CN105819486A - Auxiliary dissolving method of rare earth oxide in LiCl-KCl molten salt system - Google Patents
Auxiliary dissolving method of rare earth oxide in LiCl-KCl molten salt system Download PDFInfo
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- CN105819486A CN105819486A CN201610133147.7A CN201610133147A CN105819486A CN 105819486 A CN105819486 A CN 105819486A CN 201610133147 A CN201610133147 A CN 201610133147A CN 105819486 A CN105819486 A CN 105819486A
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Abstract
The invention discloses an auxiliary dissolving method of rare earth oxide in a LiCl-KCl molten salt system. The method comprises the following steps: 1, uniformly mixing LiCl and KCl in a crucible, and carrying out drying pretreatment on the obtained mixture; 2, heating the crucible to make LiCl and KCl become a molten salt; and 3, uniformly mixing ammonium chloride and rare earth oxide powder, directly tiling the obtained powder mixture on the top of the LiCl-KCl molten salt, and ionizing the rare earth oxide in the interface of the molten salt. Ammonium chloride is directly used as auxiliary reagent in the LiCl-KCl molten salt system in the method to realize rare earth oxide ionization at a wide temperature range and under protection of an inert gas or in air atmosphere, so a high ionization efficiency is realized, and mixing of impurity elements is avoided; and the heating decomposition and cooling coagulation principle of ammonium chloride is used to carry out cycle use and recycling. A gas generated after decomposing ammonium chloride can reduce the oxygen partial pressure of the system, so reoxidation of rare earth ions is prevented, and the rare earth oxide ionization efficiency is improved.
Description
Technical field
The present invention relates to spentnuclear fuel post processing high-temperature molten salt Electrochemical separation field, be specifically related to a kind of LiCl-KCl fused salt
The method that system middle rare earth auxiliary is dissolved.
Background technology
In recent years, high-temperature molten salt is studied the electrochemical behavior about rare earth element ion, especially by electrochemistry
Research and commercial Application demand in terms of method separation increase day by day.The relevant electrochemistry aspect of rare earth element ion to be studied,
It is necessary for dissolving in fused salt rare earth oxide.Rare earth oxide can not be directly dissolved in fused salt LiCl-KCl, will dissolve in and first need
That wants is transformed into rare earth ion by rare earth oxide exactly.Then the rare earth oxide ionizing developed in recent years dissolves in LiCl-
The auxiliary reagent of KCl molten salt system has AlCl3、MgCl2And ZrCl4Deng.All can melt when utilizing these several reagent to carry out ionizing
Salt system is brought into new foreign ion, increases system complexity and follow-up electrochemical research.
Rare earth oxide dissolve in molten salt system before ioning method have two kinds, one is ionizing in advance, and it two is
Ionizing in real time.Ionizing in advance is exactly with auxiliary reagent, rare earth oxide to be converted into rare earth chloride in advance, then tests
Or during commercial Application, it is directly added into rare earth chloride.Rare earth chloride is prepared and purifies especially difficult, the most inadequate after having prepared
Stable, especially easily deliquescence, causes purity to reduce further, and the application of ionizing the most in advance is the most extensive.Ionizing in real time is exactly
The most just by rare earth oxide ionizing, the rare earth element of ionizing is added in molten salt system in real time.Ionizing in real time
Simple to operate, but because the unfavorable factor such as be mixed into of and reagent foreign ion unstable by Ionization Efficiency is limited, use is subject to
Limit.
Summary of the invention
Brief overview about the present invention given below, in order to the basic reason about certain aspects of the invention is provided
Solve.Should be appreciated that this general introduction is not that the exhaustive about the present invention is summarized.It is not intended to determine the key of the present invention
Or pith, nor is it intended to limit the scope of the present invention.Its purpose is only to provide some concept in simplified form, with
This is as the preamble in greater detail discussed after a while.
The purpose of the embodiment of the present invention is the defect for above-mentioned prior art, it is provided that a kind of avoid the mixed of impurity element
Enter, it is ensured that the method that the LiCl-KCl molten salt system middle rare earth auxiliary of the purity of molten salt system is dissolved.
