenomena of deactivation, blockage, channeling and the like which are easily generated by using common iron powder in practical application.
The sponge iron filter material is required to be crushed and ground before being used, the crushing and grinding methods are not particularly limited in the invention, and the particle size of the sponge iron filter material can meet the use requirements, such as manual grinding, ball milling and the like.
The average particle size of the sponge iron filter material is 0.5-12mm, preferably 1-8mm, more preferably 1-2mm. According to the invention, a large number of experiments show that the smaller the particle size of the sponge iron is, the reaction can be carried out towards the direction favorable for reducing U (VI) of hexavalent uranium, and the better the treatment effect is; however, when the particle size is smaller than 1.00mm, especially smaller than 0.5mm, the resistance is too large and is easy to agglomerate in the running process, channeling is generated, and the long-time running affects the water outlet effect and the wastewater treatment capacity.
The sponge iron filter material contains iron, iron carbon compounds and the like, and also contains some impurities with fine particles dispersed in the sponge iron, and because the electrode potential of the impurities is lower than that of the iron, when the sponge iron filter material is in uranium-containing wastewater, countless micro cells can be formed to reduce high-valence uranium ions in the wastewater.
The iron ions generated in the oxidation-reduction process further form hydrate, so that the adsorption capacity of the sponge iron is further enhanced by the strong adsorption flocculation activity and the special loose and porous structure of the sponge iron. Therefore, the sponge ferroelectric has strong chemical adsorption and physical adsorption capability, and also has the advantages of better oxidation-reduction capability and flocculation precipitation. More importantly, the self-cleaning can be realized by utilizing the supporting and porous micropore structures of the sponge iron, the reactivity is improved, the environmental water pressure and the like can be utilized to a certain extent, the process requirements are met, the treatment capacity is increased, and the service life of the reaction material is prolonged. And further, the continuity treatment is realized, and the maintenance cost is greatly reduced.
According to the invention, the uranium-containing wastewater is treated by using the sponge iron as the reaction material, hexavalent uranium can be reduced, the precipitation capacity of uranium is enhanced, and meanwhile, the uranium is fixed in the sponge iron by using the adsorption flocculation effect of the sponge iron.
Step 2, regulating the pH value of uranium-containing wastewater to obtain a liquid to be treated;
The uranium-containing wastewater is industrial uranium-containing wastewater or artificial uranium-containing wastewater. The uranium-containing wastewater has a uranium concentration of not more than 100mg/L, preferably not more than 20mg/L, more preferably not more than 15mg/L.
After the pH value is adjusted, the pH value of the uranium-containing wastewater is 2-10, preferably 4-8.5, and more preferably 7-7.5.
It is presumed that in practical application, sponge iron is used as a primary cell, the iron element of the anode loses electrons to form ferrous iron Fe (II) into solution, and H + in the solution is reduced to H 2 on the surface of the carbon element serving as a cathode. Fe (II) entering the solution is used as a reducing agent to react with U (VI) in the solution, so that the U (VI) is reduced to U (IV), and part of Fe (II) is oxidized to ferric Fe (III). Along with the continuous consumption of H + in the reaction, the pH value is increased, fe (II) generated by oxidation of sponge iron forms Fe (II) or Fe (III) oxide and hydroxide, wherein Fe (OH) 3 and Fe (OH) 2 have strong adsorption-flocculation activity, and a large amount of tiny particles, metal ions and organic macromolecules dispersed in wastewater can be adsorbed to be flocculated and precipitated, and meanwhile, the oxides and the hydroxides are adsorbed on the surface of the sponge iron.
A large number of experiments prove that the smaller the pH value is, the better the treatment effect of the sponge iron filter material is. However, in actual operation, the influence of the pH value on uranium removal is various, when the pH value is less than 4, the acid consumption and the sponge iron consumption are increased, so that the treatment cost is increased, the content of Fe 2+ in water is increased, the color of the water is deepened, the subsequent treatment is needed, and in addition, the corrosion problem of equipment and pipelines exists; when the pH value is more than 10, the generation and sedimentation of iron hydroxide and oxide are accelerated due to the enhanced alkalinity of the environment, the reactivity of the sponge iron is reduced, and the service life of the reaction material is shortened. And the pH value of the wastewater treated by the sponge iron is increased, and the acidity is weakened.
