CN101717869B - Extraction and separation technology of uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element - Google Patents

Extraction and separation technology of uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element Download PDF

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CN101717869B
CN101717869B CN200910263507A CN200910263507A CN101717869B CN 101717869 B CN101717869 B CN 101717869B CN 200910263507 A CN200910263507 A CN 200910263507A CN 200910263507 A CN200910263507 A CN 200910263507A CN 101717869 B CN101717869 B CN 101717869B
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uranium
molybdenum
extraction
fuel element
type fuel
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CN101717869A (en
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任萌
李佳
朱常桂
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Nuclear Power Institute of China
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Nuclear Power Institute of China
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Abstract

The invention relates to a recovery processing technology of fission fuel, in particular to an extraction and separation technology of uranium and molybdenum contained in a uranium and molybdenum alloy diffuse-type fuel element. The extraction and separation technology of uranium and molybdenum contained in the uranium and molybdenum alloy diffuse-type fuel element comprises the following steps of: dissolving a uranium and molybdenum alloy contained in a UMo/Al diffuse-type fuel element by HNO3/HCl; separating the uranium and the molybdenum contained in the UMo/Al diffuse-type fuel element; and after the uranium and molybdenum alloy is dissolved by the HNO3/HCl, preparing into extraction feed liquid; extracting by a TBP-kerosene system so that the uranium and the molybdenum are separated. A separated and purified uranium solution can be returned to be used again in a production technology, thus requirement on environmental protection is met, and product cost is reduced; in addition, the invention solves the technical problems of dissolution and the optimization and the establishment of extracting technological parameters in the extraction and separation technology of the uranium and the molybdenum.

