CN103886925B - Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid - Google Patents
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid Download PDFInfo
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Abstract
The invention discloses uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid, first by the acid acidifying of hex Alkali absorption liquid waste liquid, regulate pH=2.7 ~ 5.5, add polymeric sorbent polystyrene Cyclohexylamino maleic acid and complete UO2 2+Absorption, solid-liquid separation by gained solid with 1 more than M acid desorption realize UO2 2+Recovery, surplus solution add Na2CO3Carry out the drip washing of subsequent cycle hex, in time circulating more than 5 times, rich in the F of high concentration in solution‑.Adding NaCl in solution makes NaF separate out because dissolubility reduces to saturated, NaF solid is recovered by filtration to obtain, adds CaCl in solution2, CaO or Ca (OH)2Solid or its saturated solution make the F of residual‑Form CaF2Precipitation, degree of depth fluorine removal.Finally achieve uranium and the recovery of a large amount of fluorine in uranic hexafluoride gas Alkali absorption liquid waste liquid.Present invention achieves the recovery of uranium in radioactive liquid waste and the zero-emission of waste liquid, make the discharge of waste liquid be up to state standards, solve the problem that in tradition defluorinating process, a large amount of calcium fluoride are difficult to filter simultaneously.
Description
Technical field
The present invention relates to recovery and the sewage disposal of a kind of radioelement uranium, be specifically related to uranic hexafluoride gas Alkali absorption
In liquid waste liquid, uranium and the recovery method of fluorine, belong to nuclear fuel and reclaim field and field of hydrometallurgy.
Background technology
Hex is a kind of active, material that respond is the strongest, is white solid under normal conditions, easily waves
Sending out, sublimation temperature is 56.54 DEG C, is currently the only the most stable but also has maximum volatile uranium compound.As
Important intermediate in nuclear fuel production process, is also that the currently the only gas centrifuges that can be used for extracts235The uranium compound of U.
In hex, fluorine atom can be replaced by other electronegative atom parts or replace completely, as there is F/O(fluorine and oxygen) displacement is instead
Should, generate oxyfluoride.The most most typical reaction is the hydrolysis of hex:
Vapor phase hydrolysis: UF6 + 3 H2O → UO2F2 •H2O + 4 HF
Liquid HF hydrolyzes: UF6 + n H2O → UOnF6-2n + 2n HF (n = 1~2)
The hydrolysis of hex is the sensitiveest, causes containing a lot of uranium in the waste material produced in its production process,
It addition, easily leak during gas conveying, canned and a large amount of storages etc., process for radioactive liquid waste and propose a difficult problem.
The most domestic have center group 504,404, four or three hex manufacturers of Aug. 1st, all with 5% ~ 10% sodium carbonate
Solution, as leacheate, carries out purified treatment to uranium-bearing, fluorine tail gas.Containing uranium 30 more than mg/L in this leacheate, must add a large amount of
Tap water dilution could meet existing metallic uranium recovery process and process requirement, processes through absorption, extraction, back extraction, neutralization precipitation
Rear waste liquid reaches to arrange outside discharging standards, and this makes last discharging of waste liquid amount be greatly increased, and process is loaded down with trivial details, and expense is relatively
Height, result is undesirable (to be seen: Zhang Xilin, uranium-bearing, fluorine tail gas drip washing and leacheate regeneration technology research, small-sized circulation warp
Ji scientific seminar paper compilation, 2009,182-196).
Summary of the invention
The technical problem to be solved in the present invention is to overcome existing defect, it is provided that one can realize Zero discharge and one-tenth
Uranium and the recovery method of fluorine in this low hex Alkali absorption liquid waste liquid.