To achieve these goals, the present invention adopts the technical scheme that:
The method that a kind of LiCl-KCl molten salt system middle rare earth auxiliary is dissolved, comprises the following steps:
(1) it is dried pretreatment after being mixed in crucible by LiCl and KCl；
(2) LiCl and KCl is made to become fused salt to crucible intensification；
(3) LiCl-KCl fused salt top directly it is laid in, at fused salt circle after ammonium chloride and RE oxide powder being mixed
Rare earth oxide ionizing is made at face.
The mass percent of described LiCl and KCl is 44.8:55.2.
Described ammonium chloride and RE oxide powder gross mass are less than 50g, and ammonium chloride addition of the present invention is based on dilute
Soil oxide mass determines.In order to obtain preferable chlorination efficiency, described ammonium chloride and light rare earth oxide powder
Mol ratio is at least 8, and the mol ratio of described ammonium chloride and heavy rare-earth oxide powder is at least 13.
The gross mass of described LiCl and KCl is 50～150 with the total mass ratio of described ammonium chloride and RE oxide powder:
0～50, except 0.
Dry pretreatment in described step (1) includes: by LiCl and KCl drying and dehydrating 72-in Muffle furnace of mixing
110 hours, the temperature being dried was 180-300 DEG C.
Further, also include: under air atmosphere or high purity inert gas bubbling are protected, carry out rare earth oxide ion
Change process.
Described step (2) including: heats up in crucible is placed in high temperature resistance furnace.
Described high temperature resistance furnace temperature elevating range is 250-550 DEG C.
Described RE oxide powder is selected from following rare earth element: cerium (Ce), neodymium (Nd), samarium (Sm), europium (Eu), terbium
(Tb), lanthanum (La), gadolinium (Gd), dysprosium (Dy), holmium (Ho), erbium (Er) or ytterbium (Yb).
Compared with prior art, the invention has the beneficial effects as follows:
The method using the present invention, in fused salt LiCl-KCl system, directly utilizes ammonium chloride permissible as auxiliary reagent
At a temperature of broad and have under inert gas shielding or air atmosphere and make rare earth oxide ionizing, so can obtain relatively
High Ionization Efficiency, it also avoid being mixed into of impurity element；The decomposes and the cooling that utilize ammonium chloride condense principle simultaneously
Recycled and recycled.It addition, according to the method, utilize ammonium chloride to decompose the gas produced and can reduce system
Partial pressure of oxygen, prevents the reoxidation of rare earth ion, improves rare earth oxide Ionization Efficiency.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, also may be used
To obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 a, Fig. 1 b, Fig. 1 c and Fig. 1 d for the present invention implement provide ammonium chloride and cerium oxide different material amount than time
Cyclic voltammetric and square wave voltammogram；
Under the ammonium chloride different temperature elevating range of mol ratio same with Dineodymium trioxide that Fig. 2 a and Fig. 2 b provides for the embodiment of the present invention
The cyclic voltammogram recorded；
Record under ammonium chloride that Fig. 3 a and Fig. 3 b respectively embodiment of the present invention provide and the same mol ratio of Disamarium trioxide follows
Ring voltammogram and square wave voltammogram；
Record under ammonium chloride that Fig. 4 a and Fig. 4 b respectively embodiment of the present invention provide and the same mol ratio of europium oxide follows
Ring voltammogram and square wave voltammogram；
Record under ammonium chloride that Fig. 5 a and Fig. 5 b respectively embodiment of the present invention provide and the same mol ratio of terbia. Diterbium trioxide follows
Ring voltammogram and square wave voltammogram；
Record under ammonium chloride that Fig. 6 a, Fig. 6 b and Fig. 6 c respectively embodiment of the present invention provide and the same mol ratio of Erbia
Cyclic voltammogram, square wave voltammogram and OCP figure；
Record under ammonium chloride that Fig. 7 a, Fig. 7 b and Fig. 7 c respectively embodiment of the present invention provide and the same mol ratio of Gadolinia.