Description

The extraction and separation technology of uranium and molybdenum in the uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element
Technical field
The present invention relates to a kind of recovery processing technique of nuclear fuel, be specifically related to the extraction and separation technology of uranium in the uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element, molybdenum.
Background technology
At present, reclaim technology, full plate nitric acid dissolve filtration method is arranged for the processing of duraluminum involucrum nuclear fuel; After alkali dissolved and shells, acid was dissolved and is filtered again; Or in nitric acid, add FeCl 3Core body is dissolved entirely.But for uranium molybdenum alloy fuel, its dissolution process is one of technological difficulties; Because molybdenum is dissolved in nitric acid and can generates a large amount of precipitate molybdic acid; Thereby next step extracting operation brought big difficulty, though with behind the sedimentation and filtration again extraction can address this problem, increased the technical process link; Make operation more complicated; And the loss of uranium can increase, thereby has limited existing duraluminum involucrum nuclear fuel and reclaimed technology, the application in uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element uranium, the molybdenum of duraluminum involucrum reclaim.
Through retrieval, do not see the RR or the report of uranium in the UMo/Al dispersion type fuel element, molybdenum extraction and separation technology.
Summary of the invention
The objective of the invention is to: a kind of simple to operate, effective extraction and separation technology of uranium, molybdenum in the Separation and Recovery uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element is provided.
Technical scheme of the present invention is following:
The extraction and separation technology of uranium and molybdenum in a kind of U-10%Mo uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element, step is following:
Step 1 dissolving: the U-10%Mo uranium molybdenum alloy fuel that will remove behind the involucrum is put into dissolution reactor; Add volumetric concentration again and be 50% nitric acid and hydrochloric acid, the volume ratio of wherein used nitric acid and hydrochloric acid is 2: 1, and used nuclear fuel is 1: 1 with sour volume ratio; Under 70 ℃～90 ℃, react; Constantly stir to add fast response, after reaction finished, cooling was left standstill;
Step 2 preparation extraction feed liquid: the uranium content of gained lysate, molybdenum content and acidity in the analytical procedure one, drawing uranium content is 180.0～270.0g L -1, molybdenum content is 20.0～30.0g L -1, acidity is 2.0～4.0mol L -1
Pipette respectively in the volumetric flask of above-mentioned lysate 5.0～50.0mL to 100mL, add concentrated nitric acid 19.0～55.0mL then in regular turn respectively, add 70.0～28.0mL water more in regular turn respectively, being mixed with acidity is 3.0～8.0mol L -1Uranium concentration is 9.00～90.00g L -1, molybdenum concentration is 1.00～10.00g L -1Extraction feed liquid;
The step 3 extracting and separating: with extraction feed liquid in 10%～50%TBP-kerosene system, compare O/A=0.5～2.5, extract under the room temperature condition, starting time 2～8 minutes is emitted water after layering finishes.
Effect of the present invention is: adopt HNO first 3Uranium molybdenum alloy in the/HCl dissolving U Mo/Al dispersion type fuel element, the uranium molybdenum alloy is through HNO 3After/HCl the dissolving, be prepared into the extraction feed liquid; Adopt the TBP-kerosene extraction to reclaim uranium molybdenum alloy HNO first 3Uranium in the/HCl system makes uranium separate with molybdenum; Each item processing parameter of TBP-kerosene extraction recovery uranium has been optimized in foundation, and the uranium solution after the separation and purification can return production technique usefulness more after treatment, has satisfied environmental requirement and has reduced production cost.
Embodiment
The extraction and separation technology concrete steps of uranium and molybdenum are following in the uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element of the present invention:
Step 1 dissolving: the U-10%Mo uranium molybdenum alloy nuclear fuel that will remove behind the involucrum is put into dissolution reactor; Add volumetric concentration and be 50% nitric acid and hydrochloric acid, the volume ratio of wherein used nitric acid and hydrochloric acid is 2: 1, and used nuclear fuel is 1: 1 with sour volume ratio; Under 70～90 ℃, react; Constantly stir to add fast response, after reaction finished, cooling was left standstill;
Step 2 preparation extraction feed liquid: the uranium content of gained lysate, molybdenum content and acidity in the analytical procedure one, drawing uranium content is 180.0～270.0g L -1, molybdenum content is 20.0～30.0g L -1, acidity is 2.0～4.0mol L -1
Pipette respectively in the volumetric flask of above-mentioned lysate 5.0～50.0mL to 100mL, add concentrated nitric acid 19.0～55.0mL then in regular turn respectively, add 70.0～28.0mL water more in regular turn respectively, being mixed with acidity is 3.0～8.0mol L -1Uranium concentration is 9.00～90.00g L -1, molybdenum concentration is 1.00～10.00g L -1Extraction feed liquid;
The step 3 extracting and separating: with extraction feed liquid in 10%～50%TBP-kerosene system, compare O/A=0.5～2.5, extract under the room temperature condition, starting time 2～8 minutes is emitted water after layering finishes.
Below in conjunction with embodiment, the extraction and separation technology to uranium and molybdenum in the uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element of the present invention further describes:
Embodiment 1