The purpose of the present invention implements by the following technical programs:
In hex Alkali absorption liquid waste liquid, uranium and the recovery method of fluorine, comprise the steps:
Step one, acidifying:
Acid adding in uranic hexafluoride gas Alkali absorption liquid waste liquid, regulates pH=2.7 ~ 5.5, obtains containing UO2 2+、Na+、F-
With Cl-Solution;Concrete reaction equation is as follows:
UF6 + 2 H2O + 2 H+→ UO2 2+ + 6 HF
[UO2(CO3)n]2-2n + 2n H+ → UO2 2+ + n H2O + n CO2 ↑ (n = 1 ~ 4)
Na2CO3 + 2 H+ → 2 Na+ + H2O + CO2 ↑
Step 2, UO2 2+Recovery
a. UO2 2+Absorption
In the solution that step one obtains, add polymeric sorbent polystyrene-Cyclohexylamino maleic acid, stir 10
More than min, the now UO in solution2 2+Adsorption equilibrium, filters isolated UO2 2+-polystyrene-Cyclohexylamino maleic acid is joined
Compound solid and Na+、F-With Cl-Solution, after separation in solution the surplus of uranium less than 0.05 ppm, adsorption rate reach 99% with
On, the solution after solid-liquid separation adds Na2CO3After carry out the drip washing of subsequent cycle hex, when circulating more than 5 times, obtain
F rich in high concentration-Solution;
b. UO2 2+Desorption
Toward UO2 2+-polystyrene-Cyclohexylamino maleic acid coordination compound adds concentration >=1 M's of 0 times of quality of ligand 1
Acid, stirs 2 more than h, filters, obtains UO2 2+Acid solution and polystyrene-Cyclohexylamino maleic acid solid, by UO2 2+'s
Acid solution concentrates, and obtains pure UO2 2+Compound, as polymeric sorbent after polystyrene-Cyclohexylamino maleic acid washing
Recycling;
Step 3, the recovery of fluorine
A. in step 2 a after solid-liquid separation gained containing high concentration F-Solution in add sodium chloride to the most saturated, due to chlorine
Change sodium and sodium fluoride different solubility in water, according to the principle of common-ion effect so that sodium fluoride separates out because dissolubility reduces,
Filtering, obtain sodium fluoride solid, the fluorine response rate reaches more than 81%;
B., surplus solution about contains a small amount of F-, add the CaCl of excess2, CaO or Ca (OH)2Solid or it is saturated molten
Liquid, generates calcium fluoride precipitate, and the degree of depth completing fluorine is removed, except the surplus solution after uranium fluorine removal contains substantial amounts of sodium chloride, and will
Its recycle and reuse.
Preferably, the acid being acidified in step one is 1 ~ 2 M hydrochloric acid.The benefit of selection hydrochloric acid is: a large amount of Cl-After can reducing
The addition of sodium chloride during continuous recovery fluorine.
Preferably, described step one adds acid for adjusting pH=3.8.
Preferably, described polymeric sorbent polystyrene-Cyclohexylamino maleic acid is at room temperature will with cyclohexylamine
The product that SMA open loop obtains.(see: Min Liu, et al., Journal of Applied
Polymer Science, 2013, 130(6), 3432-3439.)
Concrete course of reaction is as follows:
。
Preferably, polymeric sorbent polystyrene-Cyclohexylamino maleic acid addition in step a of described step 2
It is 0.2 ~ 2 g/L.
Preferably, in described step 2, the mixing time in step a is 15 min, and the mixing time in step b is 2 h.
Preferably, in step b of described step 2, adding acid is the hydrochloric acid of total concentration >=1 M, sulphuric acid, nitric acid or high chlorine
One or more in acid, add amount is part quality 10 times of acid, it is ensured that high desorption rate and make UO2 2+Solution concentration Gao Yi
Enrichment.The hydrochloric acid of preferably 1-2M or nitric acid.
Preferably, in the b of step 3, select to add the calcium chloride of excess, wherein, calcium chloride addition and solution remain
F-Mol ratio be 1:1.5 ~ 3, most preferably 1:1.5.