Step 3, adding the sponge iron filter material into the liquid to be treated, and treating to obtain a mixed liquid;
in one embodiment of the invention, the sponge iron filter material is added into the liquid to be treated, so that the sponge iron filter material fully reacts and contacts with uranium-containing wastewater, and uranium-containing substances are adsorbed and settled in the reaction material.
The mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (0.01-10) g/100 mL, preferably (0.05-8) g/100 mL, and more preferably (0.1-6) g/100 mL. In the specific application, the dosage of the sponge iron filter material is adjusted according to the concentration of uranium-containing wastewater.
In a preferred embodiment of the invention, when the concentration of the uranium-containing wastewater is more than 50mg/L, the mass-volume ratio of the sponge iron filter material to the uranium-containing wastewater is (5-10) g/100 mL; when the concentration of the uranium-containing wastewater is 5-50mg/L, the mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (1-5) g to 100mL; when the concentration of the uranium-containing wastewater is less than 5mg/L, the mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (0.1-1) g to 100mL.
The treatment temperature is 10-65 ℃, preferably 30-60 ℃, more preferably 40-55 ℃. The invention utilizes the sponge iron filter material to remove uranium, and the removing process is a comprehensive treatment process integrating the synergistic effects of adsorption, primary cell reaction, interface reduction, flocculation precipitation and the like, so that the temperature is a relatively complex influencing factor in the removing process, for example, the temperature rise is favorable for the occurrence of the interface reaction, but the temperature rise is unfavorable for the adsorption process. The sponge iron filter material can treat wastewater in a wider temperature range, and can meet the requirements in practical application. The comprehensive treatment capacity of the sponge iron filter material can be improved by properly increasing the temperature.
In the present invention, the reaction time is not particularly limited, and the reaction time is preferably 1 hour or more as long as the treatment liquid reaches 0.3mg/L or less.
In a preferred mode of the invention, the uranium-containing wastewater is preferably subjected to classification treatment, and the method specifically comprises the following steps:
Step 3-1, performing primary treatment to obtain primary treatment liquid;
in the invention, the sponge iron filter material can also react with the dissolved oxygen in the uranium-containing wastewater while removing uranium, and the dissolved oxygen and the uranium in the wastewater have a competition phenomenon during the contact reaction, so that the dissolved oxygen and the sponge iron are easier to react, and therefore, the classification design is carried out during the treatment of the uranium-containing wastewater.
The first-stage treatment is deoxidization treatment, and uranium-containing wastewater is firstly mixed and contacted with a first-stage sponge iron filter material, so that oxygen in the uranium-containing wastewater is mainly removed.
The primary treatment also comprises secondary grading treatment, namely the deoxidation process is carried out in a primary secondary mode or is divided into multiple stages of secondary modes which are sequentially treated, wherein the secondary grades are 1-5 stages, preferably 1-3 stages. After each stage of secondary grading treatment, separating the sponge iron filter material and uranium-containing wastewater, and then carrying out next stage of grading treatment.
The particle size of the sponge iron filter material is 3-15mm, preferably 5-8mm, the deoxidizing treatment temperature is 10-60 ℃, preferably 15-35 ℃, more preferably 20-30 ℃, such as 25 ℃, and the mass volume ratio of the sponge iron filter material to uranium-containing wastewater is 5g (40-150) mL, preferably 5g (80-100) mL.
And 3-2, performing secondary treatment on the primary treatment liquid to obtain a mixed liquid.
After the uranium-containing wastewater is subjected to deoxidization treatment, the interference of oxygen in the uranium-containing wastewater on the uranium removal process is eliminated, so that the uranium removal effect can be improved, the treatment time is shortened, and the uranium removal rate is improved.
The secondary treatment is uranium removal treatment, which comprises secondary classification treatment, namely the uranium removal process can be carried out in a primary secondary mode or is divided into multiple stages of secondary modes which are sequentially treated, wherein the secondary classification is 1-5 stages, preferably 1-3 stages. After each stage of secondary grading treatment, separating the sponge iron filter material and uranium-containing wastewater, and then carrying out next stage of grading treatment.
