CN110097992A - A kind of method that high-strength flour cladding nano zero valence iron removes uranium in nuclear waste - Google Patents
A kind of method that high-strength flour cladding nano zero valence iron removes uranium in nuclear waste Download PDFInfo
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- CN110097992A CN110097992A CN201910382362.4A CN201910382362A CN110097992A CN 110097992 A CN110097992 A CN 110097992A CN 201910382362 A CN201910382362 A CN 201910382362A CN 110097992 A CN110097992 A CN 110097992A
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- 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
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- 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
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Abstract
The present invention relates to the methods of uranium in a kind of high-strength flour cladding nano zero valence iron removal nuclear waste, using high-strength flour as carrier, using liquid phase reduction, NZVI is coated on high-strength flour, prepare a kind of novel composite material-NZVI/ high-strength flour, and the removal for uranyl ion in nuclear waste water, include the following steps: (1), preparation FeCl3Solution；(2), nanometer high-strength flour is prepared；(3), cladding nanometer zeroth order iron powder (NZVI/ high-strength flour) is prepared；(4), the appearance structure of NZVI/ high-strength flour is analyzed；(5), removal effect of the test NZVI/ high-strength flour to uranyl ion in nuclear waste.This method selects high-strength flour cheap and easy to get to coat as stabilizer to nano zero valence iron; due to the protection of wrapping layer; NZVI can be effectively prevented to react with the oxygen in environment; the average grain diameter of coated particle is less than 100nm; dispersity is good, has bigger than simple nano zero valence iron, more effective ratio areas (BET).
Description
Technical field
The present invention relates to nuclear waste water processing and composite material research fields more particularly to a kind of high-strength flour cladding to receive
The method of uranyl ion in rice Zero-valent Iron removal nuclear waste water.
Background technique
The radioactivity with natural radiative nucleic uranium can be generated by adopting in smelting process and nuclear facilities operational process in uranium ore
Waste water can cause great harm environment, it is necessary to could safety dumping after qualification processing.Uranium waste water treatment process is mainly
The uranyl ion in solution is removed, chemical precipitation method is to handle one of the common method of radioactive wastewater, and Zero-valent Iron is this method
One of effective reducing material.Zero-valent Iron is cheap and easy to get, environmental-friendly, can remove nuclear waste water by mechanism such as absorption, precipitate reductions
In uranyl ion.Nano zero valence iron (NZVI) particle as a kind of novel nano material, particle in 100nm hereinafter,
Not only with the characteristic of Zero-valent Iron, but also there are bigger specific surface area, higher reactivity and stronger than common Zero-valent Iron
Adsorptivity can quickly and efficiently remove the heavy metal contaminants in water body and soil, and at low cost.Studies have shown that: molten
Under the conditions of liquid pH value is 4.0, NZVI dosage 1.6g/L, a large amount of U (VI) are reduced to U (IV) deposition removal in solution, as a result
Show: by the reaction of 2h, the removal rate of U (VI) is up to 63.7%.
But nano zero valence iron, since partial size is small and is magnetic, easily oxidation corrosion in air forms the oxidation of passivation
Iron surface is agglomerated into bulky grain.Even if nano zero valence iron also can generate hydrogen by hydrogen ions in the water environment of anaerobism
And ferrous ion, reduce the migration and reactivity in reduction process.It is oxidizable, easy to reunite for nano zero valence iron at present
Limitation, main solution includes cladding process, load method and bimetal modifying method.Above-mentioned NZVI modification technology is most
Using metal material as load, the successful case applied to uranyl ion removal there is no, and the above method can give underground water
Environment and ecosystem bring serious secondary pollution.
Therefore, the purpose of the present invention is to provide a kind of preparation method of new modified nano zero valence iron, at the same this is novel
Material is applied to nuclear waste water process field, solves modified Nano Zero-valent Iron and is also easy to produce two secondary environments in nuclear waste water treatment process
The problem of pollution.
Summary of the invention
The purpose of the present invention is to solve defects of the existing technology, provide a kind of high-strength flour cladding nano zero-valence
The method that iron removes uranium in nuclear waste.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of method that high-strength flour cladding nano zero valence iron removes uranium in nuclear waste, using high-strength flour as carrier, using liquid phase
NZVI is coated on high-strength flour by reduction method, prepares a kind of novel composite material-NZVI/ high-strength flour, and useless for core
The removal of uranyl ion, includes the following steps: in water
(1), FeCl is prepared3Solution；(2), nanometer high-strength flour is prepared；(3), cladding nanometer zeroth order iron powder is prepared
(NZVI/ high-strength flour)；(4), the appearance structure of NZVI/ high-strength flour is analyzed；(5), test NZVI/ high-strength flour is to uranium in nuclear waste
The removal effect of acyl ion.