Cyclic voltammogram, square wave voltammogram and OCP figure；
Record under ammonium chloride that Fig. 8 a, Fig. 8 b and Fig. 8 c respectively embodiment of the present invention provide and the same mol ratio of holmia
Cyclic voltammogram, square wave voltammogram and OCP figure；
Record under ammonium chloride that Fig. 9 a, Fig. 9 b and Fig. 9 c respectively embodiment of the present invention provide and the same mol ratio of lanthana
Cyclic voltammogram, square wave voltammogram and OCP figure；
The cyclic voltammogram that records under ammonium chloride that Figure 10 provides for the embodiment of the present invention and the same mol ratio of dysprosia and
Square wave voltammogram；
The cyclic voltammogram that records under ammonium chloride that Figure 11 provides for the embodiment of the present invention and the same mol ratio of ytterbium oxide and
Square wave voltammogram.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
The a part of embodiment of the present invention rather than whole embodiments.Described in the accompanying drawing of the present invention or a kind of embodiment
Element and feature can combine with the element shown in one or more other accompanying drawing or embodiment and feature.Should
Note, for purposes of clarity, accompanying drawing and explanation eliminate unrelated to the invention, known to persons of ordinary skill in the art
Parts and the expression of process and description.Based on the embodiment in the present invention, those of ordinary skill in the art are not paying creation
The every other embodiment obtained under property work premise, broadly falls into the scope of protection of the invention.
Fig. 1 a, Fig. 1 b, Fig. 1 c and Fig. 1 d, Fig. 1 a is ammonium chloride and cerium oxide mol ratio is the cyclic voltammetric recorded when 8, figure
1c is ammonium chloride and cerium oxide mol ratio is the cyclic voltammogram recorded when 11, and Fig. 1 b is ammonium chloride and cerium oxide mol ratio is 8
Time the square wave voltammogram that records, Fig. 1 d is ammonium chloride and cerium oxide mol ratio is the square wave voltammogram recorded when 11.
See Fig. 2 a and Fig. 2 b, the circulation that ammonium chloride records under different temperature elevating range when being 12:1 with Dineodymium trioxide mol ratio
Voltammogram.
Seeing Fig. 3 a and Fig. 3 b, Fig. 3 a is ammonium chloride and Disamarium trioxide mol ratio is the cyclic voltammogram recorded during 20:1, figure
3b is ammonium chloride and Disamarium trioxide mol ratio is the square wave voltammogram recorded during 20:1.
Seeing Fig. 4 a and Fig. 4 b, Fig. 4 a is ammonium chloride and europium oxide mol ratio is the cyclic voltammogram recorded during 20:1, figure
4b is ammonium chloride and europium oxide mol ratio is the square wave voltammogram recorded during 20:1.
Seeing Fig. 5 a and Fig. 5 b, Fig. 5 a is ammonium chloride and terbia. Diterbium trioxide mol ratio is the cyclic voltammogram recorded during 58:1, figure
5b is ammonium chloride and terbia. Diterbium trioxide mol ratio is the square wave voltammogram recorded during 58:1.
Seeing Fig. 6 a, Fig. 6 b and Fig. 6 c, Fig. 6 a is ammonium chloride and Erbia mol ratio is the cyclic voltammetric recorded during 37:1
Figure, Fig. 6 b is ammonium chloride and Erbia mol ratio is the square wave voltammogram recorded during 37:1, and Fig. 6 c is ammonium chloride and Erbia rubs
You are than the OCP figure recorded during for 37:1.
Seeing Fig. 7 a, Fig. 7 b and Fig. 7 c, Fig. 7 a is ammonium chloride and Gadolinia. mol ratio is the cyclic voltammetric recorded during 34:1
Figure, Fig. 7 b is ammonium chloride and Gadolinia. mol ratio is the square wave voltammogram recorded during 34:1, and Fig. 7 c is ammonium chloride and Gadolinia. rubs
You are than the OCP figure recorded during for 34:1.