In step 3-2, the treatment temperature is 10 to 65 ℃, preferably 30 to 60 ℃, more preferably 40 to 55 ℃. The average grain diameter of the sponge iron filtering material is 0.5-12mm, preferably 3-8mm. The mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (0.01-10) g/100 mL, preferably (1-8) g/100 mL, and more preferably (2-6) g/100 mL.
In a preferred mode of the invention, the particle size of the sponge iron filter material is 5-8mm, the uranium removal treatment temperature is 25 ℃, and the mass-volume ratio of the sponge iron filter material to the primary treatment liquid is 5g/100mL.
And step 4, filtering the mixed solution to obtain a treatment solution.
And after the treatment is finished, filtering the mixed solution to obtain a uranium-containing sponge iron filter material and a purified treatment solution.
The invention uses the sponge iron filter material to have multiple synergistic effects when treating uranium-containing wastewater, has obvious treatment effect, wide sponge iron sources, common commercial sources and low cost, and in addition, the invention designs the grading treatment to remove dissolved oxygen first and then uranium, thereby obviously improving the treatment effect, having simple process and being more suitable for industrial application compared with the prior art.
Examples
The sponge iron filter material used in the invention has the following performance indexes:
Iron content%: 96-97%;
Metal iron content: more than or equal to 90 percent;
Carbon and impurities: 3 to 4 percent;
density: 2.3-2.7 g/cm 3;
Bulk density: 1.7-1.88 g/cm 3.
Example 1
Uranium solutions with uranium concentrations of 10.7mg/L, 20mg/L, 42mg/L, 83mg/L and 100mg/L are respectively prepared, and the pH value of the uranium solution is in the range of 7.0-7.5.
100ML of the uranium solution is respectively taken and placed in a 250mL grinding conical flask, 5g of sponge iron is added, and then the mixture is placed in a constant-temperature oscillator with the rotating speed of 260r/min and the temperature of 25 ℃ for 60min to form a mixed solution. Wherein the particle size of the sponge iron is 5-8mm.
After the reaction is finished, sponge iron is filtered out, the filtrate is analyzed by ICP-MS, and in the analysis process, if the concentration of the water sample is too high, the water sample is diluted and then analyzed. The analysis results are shown in Table 1.
TABLE 1 concentration and removal rate of uranium solution after reaction adsorption
As can be seen from table 1, the removal rate of uranium in the uranium solution with low concentration of 10mg/L reaches 92.5% after 60min of reaction adsorption of sponge iron, the concentration of uranium is reduced to 0.75mg/L, and the emission standard is completely satisfied (according to the standard GB 23727-2009 uranium smelting radiation protection and environmental protection regulations, the emission standard of uranium (U) is 0.3 mg/L). The sponge iron has good effect of removing the uranium solution with low concentration.
Example 2
Uranium solutions with uranium concentrations of 10.7mg/L, 20mg/L and 42mg/L are prepared respectively, so that the pH value of the uranium solution is in the range of 7.0-7.5.
Respectively taking 100mL of the uranium solution, placing the uranium solution into a 250mL grinding conical flask, adding 5g of sponge iron, placing the mixture into a constant-temperature oscillator with the rotating speed of 260r/min and the temperature of 25 ℃ to ensure that the contact reaction time is respectively 10min, 20min, 40min and 60min, and forming mixed solution. Wherein the particle size of the sponge iron is 5-8mm.
After the contact reaction time is reached, part of the mixed solution is taken out in batches, sponge iron is filtered out, the filtrate is analyzed by ICP-MS, and in the analysis process, if the concentration of the water sample is too high, the water sample is diluted and then analyzed. The analysis results are shown in FIG. 1.
As can be seen from fig. 1, the lower the initial concentration of uranium, the better the treatment effect. It is presumed that the uranium wastewater treated by sponge iron has a surface adsorption reaction process, and pollutants are adsorbed on the surface of the sponge iron and then reduced, adsorbed, flocculated and deposited, and the treatment process is controlled by the adsorption and the surface reaction. Under the condition that the using amount of the sponge iron is unchanged, the higher the uranium-containing wastewater concentration is, the probability that pollutant molecules are combined to the surface of the sponge iron and react is reduced, and the worse the treatment effect is.