Further, step (1) prepares FeCl3Solution method particularly includes: take addition 35mL water in 15mL ethyl alcohol, obtain
30% dehydrated alcohol；It measures in the 30% dehydrated alcohol merging conical flask of 50mL, weighs the FeCl of 4.83g3·6 H2O is placed in cone
It is mixed in shape bottle with 30% dehydrated alcohol, is uniformly mixing to obtain FeCl3Solution.
Prepare FeCl3Solution calculation formula are as follows:
m(FeCl3·6H2O)=n (FeCl3·6H2O)/n (Fe) * m (Fe)=270.5g/mol/56g/mol*1g=4.
83g。
Further, step (2) prepares nanometer high-strength flour method particularly includes: weighs 20 grams of common high-strength flours, uses ball milling
Machine grinds 15min, sieves with 100 mesh sieve, obtains a nanometer high-strength flour；It accurately weighs 2g and is added to FeCl3In solution, it is placed in magnetic force and stirs
It mixes and stirs 1h on device.
Further, step (3) prepares cladding nanometer zeroth order iron powder (NZVI/ high-strength flour) method particularly includes: weighs
4.32g KBH4 is configured to 0.8mol/L KBH in the distilled water of 100mL4Solution, and it is slowly added to FeCl3Solution conical flask
In, when addition, persistently stirs, and is accompanied by black foam, stirs 30min, and the nano zero valence iron for obtaining being coated on high-strength flour is molten
Liquid.Nano zero-valence ferrous solution is spent after ionized water and dehydrated alcohol wash 3 times respectively, is dried in 80 DEG C of vacuum ovens
Cladding nanometer zeroth order iron powder.
Wherein, 0.8mol/L KBH is prepared4Solution calculation formula are as follows:
M (kBH4)=0.8mol/L*0.1L*54g/mol=4.32g.
Prepare the chemical reaction process of nano zero valence iron are as follows:
4Fe2++2BH4 -+6H2O→4Fe0+2B(OH)3+7H2
4Fe3++3BH4 -+9H2O→4Fe0+3B(OH)3+6H2+9H+
Further, step (4) analyzes the appearance structure of NZVI/ high-strength flour method particularly includes: after vacuum drying
NZVI/ high-strength flour sticks on objective table, specimen surface spray one layer of golden film, then with S- 520HTACHI type scanning electron microscope into
Row surface of solids pattern and energy spectrum analysis.
NZVI/ high-strength flour particle is characterized through transmission electron microscope, SEM figure show the NZVI partial size after high-strength flour cladding 80~
100nm, it is spherical in shape and dispersed preferable, illustrate that the introducing of covering material can effectively inhibit the reunion of nano zero valence iron, increases
Its big reaction surface area, increases reactivity site.
Further, specific method of step (5) the test NZVI/ high-strength flour to the removal effect of uranyl ion in nuclear waste
Are as follows: it accurately weighs 0.1g NZVI/ high-strength flour and is placed in 250mL conical flask, the U that 100mL mass concentration is 45mg/L is added
(VI) solution, with 0.5mol/L HNO3Or NaOH adjusts solution PH=5.5, is placed in thermostatic control oscillator vibration, in 30 DEG C of rings
To staticly settle after 150r/min rate oscillation 2.0h in border, the residual for taking supernatant spectrophotometry to survey uranium in water phase is dense
Degree, calculates the removal rate of uranium.
Further, test solution pH value goes the influence of uranium effect to NZVI/ high-strength flour: with 0.5mol/L HNO3Or NaOH
U (VI) solution pH value is adjusted, adjusting pH range is 3~6.5, investigates influence of the pH value to removal U (VI).
The invention has the benefit that this method selects high-strength flour cheap and easy to get as stabilizer to nano zero valence iron
It is coated, due to the protection of wrapping layer, can effectively prevent NZVI from reacting with the oxygen in environment, the average grain of coated particle
Diameter is less than 100nm, and dispersity is good, has bigger than simple nano zero valence iron, more effective ratio areas (BET).
Coated particle can be always held at Nano Particle range in the water of anaerobic environment and maintain dispersity, be removed with it
Uranyl ion in nuclear waste water, removal rate are without secondary pollution to underground water and ecological environment up to 96%.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of NZVI/ high-strength flour made from the embodiment of the present invention；
Fig. 2 be in the embodiment of the present invention test solution ph to going uranium effect diagram.
Specific embodiment
The present invention is further described in detail With reference to embodiment, the embodiment provided only for
The present invention is illustrated, the range being not intended to be limiting of the invention.All technologies realized based on above content of the present invention belong to this
The range of invention.