1. dissolving: the U-10%Mo uranium molybdenum alloy nuclear fuel that will remove behind the involucrum is put into dissolution reactor; In reactor drum, add volume by volume concentration and be 50% nitric acid and hydrochloric acid, the volume ratio of wherein used nitric acid and hydrochloric acid is 2: 1, and used nuclear fuel is 1: 1 with sour volume ratio; Under 80 ℃ of temperature, react; Constantly stir to add fast response, after reaction finished, cooling was left standstill;
2. prepare extraction feed liquid: the uranium content of gained lysate, molybdenum content and acidity in the analytical procedure 1, drawing uranium content is 180.0g L -1, molybdenum content is 20.0g L -1, acidity is 2.0mol L -1
Pipette respectively in above-mentioned lysate 5.0mL, 10.0mL, 20.0mL, 30.0mL, 40.0mL, 50.0mL to the 100mL volumetric flask (totally six), add concentrated nitric acid 27.8mL, 27.1mL, 25.7mL, 24.3mL, 22.9mL, 21.4mL then in regular turn respectively; Add entry 67.2mL, 62.9mL, 54.3mL, 45.7mL, 37.1mL, 28.9mL more in regular turn respectively, it is 4.0mol L that six lysates are mixed with acidity -1, uranium concentration is respectively 9.00g L -1, 18.00g L -1, 36.00g L -1, 54.00gL -1, 72.00g L -1, 90.00g L -1Molybdenum concentration is respectively 1.00g L -1, 2.00g L -1, 4.00g L -1, 6.00g L -1, 8.00gL -1, 10.00gL -1Six laboratory samples;
3. extracting and separating: with above-mentioned six laboratory samples in the 30%TBP-kerosene system, compare O/A=1: 1, extract under the room temperature condition, starting time 2 minutes is emitted water after layering finishes.
Analytical results demonstrates: increase uranium partition ratio D with uranium concentration UElder generation increases afterwards and reduces, at uranium=36.00g L -1The time reach peak; And molybdenum partition ratio D MoNumerical value is very little, is almost 0; At uranium=36.00～90.00g L -1Uranium, molybdenum all have good separating effect in the concentration range.
Embodiment 2
1. with embodiment 1;
2. prepare extraction feed liquid: the uranium content of gained lysate, molybdenum content and acidity in the analytical procedure 1, drawing uranium content is 210.0g L -1, molybdenum content is 23.3g L -1, acidity is 2.0mol L -1
Pipette respectively in the volumetric flask (totally six) of above-mentioned each 17.1mL to 100mL of lysate; Add concentrated nitric acid 19.0mL, 26.1mL, 33.3mL, 40.4mL, 47.6mL, 54.7mL then in regular turn respectively; Add entry 63.9mL, 56.8mL, 49.6mL, 42.5mL, 35.3mL, 28.2mL more in regular turn respectively, it is 36.00gL that lysate is mixed with uranium concentration -1, molybdenum concentration is 4.00g L -1, acidity is respectively 3.0molL -1, 4.0mol L -1, 5.0mol L -1, 6.0mol L -1, 7.0mol L -1, 8.0mol L -1Six laboratory samples;
3. extracting and separating: with above-mentioned six laboratory samples in the 30%TBP-kerosene system, compare O/A=1: 1, extract under the room temperature condition, starting time 4 minutes is emitted water after layering finishes.
Analytical results demonstrates: with the increase of acidity, and uranium partition ratio D UAt [H +]=6.0molL -1In time, begin to reduce gradually after reaching peak; But molybdenum partition ratio D MoThe amplitude that reduces to increase is all very little, and total trend changes about 0; In acidity is 3.0～8.0mol L -1In the scope, uranium, molybdenum all have good separating effect.
Embodiment 3
1. with embodiment 1;
2. prepare extraction feed liquid: the uranium content of gained lysate, molybdenum content and acidity in the analytical procedure 1, drawing uranium content is 240.0g L -1, molybdenum content is 26.7g L -1, acidity is 3.0mol L -1
Pipette in above-mentioned lysate 15mL to the 100mL volumetric flask, add concentrated nitric acid 39.6mL then, add entry 45.4mL dilution again, it is 36.00gL that lysate is mixed with uranium concentration -1, molybdenum concentration is 4.00gL -1, acidity is 6.0mol L -1The extraction feed liquid;
3. extracting and separating: in the 30%TBP-kerosene system, compare that O/A is respectively 0.5,1.0,1.5,2.0,2.5, carry out extraction experiments under the room temperature condition, starting time 6 minutes is emitted water after layering finishes.
Analytical results demonstrates: increase uranium partition ratio D with comparing O/A UPeak value appears when O/A=1.5; Molybdenum partition ratio D MoIt is less influenced by it, is in 0.5～2.5 scope comparing O/A, and uranium, molybdenum all have good separating effect.
Embodiment 4
1. with embodiment 1;
2. prepare extraction feed liquid: the uranium content of gained lysate, molybdenum content and acidity in the analytical procedure 1, drawing uranium content is 270.0g L -1, molybdenum content is 30.0g L -1, acidity is 4.0mol L -1
Pipette in above-mentioned lysate 13.3mL to the 100mL volumetric flask, add concentrated nitric acid 39.1mL then, add entry 47.6mL dilution again, it is 36.00gL that lysate is mixed with uranium concentration -1, molybdenum concentration is 4.00gL -1, acidity is 6.0mol L -1The extraction feed liquid;
3. extracting and separating: comparing under O/A=1.5, the room temperature condition, using TBP concentration respectively is that 10%, 20%, 30%, 40%, 50% kerosene system extracts above-mentioned feed liquid, and starting time 8 minutes is emitted water after layering finishes.
Analytical results demonstrates: with the increase of organic phase TBP concentration, and uranium partition ratio D UIncrease gradually; Molybdenum partition ratio D MoNumerical value approaches 0; In TBP concentration was 10%～50% scope, uranium, molybdenum all had good separating effect.
Comprehensive above-mentioned 4 embodiment reach a conclusion: at uranium concentration is 36.00～90.00g L -1, [H +]=3.0～8.0mol L -1, to compare O/A=0.5～2.5, organic phase TBP concentration be under 10%～50% the extraction conditions, uranium and molybdenum all to be had good separating effect.
Following table provides: uranium concentration is 36g L -1, molybdenum concentration is 4g L -1, acidity is 6mol L -1, in the 30%TBP-kerosene system, room temperature condition is extraction down, starting time 8 minutes, and gained uranium molybdenum partition ratio is with the variation of comparing.