Beneficial effects of the present invention:
The present invention utilizes the polymeric sorbent adsorption and enrichment UO being inexpensively easily-synthesized2 2+.First hex Alkali absorption liquid is given up
Liquid is acidified with 1 ~ 2 M hydrochloric acid, adds polymeric sorbent and completes UO2 2+Absorption, solid-liquid separation by gained solid with 1 more than M
Acid desorption, it is thus achieved that high concentration UO2 2+Solution, it is achieved UO2 2+Recovery, surplus solution add Na2CO3Carry out subsequent cycle hexafluoro
Change the drip washing of uranium.In time circulating more than 5 times, rich in the F of high concentration in solution-.In solution add NaCl to the most saturated make NaF because of
Dissolubility reduces precipitation, filters to obtain NaF solid, adds CaCl2, CaO or Ca (OH)2Solid or its saturated solution make F-Formed
CaF2Precipitation, degree of depth fluorine removal.Therefore present invention achieves the recovery of uranium in radioactive liquid waste and the zero-emission of waste liquid, again according to fluorine
Change sodium and sodium chloride dissolubility different in water, reclaim substantial amounts of F-, add calcium chloride and realize the degree of depth removal of fluorine.Final realization
In uranic hexafluoride gas Alkali absorption liquid waste liquid, uranium and the recovery of a large amount of fluorine, make the discharge of waste liquid be up to state standards, solve simultaneously
Determine the problem that a large amount of calcium fluoride are difficult to filter in traditional defluorinating process.Technique is simple, easy to operate, environmental protection, economical high
Effect.
At UO2 2+Absorption in, due to use the application polymeric sorbent polystyrene-Cyclohexylamino maleic acid,
After making to separate, in solution, the surplus of uranium is less than 0.05 ppm, and adsorption rate reaches more than 99%, at optimum conditions, and adsorption rate
Can reach 100%(and see embodiment 2,3).In the recovery of fluorine, use and add sodium chloride to the most saturated method, due to sodium chloride with
Sodium fluoride is different solubility in water, according to the principle of common-ion effect so that sodium fluoride separates out because dissolubility reduces, and filters,
Obtaining sodium fluoride solid, the fluorine response rate reaches 86.7%(and sees embodiment 3).
Accompanying drawing explanation
Accompanying drawing is for providing a further understanding of the present invention, and constitutes a part for description, with the reality of the present invention
Execute example together for explaining the present invention, be not intended that limitation of the present invention.In the accompanying drawings:
Fig. 1 is uranium and the recovery method schematic flow sheet of fluorine in hex Alkali absorption liquid waste liquid of the present invention;
Fig. 2 is UO in embodiment 42 2+The difference pH influence curve figure to uranium response rate when initial concentration is 48 mg/L.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred reality described herein
Execute example be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1:
In hex Alkali absorption liquid waste liquid, uranium and the recovery method of fluorine, contain UO in its waste liquid2 2+Reach 48 mg/L, circulation
F after 5 times-Reach 9 g/L.Taking this waste liquid of 1 L as object of study, concrete reaction scheme and operating procedure are as follows:
Step one, the acidifying of hex Alkali absorption liquid waste liquid
In uranic hexafluoride gas Alkali absorption liquid waste liquid, drip 1 M hydrochloric acid, regulate pH=4.5, obtain containing UO2 2+、Na+、F-With Cl-Solution;
Step 2, UO2 2+Recovery
a. UO2 2+Absorption
0.2 g polymeric sorbent polystyrene-Cyclohexylamino maleic acid is added, stirring in step one gained solution
10 min make the UO in solution2 2+Adsorption equilibrium, filters isolated UO2 2+-polystyrene-Cyclohexylamino maleic acid coordinates
Thing solid and containing Na+、F-With Cl-Solution, in solution, the surplus of uranium is 0.048 mg/L (less than 0.05 ppm), absorption
Rate reaches 99.9%, and Na+、F-With Cl-Solution in add Na2CO3After carry out the drip washing of subsequent cycle hex.When circulation 5
Time secondary, obtain rich in F-Concentration reaches the solution of 9 g/L.