A kind of method that high-strength flour cladding nano zero valence iron removes uranium in nuclear waste, using high-strength flour as carrier, using liquid phase
NZVI is coated on high-strength flour by reduction method, prepares a kind of novel composite material-NZVI/ high-strength flour, and useless for core
The removal of uranyl ion, includes the following steps: in water
(1), FeCl is prepared3Solution；(2), nanometer high-strength flour is prepared；(3), cladding nanometer zeroth order iron powder is prepared
(NZVI/ high-strength flour)；(4), the appearance structure of NZVI/ high-strength flour is analyzed；(5), test NZVI/ high-strength flour is to uranium in nuclear waste
The removal effect of acyl ion.
Further, step (1) prepares FeCl3Solution method particularly includes: take addition 35mL water in 15mL ethyl alcohol, obtain
30% dehydrated alcohol；It measures in the 30% dehydrated alcohol merging conical flask of 50mL, weighs the FeCl of 4.83g3·6H2O is placed in cone
It is mixed in shape bottle with 30% dehydrated alcohol, is uniformly mixing to obtain FeCl3Solution.Prepare FeCl3Solution calculation formula are as follows:
m(FeCl3·6H2O)=n (FeCl3·6H2O)/n (Fe) * m (Fe)=270.5g/mol/56g/mol*1g=
4.83g 。
Further, step (2) prepares nanometer high-strength flour method particularly includes: weighs 20 grams of common high-strength flours, uses ball milling
Machine grinds 15min, sieves with 100 mesh sieve, obtains a nanometer high-strength flour；It accurately weighs 2g and is added to FeCl3In solution, it is placed in magnetic force and stirs
It mixes and stirs 1h on device.
Further, the preparation of NZVI/ high-strength flour: 35mL water is added in accurate measure in 15mL ethyl alcohol, obtain 30% anhydrous second
Alcohol；It measures in the 30% dehydrated alcohol merging conical flask of 50mL, weighs the FeCl of 4.83g36H2O be placed in conical flask with
The mixing of 30% dehydrated alcohol, is uniformly mixing to obtain FeCl3Solution；20 grams of common high-strength flours are weighed, ball mill grinding is used
15min is sieved with 100 mesh sieve, and obtains high-strength flour raw material.It accurately weighs high-strength flour raw material 2g and is added to FeCl3In solution, magnetic force is set
1h is stirred on blender；Weigh 4.32g KBH4In 100mL H20.8mol/L KBH is configured in O4Solution is simultaneously slowly added to
FeCl3In solution conical flask, when addition, is persistently stirred, and is accompanied by black foam, is stirred 30min, is obtained being coated on high-strength flour
On nano zero-valence ferrous solution；Nano zero-valence ferrous solution is spent after ionized water and dehydrated alcohol wash 3 times respectively, true at 80 DEG C
Cladded type NZVI/ high-strength flour powder is dried to obtain in empty drying box.
Wherein, 0.8mol/L KBH is prepared4Solution calculation formula are as follows:
m(KBH4)=0.8mol/L*0.1L*54g/mol=4.32g.
Prepare the chemical reaction process of nano zero valence iron are as follows:
4Fe2++2BH4 -+6H2O→4Fe0+2B(OH)3+7H2
4Fe3++3BH4 -+9H2O→4Fe0+3B(OH)3+6H2+9H+
Further, the structure and pattern of NZVI/ high-strength flour are characterized: the NZVI/ high-strength flour after vacuum drying is glued
In on objective table, one layer of golden film is sprayed in specimen surface, then carries out surface of solids shape with S-520HTACHI type scanning electron microscope
Looks analysis, as shown in Figure 1, SEM figure show the NZVI partial size after high-strength flour cladding in 80~100nm, it is spherical in shape and it is dispersed compared with
It is good, illustrate that the introducing of covering material can effectively inhibit the reunion of nano zero valence iron, increase its reaction surface area, increases anti-
Answer active site.Spherical in shape or elliposoidal, particle dispersity are good.
Further, removal effect of the NZVI/ high-strength flour to uranyl ion in nuclear waste water: 0.1g NZVI/ high muscle is accurately weighed
Powder is placed in 250mL conical flask, U (VI) solution that 100mL mass concentration is 45mg/L is added, with 0.5mol/L HNO3Or
NaOH adjusts solution PH=5.5, is placed in thermostatic control oscillator vibration, with 150r/min rate oscillation 2.0h in 30 DEG C of environment
After staticly settle, take supernatant to be measured.
Step 4, the residual concentration of uranium in water phase, C are surveyed using atomic absorption spectrophotometer0For the initial concentration of uranium
(mg/L), CtFor the concentration (mg/L) of uranium in supernatant.The removal rate R of uranium is calculated according to the following formula:
Further, test solution pH value goes the influence of uranium effect to NZVI/ high-strength flour: with 0.5mol/L HNO3Or NaOH
U (VI) solution pH value is adjusted, adjusting pH range is 3~6.5, investigates influence of the pH value to removal U (VI).As seen from Figure 2:
PH value has apparent influence to removal U (VI), and with the increase of solution pH value, the removal rate of U (VI) increases, as PH > 5.5
Afterwards, the removal rate of U (VI) no longer increases begins to decline instead.When PH is 5.5, optimal U (VI) removal rate 96% is obtained.