Seeing Fig. 8 a, Fig. 8 b and Fig. 8 c, Fig. 8 a is ammonium chloride and holmia mol ratio is the cyclic voltammetric recorded during 36:1
Figure, Fig. 8 b is ammonium chloride and holmia mol ratio is the square wave voltammogram recorded during 36:1, and Fig. 8 c is ammonium chloride and holmia rubs
You are than the OCP figure recorded during for 36:1.
Seeing Fig. 9 a, Fig. 9 b and Fig. 9 c, Fig. 9 a is ammonium chloride and lanthana mol ratio is the cyclic voltammetric recorded during 21:1
Figure, Fig. 9 b is ammonium chloride and lanthana mol ratio is the square wave voltammogram recorded during 21:1, and Fig. 9 c is ammonium chloride and lanthana rubs
You are than the OCP figure recorded during for 21:1.
Seeing Figure 10, Tu10Zhong: a is ammonium chloride and dysprosia mol ratio is the cyclic voltammogram recorded during 42:1, and b is chlorine
Change ammonium and dysprosia mol ratio is the square wave voltammogram (illustration) recorded during 42:1.
Seeing Figure 11, Tu11Zhong: a is ammonium chloride and ytterbium oxide mol ratio is the cyclic voltammogram recorded during 44:1, and b is chlorine
Change ammonium and ytterbium oxide mol ratio is the square wave voltammogram (illustration) recorded during 44:1.
In this experiment, different electrochemistry transient state technical method (cyclic voltammetry, square wave voltammetry and open circuit electricity is utilized
Position method) have studied ammonium chloride as auxiliary reagent, fused salt middle rare earth is carried out the situation of chlorination.Fig. 1 to Figure 11 gives
Measured corresponding voltammogram under ammonium chloride and rare earth oxide different mol ratio and different chlorination temperatures in system.Head from figure
First it is observed that have obvious a pair or two pairs of oxidoreduction peak-to-peak signals, first, this illustrates in fused salt LiCl-KCl system
In, directly utilizing ammonium chloride can be at a temperature of broad and have under inert gas shielding or air atmosphere as auxiliary reagent
Rare earth oxide is carried out ionizing.Secondly, from figure, the rare earth oxide reducing machine to rare earth ion can also be further appreciated that
Reason, as La2O3、CeO2、Tb4O7Deng the diffusion controlled process being reduced to step 3 electronics of transfer of oxide, and some oxide
(such as Nd2O3, Sm2O3, Eu2O3, Yb2O3) two steps (first transfer one electronics, retransfer 2 electronics afterwards) that are reduced to spread
The process controlled.All above information is all demonstrated and is mixed by ammonium chloride and RE oxide powder in fused salt LiCl-KCl
After be laid in fused salt LiCl-KCl interface can preferably realize in air atmosphere at a certain temperature rare earth oxide from
Sonization.
In figure: current is electric current, potential is current potential.
Embodiment 1
The method that a kind of LiCl-KCl molten salt system middle rare earth auxiliary is dissolved, comprises the following steps:
(1), after 44.8g LiCl and 55.2g KCl is weighed being placed in crucible mixing, crucible is placed in Muffle furnace and is dried
Being dehydrated 72 hours, the temperature being dried is 200 DEG C, is dried pretreatment；
(2) heating up in crucible is placed in high temperature resistance furnace, high temperature resistance furnace temperature elevating range is 300-550 DEG C, makes
LiCl and KCl becomes fused salt；
(3) ammonium chloride and RE oxide powder (are taken 2g rare earth oxide and 6g chlorine according to the ratio that mol ratio is 8:1
Compound) mixing after be directly laid in LiCl-KCl fused salt top, in air atmosphere, make in fused salt interface rare earth oxide from
Sonization.
Embodiment 2
The method that a kind of LiCl-KCl molten salt system middle rare earth auxiliary is dissolved, comprises the following steps:
(1) after mixing in 53.76g LiCl and 66.24g KCl is placed on crucible, directly drying and dehydrating 96 in Muffle furnace
Hour, the temperature being dried is 180 DEG C, is dried pretreatment；
(2) heating up in crucible is placed in high temperature resistance furnace, high temperature resistance furnace temperature elevating range is 400-550 DEG C, makes
LiCl and KCl becomes fused salt；
(3) it is first that 11:1 weighs the mixture that gross weight is 10g and puts according to ammonium chloride and RE oxide powder mol ratio
After valve bag, mixing, directly it is laid in LiCl-KCl fused salt top, under air atmosphere, makes rare earth oxide in fused salt interface
Ionizing.