b. UO2 2+Desorption
Toward UO2 2+-polystyrene-Cyclohexylamino maleic acid coordination compound adds 2.0 g (1.9 ml, ρ=1.035 g/
Ml) concentration is the nitric acid of 1 M, stirs 3 h, filters and makes solid-liquid separation, obtains UO2 2+Salpeter solution and solid-state polystyrene-
Cyclohexylamino maleic acid, desorption rate reaches more than 99%.By UO2 2+Salpeter solution concentrate, available pure UO2(NO3)2, contain
There is uranium 47.5 mg, and the structure of polystyrene-Cyclohexylamino maleic acid and non-being not affected by of character are destroyed, scrubbed repeatable
Utilize;
Step 3, the recovery of fluorine
A. the solution of fluorine-containing 9 g/L of gained after solid-liquid separation in step 2 a, adds sodium chloride to the most saturated, due to sodium chloride
With sodium fluoride different solubility in water, according to the principle of common-ion effect so that sodium fluoride because of dissolubility reduce separate out, mistake
Filter, obtains sodium fluoride solid 16.1 g, remains F-Being 1.7 g/L, the fluorine response rate reaches 81%;
B., surplus solution about contains a small amount of F-, add calcium chloride 5 g, generate calcium fluoride precipitate, remain F-Less than state
Family sewage drainage standard 10 mg/L, the degree of depth completing fluorine is removed.Except the surplus solution after uranium fluorine removal contains substantial amounts of chlorination
Sodium, can be by its recycle and reuse.
Embodiment 2:
In uranic hexafluoride gas Alkali absorption liquid waste liquid, uranium and the recovery method of fluorine, contain UO in its waste liquid2 2+Reach 130 mg/
L, F after circulating 5 times-Reach 8 g/L.Take this waste liquid of 1 L as object of study:
Step one, the acidifying of hex Alkali absorption liquid waste liquid
In uranic hexafluoride gas Alkali absorption liquid waste liquid, drip 2 M hydrochloric acid, regulate pH=3.8, obtain containing UO2 2+、Na+、F-With Cl-Solution;
Step 2, UO2 2+Recovery
a. UO2 2+Absorption
In step one gained solution, add 0.5 g styrene-Cyclohexylamino maleic acid, stir 15 min and make solution
In UO2 2+Adsorption equilibrium, filters isolated UO2 2+-polystyrene-Cyclohexylamino maleic acid coordination compound solid and containing Na+、F-With Cl-Solution, in solution, the surplus of uranium is 0 (less than 0.05 ppm), and adsorption rate reaches 100%, and Na+、F-With Cl-
Solution in add Na2CO3After carry out the drip washing of subsequent cycle hex.When circulating 5 times, obtain rich in F-Concentration reaches 8
The solution of g/L;
b. UO2 2+Desorption
Toward UO2 2+It is dense that-polystyrene-Cyclohexylamino maleic acid coordination compound adds 5 g (4.7 ml, ρ=1.065 g/ml)
Degree is the nitric acid of 2 M, stirs 2 h, filters and makes solid-liquid separation, obtains UO2 2+Salpeter solution and polystyrene-Cyclohexylamino
Maleic acid, desorption rate reaches more than 99%.By UO2 2+Salpeter solution concentrate, available pure UO2(NO3)2, containing uranium 128
Mg, and the scrubbed repeatable utilization of polystyrene-Cyclohexylamino maleic acid;
Step 3, the recovery of fluorine
A. the solution of fluorine-containing 8 g/L of gained after solid-liquid separation in step 2 a, adds sodium chloride to the most saturated, and sodium fluoride is because of molten
Xie Du reduces precipitation, filters, and obtains sodium fluoride solid 14.6 g, remains F-Being 1.4 g/L, the fluorine response rate reaches 83%;
B. calcium chloride 5 g, a small amount of F in surplus solution are added-Generation calcium fluoride precipitate separates out, and remains F-Less than country
Sewage drainage standard 10 mg/L, the degree of depth completing fluorine is removed.Except the surplus solution after uranium fluorine removal contains substantial amounts of sodium chloride,
Can be by its recycle and reuse.