Claims (1)

1. the extraction and separation technology of uranium and molybdenum in the U-10%Mo uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element, step is following:
Step 1 dissolving: the U-10%Mo uranium molybdenum alloy fuel that will remove behind the involucrum is put into dissolution reactor; Add volumetric concentration again and be 50% nitric acid and hydrochloric acid, the volume ratio of wherein used nitric acid and hydrochloric acid is 2: 1, and used nuclear fuel is 1: 1 with sour volume ratio; Under 70～90 ℃, react; Constantly stir to add fast response, after reaction finished, cooling was left standstill;
Step 2 preparation extraction feed liquid: the uranium content of gained lysate, molybdenum content and acidity in the analytical procedure one, drawing uranium content is 180.0～270.0g L -1, molybdenum content is 20.0～30.0gL -1, acidity is 2.0～4.0mol L -1
Pipette respectively in the volumetric flask of above-mentioned lysate 5.0～50.0mL to 100mL, add concentrated nitric acid 19.0～55.0mL then in regular turn respectively, add 70.0～28.0mL water more in regular turn respectively, being mixed with acidity is 3.0～8.0mol L -1Uranium concentration is 9.00～90.00g L -1, molybdenum concentration is 1.00～10.00g L -1Extraction feed liquid;
The step 3 extracting and separating: with extraction feed liquid in 10%～50%TBP-kerosene system, compare O/A=0.5～2.5, extract under the room temperature condition, starting time 2～8 minutes is emitted water after layering finishes.
CN200910263507A 2009-12-21 2009-12-21 Extraction and separation technology of uranium and molybdenum contained in uranium and molybdenum alloy diffuse-type fuel element Active CN101717869B (en)

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Citations (3)

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Publication number Priority date Publication date Assignee Title
US3083076A (en) * 1959-06-05 1963-03-26 Gen Mills Inc Control of molybdenum during liquidliquid extraction of uranium using amine extractants
US3156524A (en) * 1958-09-22 1964-11-10 Gen Mills Inc Prevention of insoluble molybdenumamine complexes in the liquid-liquid extraction ofuranium using amine extractants
US4363788A (en) * 1979-03-19 1982-12-14 Uranium Pechiney Ugine Kuhlmann Separation of uranium and molybdenum using a solvent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3156524A (en) * 1958-09-22 1964-11-10 Gen Mills Inc Prevention of insoluble molybdenumamine complexes in the liquid-liquid extraction ofuranium using amine extractants
US3083076A (en) * 1959-06-05 1963-03-26 Gen Mills Inc Control of molybdenum during liquidliquid extraction of uranium using amine extractants
US4363788A (en) * 1979-03-19 1982-12-14 Uranium Pechiney Ugine Kuhlmann Separation of uranium and molybdenum using a solvent

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