Example 3
Preparing uranium solution with uranium concentration of 100mg/L, and the pH value of the uranium solution is 7.03.
100ML of the uranium solution is taken and placed in a 250mL grinding conical flask, 5g of sponge iron is added, and then the mixture is placed in a constant temperature oscillator with the rotating speed of 260r/min and the temperature of 25 ℃, 35 ℃, 45 ℃ and 55 ℃ respectively, and the contact reaction time is 60min, so that a mixed solution is formed. Wherein the particle size of the sponge iron is 5-8mm.
After reaching the contact reaction time, sponge iron is filtered, the filtrate is analyzed by ICP-MS, and in the analysis process, if the concentration of a water sample is too high, the water sample is diluted and then analyzed, and the graph of the concentration C of the uranium solution after treatment and the reaction time t is shown in figure 2.
In the experiment, the reaction temperatures were 25℃and 35℃and 45℃and 55℃respectively. As can be seen from FIG. 2, when the water temperature of the wastewater is increased during uranium wastewater treatment by the sponge iron, the reaction rate is increased, and the removal rate of pollutants is correspondingly increased.
Fitting a curve of the treated uranium solution concentration C and the reaction time T, and performing a relational equation of a reaction rate constant (k) and a temperature (T): lgk = 1.197 x 10 3/t+ 2.8787, where the reaction rate constant and apparent activation energy are macroscopic reaction kinetic parameters, where the correlation coefficient is 0.8449. The equation basically accords with the Arrhenius equation form, and the activation energy Ea is 22.88kJ/mol.
Example 4
Uranium solutions with uranium concentration of 100mg/L are prepared, and the pH values of the uranium solutions are adjusted to be 2.00, 3.05, 3.97, 5.05, 5.93, 7.01, 8.08 and 9.04 respectively.
100ML of the uranium solution is taken and placed in a 250mL grinding conical flask, 5g of sponge iron is added, and then the mixture is placed in a constant-temperature oscillator with the rotating speed of 260r/min and the temperature of 25 ℃ to ensure that the contact reaction time is 60min, so as to form a mixed solution. Wherein the particle size of the sponge iron is 5-8mm.
After reaching the contact reaction time, sponge iron is filtered, the filtrate is analyzed by ICP-MS, and in the analysis process, if the concentration of the water sample is too high, the water sample is diluted and then analyzed, and the test results are shown in Table 2 and FIG. 3. From the analysis results, the uranium solution concentration after treatment is lower when the pH value is less than 6.
TABLE 2 analysis results after uranium removal at different pH values
From the above data, it can be seen that the lower the pH the lower the uranium solution concentration after treatment. However, in practical application, the influence of the pH value is various, and when the pH value is less than 4, the acid consumption and the consumption of reaction materials are increased, so that the treatment cost is increased, the content of Fe 2+ in water is increased, the color of the water is deepened, the subsequent treatment is needed, and in addition, the corrosion problem of equipment and pipelines is also caused. The actual pH value of uranium ore water to be treated is 7-7.5, and mine tail water can be treated through multiple stages.
Example 5
Two uranium solution concentration levels of 5mg/L and 100mg/L are respectively configured, and the pH value is 7.7-8.0.
Respectively taking sponge iron with particle size ranges of 2.0mm-2.5mm, 1.5mm-2.0mm, 1.0mm-1.5mm and 0.5mm-1.0mm for experiment, wherein the contact reaction time of the sponge iron with the particle size ranges is set to be 60min during the experiment; when the original uranium concentration is 100mg/L, taking 100mL uranium solution, and adding 5g of sponge iron; when the uranium concentration of the stock solution is 5mg/L or less, 0.1g of sponge iron is added. The oscillation speed was 260r/min and the reaction temperature was 25 ℃.
After the treatment, the uranium solution concentration C and the oxidation-reduction potential Eh were measured, and the test results are shown in table 3 and fig. 4. Experimental results show that the smaller the particle size of the sponge iron, the larger the surface area provided by the unit reaction volume, the higher the total surface energy, the reaction can be carried out towards the direction favorable for U (VI) reduction, and the better the treatment effect is. However, when the particle size is smaller than 1.00mm, the filter material is easy to agglomerate without the assistance of external force, and in practical application, the water outlet effect and the water yield can be influenced after long-time use.