Embodiment 3:
In uranic hexafluoride gas Alkali absorption liquid waste liquid, uranium and the recovery method of fluorine, contain UO in its waste liquid2 2+Reach 238 mg/
L, F after circulating 5 times-Reach 10 g/L.Taking this waste liquid of 1 L as object of study, concrete reaction scheme and operating procedure are as follows:
Step one, the acidifying of hex Alkali absorption liquid waste liquid
In uranic hexafluoride gas Alkali absorption liquid waste liquid, drip 2 M hydrochloric acid, regulate pH=3.5, obtain containing UO2 2+、Na+、F-With Cl-Solution;
Step 2, UO2 2+Recovery
a. UO2 2+Absorption
In step one gained solution, add 1 g polymeric sorbent polystyrene-Cyclohexylamino maleic acid, stir 15
Min makes the UO in solution2 2+Adsorption equilibrium, filters isolated UO2 2+-polystyrene-Cyclohexylamino maleic acid coordination compound
Solid and containing Na+、F-With Cl-Solution, in solution, the surplus of uranium is 0 (less than 0.05 ppm), and adsorption rate reaches 100%,
And Na+、F-With Cl-Solution in add Na2CO3After carry out the drip washing of subsequent cycle hex.When circulating 5 times, obtain richness
Containing F-Concentration reaches the solution of 10 g/L;
b. UO2 2+Desorption
Toward UO2 2+-polystyrene-Cyclohexylamino maleic acid coordination compound adds 10.0 g (9.9 ml, ρ=1.015 g/
Ml) concentration is the hydrochloric acid of 2 M, stirs 3 h, filters and makes solid-liquid separation, obtains UO2 2+Hydrochloric acid solution and polystyrene-cyclohexyl
Amino maleic acid, desorption rate reaches more than 99%.By UO2 2+Hydrochloric acid solution concentrate, obtain uranium 235 mg, and polystyrene-ring
The scrubbed repeatable utilization of hexylamino maleic acid;
Step 3, the recovery of fluorine
A. the solution of fluorine-containing 10 g/L of gained after solid-liquid separation in step 2 a, adds sodium chloride to the most saturated so that fluorination
Sodium separates out because dissolubility reduces, and filters, and obtains sodium fluoride solid 19.2 g, remains F-Being 1.3 g/L, the fluorine response rate reaches
86.7%;
B., surplus solution adds calcium chloride 5 g, generates calcium fluoride precipitate, remain F-Less than state sewage emission standard
10 mg/L, the degree of depth completing fluorine is removed.Except the surplus solution after uranium fluorine removal contains substantial amounts of sodium chloride, can be reclaimed and be followed
Ring utilizes.
Embodiment 4:
Different pH are to UO2 2+The response rate impact experiment
In hex Alkali absorption liquid waste liquid, uranium and the recovery method of fluorine, contain UO in its waste liquid2 2+Reach 48 mg
/ L, takes this waste liquid of 1 L as object of study, and concrete reaction scheme and operating procedure are as follows:
Step one, acidifying
1) in uranic hexafluoride gas Alkali absorption liquid waste liquid, drip 1 M hydrochloric acid, regulate respectively pH=1.44,1.99,
2.93,4.10,4.58,6.38,7.42, obtain containing UO2 2+、Na+、F-With Cl-Solution;
Step 2, UO2 2+Absorption
0.2 g polymeric sorbent polystyrene-Cyclohexylamino Malaysia is added respectively in the solution of step one gained
Acid, stirs 10 min and makes the UO in solution2 2+Adsorption equilibrium, filters isolated UO2 2+-polystyrene-Cyclohexylamino horse
Carry out sour coordination compound solid and containing Na+、F-With Cl-Solution, adsorption rate is respectively as follows: 92.9%, 94.8%, 100%, 100%, 100%,
98.1%, 96.1%, draw curve chart, see accompanying drawing 2.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to aforementioned reality
Executing example to be described in detail the present invention, for a person skilled in the art, it still can be to aforementioned each enforcement
Technical scheme described in example is modified, or wherein portion of techniques feature is carried out equivalent.All essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (10)
1. uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid, it is characterised in that: comprise the steps:
Step one, acidifying:
In the hex Alkali absorption liquid waste liquid obtained with sodium carbonate liquor drip washing, containing UO2 2+, Na+And F-Ion, at this solution
Middle addition hydrochloric acid is acidified to pH value of solution=2.7 ~ 5.5, obtains containing UO2 2+、Na+、F-With Cl-Solution;
Step 2, UO2 2+Recovery
a. UO2 2+Absorption
In the solution that step one obtains, add polymeric sorbent polystyrene-Cyclohexylamino maleic acid, stir 10 min
Above, the now UO in solution2 2+Adsorption equilibrium, filters isolated UO2 2+-polystyrene-Cyclohexylamino maleic acid coordinates
Thing solid and Na+、F-With Cl-Solution, the solution after solid-liquid separation adds Na2CO3After carry out the pouring of subsequent cycle hex
Wash, when circulating more than 5 times, obtain rich in F-Solution;
b. UO2 2+Desorption
Toward UO2 2+-polystyrene-Cyclohexylamino maleic acid coordination compound adds the acid of concentration >=1 M of 0 times of quality of ligand 1,
Stir 2 more than h, filter, obtain UO2 2+Acid solution and polystyrene-Cyclohexylamino maleic acid solid, by UO2 2+Acid molten
Liquid concentrates, and obtains pure UO2 2+Compound, as polymeric sorbent after polystyrene-Cyclohexylamino maleic acid solid washing
Recycling;
Step 3, the recovery of fluorine
A. in step 2 a after solid-liquid separation gained rich in F-Solution in add sodium chloride to the most saturated, sodium fluoride is because of dissolubility
Reduce and separate out, filter, obtain sodium fluoride solid;
B., surplus solution adds the CaCl of excess2, CaO or Ca (OH)2Solid, or CaCl2Saturated solution, or Ca (OH)2's
Saturated solution, generates calcium fluoride precipitate, and the degree of depth completing fluorine is removed, except the surplus solution after uranium fluorine removal contains sodium chloride, and will
Its recycle and reuse.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 1, it is characterised in that: step
The concentration of hydrochloric acid being acidified in rapid one is 1 ~ 2 M.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 1, it is characterised in that: institute
State and step one adds hydrochloric acid to pH value of solution=3.8.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 1, it is characterised in that: institute
Stating polymeric sorbent polystyrene-Cyclohexylamino maleic acid in step a of step 2 is at room temperature will be poly-with cyclohexylamine
The product that maleic anhydride of styrene open loop obtains.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 1, it is characterised in that: institute
Stating in step a of step 2, polystyrene-Cyclohexylamino maleic acid addition is 0.2 ~ 2 g/L.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 1, it is characterised in that: institute
Stating in step 2, the mixing time in step a is 15 min, and the mixing time in step b is 2 h.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 1, it is characterised in that: institute
Stating in step b of step 2, the acid of addition is one or more in the hydrochloric acid of total concentration >=1 M, sulphuric acid, nitric acid or perchloric acid
Combination.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 7, it is characterised in that: institute
State in step b of step 2, add hydrochloric acid or nitric acid that acid is 1 ~ 2 M.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 1, it is characterised in that: step
In the b of rapid three, select to add calcium chloride, wherein, calcium chloride addition and solution remain F-Mol ratio be 1:1.5 ~ 3.
Uranium and the recovery method of fluorine in hex Alkali absorption liquid waste liquid the most according to claim 9, it is characterised in that:
In the b of step 3, select to add calcium chloride, wherein, calcium chloride addition and solution remain F-Mol ratio be 1:1.5.
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CN105448373B (en) * | 2015-11-06 | 2018-06-01 | 西南科技大学 | A kind of uranium-containing waste water with high salt or waste liquid quickly remove uranium salt reduction method |
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