Embodiment 3
The method that a kind of LiCl-KCl molten salt system middle rare earth auxiliary is dissolved, comprises the following steps:
(1), after mixing in 22.4g LiCl and 27.6g KCl is placed on crucible, it is placed directly within drying and dehydrating in Muffle furnace
110 hours, the temperature being dried was 220 DEG C, is dried pretreatment；
(2) heating up in crucible is placed in high temperature resistance furnace, high temperature resistance furnace temperature elevating range is 500-600 DEG C, makes
LiCl and KCl becomes fused salt；
(3) ammonium chloride of 2g oxide and 3.8g is laid in LiCl-KCl fused salt top, in air atmosphere, at fused salt
Interface makes rare earth oxide ionizing.
The present invention, in LiCl-KCl molten salt system, uses ammonium chloride to do chlorination reagent, is directly realized by rare earth oxide
Dissolving presented in rare earth element ion in LiCl-KCl fused salt, ammonium chloride is cracked into gas in the case of being heated and overflows
Go out, it is to avoid being mixed into of impurity element, it is ensured that the purity of molten salt system.The method using the present invention, at LiCl-KCl fused salt
In system, utilize ammonium chloride to carry out the temperature of rare earth oxide ionizing requirement broad, typically can control at 250-550
℃.Secondly rare earth ion easily re-forms oxide or oxychloride in oxidizing atmosphere, and ammonium chloride decomposes generation hydrogen chloride
And ammonia, the effect of oxygen in removal system can be played, prevent inversely carrying out of ionization process.Hence with ammonium chloride from
It is possible not only to during sonization be smoothed out under inert gas shielding, possibly even carries out the most smoothly under air atmosphere.
3rd, ammonium chloride is by being just re-condensed into ammonium chloride when catching a cold after thermal cracking, the ammonia chloride crystal granule of condensation is the most direct
Can come back to molten salt system proceeds assist ionization, or reclaim stand-by.The most not only can be by adding
Surplus auxiliary reagent improves Ionization Efficiency, and recycling or recycling by auxiliary reagent simultaneously improves auxiliary reagent
Service efficiency.Therefore, the present invention has weight for the dissolving of oxide spentnuclear fuel dry method post processing middle rare earth fuel
Want meaning.
The data be given according to table 1 complete embodiment 4-with reference to embodiment 1-3 and implement 13.
Under rare earth oxide that table 1 provides for the embodiment of the present invention and ammonium chloride not jljl mol ratio and different chlorination temperatures
Chlorination efficiency.
Wherein in embodiment 9 and embodiment 11, making rare earth oxide ionizing in fused salt interface is at high-purity indifferent gas
Carry out under the protection of body bubbling.
Chlorination efficiency under table 1 rare earth oxide and ammonium chloride not jljl mol ratio and different chlorination temperature
Although here it is emphasized that utilize this method can be by rare earth oxide ion within the scope of wider temperature
Change, but its chlorination efficiency is all had a major impact by rare earth oxide and the ratio of auxiliary reagent and furnace temperature.When being in equal feelings
During condition (as light, heavy rare-earth oxide quality is suitable, chlorination temperature is identical), the auxiliary reagent that light rare earth chloride oxide need to introduce
More much more than heavy rare-earth oxide.
Although it is last it is noted that the present invention and advantage thereof have been described in detail above it should be appreciated that not
Beyond can carry out in the case of the spirit and scope of the present invention that are defined by the claims appended hereto various change, replacement and
Conversion.And, the scope of the present invention is not limited only to the concrete reality of the process described by description, equipment, means, method and steps
Execute example.One of ordinary skilled in the art will readily appreciate that from the disclosure, can use according to the present invention and hold
The row function essentially identical to corresponding embodiment described herein or obtain the result essentially identical with it, existing and future
Process, equipment, means, method or step to be developed.Therefore, appended claim is directed in the range of them wrapping
Include such process, equipment, means, method or step.