TABLE 3 treatment effect data of sponge iron of different particle size ranges
Example 6
Preparing uranium solution with uranium concentration of 100mg/L, wherein the pH value of the uranium solution is 7.03, and the dissolved oxygen is 8mg/L.
100ML of the uranium solution is taken and placed in a 250mL grinding conical flask, 5g of sponge iron is added, and then the mixture is placed in a constant-temperature oscillator with the rotating speed of 260r/min and the temperature of 25 ℃ for primary treatment to remove dissolved oxygen, the contact reaction time is 60min, and after the contact reaction time is reached, the sponge iron is filtered out, so that primary treatment liquid is obtained. Wherein the particle size of the sponge iron is 5-8mm.
And (3) analyzing the primary treatment liquid by utilizing ICP-MS, and if the concentration of the water sample is too high in the analysis process, firstly diluting and then analyzing to obtain the uranium concentration in the primary treatment liquid is 42mg/L and the dissolved oxygen is 0.2mg/L.
The primary treatment liquid is placed in a 250ml grinding conical flask, 5g of sponge iron is added, and secondary treatment is carried out. And (3) placing the conical flask in a constant-temperature oscillator with the rotating speed of 260r/min and the temperature of 25 ℃ for secondary treatment to remove uranium, and obtaining the mixed solution after the contact reaction time of 60 min. Wherein the particle size of the sponge iron is 5-8mm.
After the contact reaction time was reached, sponge iron was filtered, and the obtained filtrate was analyzed by ICP-MS, and the uranium concentration was 16mg/L.
The present invention has been described in detail in connection with the detailed description and/or the exemplary examples and the accompanying drawings, but the description is not to be construed as limiting the invention. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, and these fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (5)
1. The static uranium removal method for the sponge iron filter material is characterized by utilizing the classification treatment of the sponge iron filter material to remove uranium in wastewater;
the method comprises the following steps:
Step 1, preprocessing sponge iron filter materials;
step 2, regulating the pH value of uranium-containing wastewater to be 4-8.5 to obtain a liquid to be treated;
step 3, adding the sponge iron filter material into the liquid to be treated, and treating to obtain a mixed liquid;
Step 4, filtering the mixed solution to obtain a treatment solution;
in the step 3, when the concentration of the uranium-containing wastewater is more than 50mg/L, the mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (5-10) g to 100mL; when the concentration of the uranium-containing wastewater is 5-50mg/L, the mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (1-5) g to 100mL; when the concentration of the uranium-containing wastewater is less than 5mg/L, the mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (0.1-1) g to 100mL;
In the step 3, uranium-containing wastewater is subjected to grading treatment, and the method specifically comprises the following steps:
Step 3-1, performing primary treatment to obtain primary treatment liquid,
The primary treatment is deoxidization treatment, the particle size of the sponge iron filter material is 5-8mm, the deoxidization treatment temperature is 15-35 ℃, and the mass volume ratio of the sponge iron filter material to uranium-containing wastewater is 5g (80-100) mL;
step 3-2, performing secondary treatment on the primary treatment liquid to obtain mixed liquid,
The secondary treatment is uranium removal treatment, the treatment temperature is 30-60 ℃, and the average particle size of the sponge iron filter material is 3-8mm.
2. The method according to claim 1, wherein, in step 3-1,
The deoxidization treatment temperature is 20-30 ℃.
3. The method according to claim 1, wherein, in step 3-2,
The mass volume ratio of the sponge iron filter material to the uranium-containing wastewater is (0.01-10) g/100 mL.
4. The method according to claim 1, wherein in the step 3-2, the particle size of the sponge iron filter material is 5-8mm, and the deoxidizing treatment temperature is 25 ℃.
5. The method according to claim 1, wherein, in step 3,
The primary treatment also comprises secondary grading treatment, namely the deoxidation process is carried out in a primary secondary mode or is divided into multiple stages of secondary modes which are sequentially treated, and the secondary grades are 1-5 grades;
The secondary treatment comprises secondary grading treatment, namely the uranium removal process can be completed in a primary grade or is completed in a multi-grade secondary grade in sequence, and the secondary grade is 1-5 grade.
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