This method selects high-strength flour cheap and easy to get to coat as stabilizer to nano zero valence iron, due to wrapping layer
Protection, can effectively prevent NZVI from reacting with the oxygen in environment, the average grain diameter of coated particle is less than 100nm, dispersity
Well, there are bigger than simple nano zero valence iron, more effective ratio areas (BET).Coated particle is in anaerobic environment
It can be always held at Nano Particle range in water and maintain dispersity, remove the uranyl ion in nuclear waste water with it, go
It is without secondary pollution to underground water and ecological environment except rate is up to 96%.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and
Its equivalent defines.
Claims (7)
1. a kind of method of uranium in high-strength flour cladding nano zero valence iron removal nuclear waste, which comprises the steps of:
(1), FeCl is prepared3Solution；(2), nanometer high-strength flour is prepared；(3), cladding nanometer zeroth order iron powder (NZVI/ high is prepared
Strength flour)；(4), the appearance structure of NZVI/ high-strength flour is analyzed；(5), test NZVI/ high-strength flour removes uranyl ion in nuclear waste
Except effect.
2. the method for uranium, feature in a kind of high-strength flour cladding nano zero valence iron removal nuclear waste according to claim 1
It is, step (1) prepares FeCl3Solution method particularly includes: take addition 35mL water in 15mL ethyl alcohol, obtain 30% dehydrated alcohol；Amount
It takes 30% dehydrated alcohol of 50mL to be placed in conical flask, weighs the FeCl of 4.83g3·6 H2O is placed in conical flask and 30% anhydrous second
Alcohol mixing, is uniformly mixing to obtain FeCl3Solution.
3. the method for uranium, feature in a kind of high-strength flour cladding nano zero valence iron removal nuclear waste according to claim 2
It is, step (2) prepares nanometer high-strength flour method particularly includes: weighs 20 grams of common high-strength flours, uses ball mill grinding
15min is sieved with 100 mesh sieve, and obtains a nanometer high-strength flour；It accurately weighs 2g and is added to FeCl3In solution, it is placed on magnetic stirring apparatus and stirs
Mix 1h.
4. the method for uranium, feature in a kind of high-strength flour cladding nano zero valence iron removal nuclear waste according to claim 3
It is, step (3) prepares cladding nanometer zeroth order iron powder (NZVI/ high-strength flour) method particularly includes: weighs 4.32g KBH4
0.8mol/L KBH is configured in the distilled water of 100mL4Solution, and it is slowly added to FeCl3In solution conical flask, when addition, is held
Continuous stirring, is accompanied by black foam, stirs 30min, obtains being coated on the nano zero-valence ferrous solution on high-strength flour;
Nano zero-valence ferrous solution is spent after ionized water and dehydrated alcohol wash 3 times respectively, is dried in 80 DEG C of vacuum ovens
Obtain cladding nanometer zeroth order iron powder.
5. the method for uranium, feature in a kind of high-strength flour cladding nano zero valence iron removal nuclear waste according to claim 4
It is, step (4) analyzes the appearance structure of NZVI/ high-strength flour method particularly includes: glues the NZVI/ high-strength flour after vacuum drying
In on objective table, one layer of golden film is sprayed in specimen surface, then carries out surface of solids shape with S-520HTACHI type scanning electron microscope
Looks analysis.
6. the method for uranium, feature in a kind of high-strength flour cladding nano zero valence iron removal nuclear waste according to claim 5
It is, step (5) tests NZVI/ high-strength flour to the removal effect of uranyl ion in nuclear waste method particularly includes: accurately weighs
0.1g NZVI/ high-strength flour is placed in 250mL conical flask, and U (VI) solution that 100mL mass concentration is 45 mg/L is added, uses
0.5mol/L HNO3Or NaOH adjusts solution PH=5.5, is placed in thermostatic control oscillator vibration, with 150 r/ in 30 DEG C of environment
It is staticly settled after 2.0 h of min rate oscillation, takes supernatant spectrophotometry to survey the residual concentration of uranium in water phase, calculate uranium
Removal rate.
7. the method for uranium, feature in a kind of high-strength flour cladding nano zero valence iron removal nuclear waste according to claim 6
It is, test solution pH value goes the influence of uranium effect to NZVI/ high-strength flour: with 0.5 mol/L HNO3Or NaOH adjusts U (VI)
Solution pH value, adjusting pH range is 3~6.5, investigates influence of the pH value to removal U (VI).
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