CN104109757B - A kind of technique recycling calciothermic reduction fused salt used - Google Patents
A kind of technique recycling calciothermic reduction fused salt used Download PDFInfo
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- CN104109757B CN104109757B CN201410383808.2A CN201410383808A CN104109757B CN 104109757 B CN104109757 B CN 104109757B CN 201410383808 A CN201410383808 A CN 201410383808A CN 104109757 B CN104109757 B CN 104109757B
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Abstract
The invention belongs to nuclear chemical industry and nuclear fuel reprocessing technical field, disclose a kind of technique recycling calciothermic reduction fused salt used.This technique comprises: will be placed in container containing the calcium chloride fused salt of calcium oxide after calciothermic reduction, heats this fused salt to 820 DEG C ~ 900 DEG C; After fused salt melting, hydrogen chloride gas or chlorine are passed in fused salt through pipeline, react with calcium oxide and generate calcium chloride; After reaction terminates, off-response gas; Argon gas is passed into, to drive the reactant gases in fused salt and gas pipeline away in fused salt.This technique is simple, with low cost, chlorination rate is high, avoid environmental pollution, can recycle oxide compound spent fuel calciothermic reduction process fused salt used.
Description
Technical field
The invention belongs to nuclear chemical industry and nuclear fuel reprocessing technical field, be specifically related to a kind of technique recycling calciothermic reduction fused salt used.
Background technology
At present, dry method aftertreatment has been listed in the one preferred technique of fast reactor spent fuel fuel that process has dark burnup, Gao Bifang, high plutonium content feature.Wherein, fused-salt electrolytic refining technology studies the dry method post-processing technology the most extensive, development is more ripe, but fused-salt electrolytic refining processing requirement anode feed is metal form, is therefore particularly suitable for process metal form spent fuel.For fused-salt electrolytic refining technology popularization being applied to the aftertreatment of oxide compound spent fuel, first the reduction of oxide compound spent fuel must be converted into metal form.Calciothermy is the common method of metal by Reduction of Oxide, oxide compound spent fuel can be converted into metal, prepare the anode feed met needed for follow-up electrorefining separating technology.
The calciothermic reduction process of oxide compound spent fuel can produce by product calcium oxide, and these Calcium oxide dissolution can increase the viscosity of fused salt in fused salt (being generally calcium chloride), affect stirring technique, reduces the reduction ratio of spent fuel.For improving the reduction ratio of oxide compound spent fuel, need regularly replace fused salt, this will produce a large amount of waste fused salts (calcium oxide containing the 10wt% that has an appointment).These waste fused salts must as radioactive waste disposal, there is alpha-contamination danger and cost of disposal is high.Therefore, be badly in need of one and waste fused salt is processed, and the technique of use can be reclaimed.
Summary of the invention
(1) goal of the invention
Problem existing for prior art, the invention provides the technique that a kind of processing condition are simple, with low cost, chlorination rate is high, avoid environmental pollution, can recycle oxide compound spent fuel calciothermic reduction process fused salt used.
(2) technical scheme
In order to solve the problem existing for prior art, the present invention is achieved by the following technical solutions:
Recycle a technique for calciothermic reduction fused salt used, this technique comprises the following steps:
(1) will be placed in container containing the calcium chloride fused salt of calcium oxide after calciothermic reduction, heat this fused salt to 820 DEG C ~ 900 DEG C, make fused salt melting; Described container is high temperature resistant, resistance to reactant gases and fused salt corrosion and the good container of thermal shock resistance.
(2) by reactant gases in the fused salt that pipeline passes into the melting described in step (1), react with calcium oxide and generate calcium chloride; Wherein reactant gases is hydrogen chloride gas or chlorine; Described pipeline is high temperature resistant, resistance to reactant gases and fused salt corrosion and the good pipeline of thermal shock resistance.
(3) after the reaction in step (2) terminates, off-response gas;
(4) in fused salt, argon gas is passed into, to drive the reactant gases in fused salt away.
Preferably, mole the measuring than being 1:1 ~ 1.5 ~ 1 of reactant gases described in step (2) and calcium oxide.
Preferably, lower end of duct described in step (2) is apart from container bottom 5 ~ 10mm.
Preferably, described in step (2), the flow velocity of reactant gases is 0.1 ~ 1L/min.
Preferably, under described in step (1), container is in argon atmosphere.
Preferably, described in step (1), container is corundum crucible.
Preferably, described in step (2), pipeline is alundum tube.
Preferably, in fused salt, pass into argon gas in step (4) is pass into via the pipeline described in step (2).