Claims (9)
1. the method that a LiCl-KCl molten salt system middle rare earth auxiliary is dissolved, it is characterised in that comprise the following steps:
(1) it is dried pretreatment after being mixed in crucible by LiCl and KCl；
(2) LiCl and KCl is made to become fused salt to crucible intensification；
(3) LiCl-KCl fused salt top directly it is laid in, in fused salt interface after ammonium chloride and RE oxide powder being mixed
Make rare earth oxide ionizing.
Method the most according to claim 1, it is characterised in that the mass percent of described LiCl and KCl is 44.8:
55.2。
Method the most according to claim 1, it is characterised in that described ammonium chloride and the mol ratio of light rare earth oxide powder
At least 8, the mol ratio of described ammonium chloride and heavy rare-earth oxide powder is at least 13.
Method the most according to claim 1, it is characterised in that the gross mass of described LiCl and KCl and described ammonium chloride and
The total mass ratio of RE oxide powder is 50～150:0～50, except 0.
Method the most according to claim 1, it is characterised in that the dry pretreatment in described step (1) includes: will mixing
LiCl and KCl drying and dehydrating 72-110 hour in Muffle furnace, be dried temperature be 180-300 DEG C.
Method the most according to claim 5, it is characterised in that also include: at air atmosphere or high purity inert gas drum
Under bubble protection, carry out rare earth oxide ionization process.
7. according to the method described in any one of claim 1-6, it is characterised in that described step (2) including: crucible is placed in height
Heat up in temperature resistance furnace.
Method the most according to claim 7, it is characterised in that described high temperature resistance furnace temperature elevating range is 250-550 DEG C.
Method the most according to claim 7, it is characterised in that described RE oxide powder is selected from following rare earth element:
Cerium Ce, neodymium Nd, samarium Sm, europium Eu, terbium Tb, lanthanum La, gadolinium Gd, dysprosium Dy, holmium Ho, erbium Er or ytterbium Yb.
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Cited By (5)
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| CN107572573A (en) * | 2017-10-26 | 2018-01-12 | 贵州大学 | A kind of preparation method of the nano ceric oxide particle of polyhedral structure |
| CN107601546A (en) * | 2017-10-26 | 2018-01-19 | 贵州大学 | A kind of environment-friendly preparation method thereof of nano ceric oxide particle |
| CN108364703A (en) * | 2018-01-23 | 2018-08-03 | 中国科学院高能物理研究所 | Application of the ammonium chloride in uranium dioxide is detached with lanthanide oxide |
| CN109682870A (en) * | 2019-01-09 | 2019-04-26 | 中国原子能科学研究院 | The method and device of concentration of metal ions in a kind of measurement fused salt |
| CN111099659A (en) * | 2019-12-20 | 2020-05-05 | 中国科学院高能物理研究所 | Preparation method and application of pentavalent uranium |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107572573A (en) * | 2017-10-26 | 2018-01-12 | 贵州大学 | A kind of preparation method of the nano ceric oxide particle of polyhedral structure |
| CN107601546A (en) * | 2017-10-26 | 2018-01-19 | 贵州大学 | A kind of environment-friendly preparation method thereof of nano ceric oxide particle |
| CN108364703A (en) * | 2018-01-23 | 2018-08-03 | 中国科学院高能物理研究所 | Application of the ammonium chloride in uranium dioxide is detached with lanthanide oxide |
| CN108364703B (en) * | 2018-01-23 | 2019-09-17 | 中国科学院高能物理研究所 | Application of the ammonium chloride in uranium dioxide is separated with lanthanide oxide |
| CN109682870A (en) * | 2019-01-09 | 2019-04-26 | 中国原子能科学研究院 | The method and device of concentration of metal ions in a kind of measurement fused salt |
| CN111099659A (en) * | 2019-12-20 | 2020-05-05 | 中国科学院高能物理研究所 | Preparation method and application of pentavalent uranium |
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| CN105819486B (en) | 2017-07-07 |
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