(3) beneficial effect
The present invention adopts gas sparging method to carry out recovery to calciothermic reduction fused salt used and uses, and by passing into hydrogen chloride gas in calcium chloride fused salt, calcium oxide is wherein carried out chlorination, chlorination rate is up to more than 99.9%.This technique reduces waste fused salt amount and does not introduce other metallic impurity, and the fused salt that can realize after chlorination returns to calciothermic reduction process and uses.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
Embodiment 1
Recycle a technique for calciothermic reduction fused salt used, this technique comprises:
(1) the calcium chloride fused salt after oxide compound spent fuel calciothermic reduction is placed in corundum crucible, heats this fused salt to 820 DEG C, make fused salt melting; Under wherein corundum crucible is in argon shield atmosphere.
(2) by hydrogen chloride gas with the flow velocity of 0.1L/min in the fused salt that alundum tube passes into the melting in step (1), alundum tube lower end outlet distance corundum crucible bottom 5mm, hydrogen chloride gas and calcium oxide react and generate calcium chloride; Wherein mole the measuring than being 1:1 of hydrogen chloride gas and calcium oxide.
(3), after the reaction in step (2) terminates, close hydrogen chloride gas, then in fused salt, pass into argon gas by alundum tube, to drive the reactant gases in fused salt away.
Recycle the calcium chloride fused salt after oxide compound spent fuel calciothermic reduction through above-mentioned steps, chlorination rate is 99.92%, calcium chloride fused salt can be it can be used as to reuse, not only saved cost, also decrease radwaste content to the full extent.
Embodiment 2
As different from Example 1, chlorine is reacted as reactant gases with 1L/min and calcium oxide, chlorine and calcium oxide mole measure than being 1.5:1; The Heating temperature of fused salt is 900 DEG C.10mm bottom alundum tube distance corundum crucible.
Embodiment 3
As different from Example 1, chlorine is reacted as reactant gases with 0.5L/min and calcium oxide, chlorine and calcium oxide mole measure than being 1.2:1; The Heating temperature of fused salt is 850 DEG C.8mm bottom alundum tube distance corundum crucible.
Claims (4)
1. recycle a technique for calciothermic reduction fused salt used, it is characterized in that, this technique is used for recycling oxide compound spent fuel calciothermic reduction process waste fused salt used, and this technique comprises the following steps:
(1) will be placed in container containing the calcium chloride fused salt of calcium oxide after calciothermic reduction, heat this fused salt to 820 DEG C ~ 900 DEG C, make fused salt melting; Described container is high temperature resistant, resistance to reactant gases and fused salt corrosion and the good container of thermal shock resistance;
(2) by reactant gases in the fused salt that pipeline passes into the melting described in step (1), react with calcium oxide and generate calcium chloride; Wherein reactant gases is hydrogen chloride gas; Described pipeline is high temperature resistant, resistance to reactant gases and fused salt corrosion and the good pipeline of thermal shock resistance;
(3) after the reaction in step (2) terminates, off-response gas;
(4) in fused salt, argon gas is passed into, to drive the reactant gases in fused salt away;
Lower end of duct described in step (2) is apart from container bottom 5 ~ 10mm; Described in step (2), the flow velocity of reactant gases is 0.1 ~ 1L/min; Under described in step (1), container is in argon atmosphere; In fused salt, pass into argon gas in step (4) is pass into via the pipeline described in step (2).
2. a kind of technique recycling calciothermic reduction fused salt used according to claim 1, is characterized in that, reactant gases and calcium oxide mole measure than being 1:1 ~ 1.5:1 in described step (2).
3. a kind of technique recycling calciothermic reduction fused salt used according to claim 1, is characterized in that, described in step (1), container is corundum crucible.
4. a kind of technique recycling calciothermic reduction fused salt used according to claim 1, is characterized in that, described in step (2), pipeline is alundum tube.
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| CN201410383808.2A CN104109757B (en) | 2014-08-06 | 2014-08-06 | A kind of technique recycling calciothermic reduction fused salt used |
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| CN201410383808.2A CN104109757B (en) | 2014-08-06 | 2014-08-06 | A kind of technique recycling calciothermic reduction fused salt used |
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| CN104109757A CN104109757A (en) | 2014-10-22 |
| CN104109757B true CN104109757B (en) | 2016-03-30 |
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| CN112048620A (en) * | 2020-09-03 | 2020-12-08 | 中国原子能科学研究院 | System and method for preparing uranium metal |
| CN114016083B (en) * | 2021-11-05 | 2023-11-03 | 澳润新材料科技(宜兴)有限公司 | Method for regenerating alkali metal reducing agent in process of preparing metal by alkali metal thermal reduction of metal oxide |
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| JP2002129250A (en) * | 2000-10-30 | 2002-05-09 | Katsutoshi Ono | Method for producing metallic titanium |
| JP4193985B2 (en) * | 2003-08-28 | 2008-12-10 | 株式会社大阪チタニウムテクノロジーズ | Metal production method and apparatus by Ca reduction |
| JP4193984B2 (en) * | 2003-08-28 | 2008-12-10 | 株式会社大阪チタニウムテクノロジーズ | Metal manufacturing equipment |
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