CN102553664B - Molten salt electrochemical experimental apparatus - Google Patents
Molten salt electrochemical experimental apparatus Download PDFInfo
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- CN102553664B CN102553664B CN 201210003346 CN201210003346A CN102553664B CN 102553664 B CN102553664 B CN 102553664B CN 201210003346 CN201210003346 CN 201210003346 CN 201210003346 A CN201210003346 A CN 201210003346A CN 102553664 B CN102553664 B CN 102553664B
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Abstract
The invention discloses a molten salt electrochemical experimental apparatus. The molten salt electrochemical experimental apparatus comprises a glove box filled with inert gas, a transition connection pipe and a vacuum tube furnace. The transition connection pipe is arranged between the glove box and the gas inlet end of the vacuum tube furnace and is respectively connected with the glove box and the gas inlet end of the vacuum tube furnace. According to the molten salt electrochemical experimental apparatus disclosed by the invention, the anhydrous and oxygen-free environmental environment can be provided for a high temperature molten salt electrochemical experiment by utilizing the atmosphere of the inert gas in the glove box. The experimental apparatus further has a function of carrying out pre-dissolving bubble elimination and recrystallization purification on molten salt electrolyte. Meanwhile, due to the design of the transition connection pipe, the experimental apparatus can also be used for carrying out operations of opening, cleaning, disassembling and replacing a furnace tube on the premise of not influencing the normal work of the glove box.
Description
Technical field
The present invention relates to a kind of molten salt electrochemical experimental apparatus, particularly relate to and a kind ofly can provide for melten salt electriochemistry experiment the molten salt electrochemical experimental apparatus of the experimental situation of anhydrous, anaerobic.
Background technology
The high-temperature molten salt electrochemical techniques have many important application at chemical field, as maximum electrochemistry metallurgical industry---the aluminium electrolytic industry in the whole world, carry out electrolysis and obtain metallic aluminium in the fluorine molten salt system.In addition, in nuclear power industry, spentnuclear fuel also usually adopts the molten-salt electrolysis Scouring Technology to process nuclear fuels such as reclaiming metallic uranium, plutonium, thorium.Molten salt electrolyte belongs to the electrolyte of non-aqueous system, has very wide electrochemical window and chemical stability, and this is also the basic reason that molten salt electrolyte is widely adopted.Yet, because traditional melten salt electriochemistry device is very easy to absorb airborne oxygen and moisture, oxygen and moisture can cause the melten salt electriochemistry window to reduce or fused salt is decomposed, and the existence of oxygen also can be accelerated the corrosion rate of various device material in hot environment.Therefore, traditional melten salt electriochemistry device can make the problem that oxygen disturbs of usually meeting in melten salt electriochemistry industry or experimental study near water, has increased no small difficulty to the melten salt electriochemistry experimental study that originally just is difficult to carry out.
Summary of the invention
The technical problem to be solved in the present invention is easily to absorb the defect of oxygen and moisture in air in order to overcome melten salt electriochemistry device in prior art, provides a kind of the molten salt electrochemical experimental apparatus of the experimental situation of anhydrous, anaerobic can be provided for the melten salt electriochemistry experiment.
The present invention solves above-mentioned technical problem by following technical proposals:
The invention provides a kind of molten salt electrochemical experimental apparatus, this molten salt electrochemical experimental apparatus comprises a vacuum tube furnace, its characteristics are, this molten salt electrochemical experimental apparatus also comprises that one is full of the glove box of inert gas, and this glove box is connected with the inlet end of this vacuum tube furnace.The present invention is connected glove box and vacuum tube furnace, and make the inert gas of this glove box inside enter this vacuum tube furnace from the inlet end of this vacuum tube furnace, be full of inert gas thereby make in vacuum tube furnace, for the high-temperature molten salt electrochemistry experiment carried out in vacuum tube furnace provides experimental situation anhydrous, anaerobic.
Preferably, this molten salt electrochemical experimental apparatus also comprises a transition connecting pipe, and this transition connecting pipe is arranged between the inlet end of this glove box and this vacuum tube furnace, and with the inlet end of this glove box and this vacuum tube furnace, be connected respectively.
Preferably, the two ends of this transition connecting pipe are communicated with flange by one respectively and are connected with the inlet end of this glove box and this vacuum tube furnace, also can be so that carry out electro-chemical test in the melten salt electriochemistry pond of measurement electrode in stretching into this vacuum tube furnace by the hole of this connection flange when the experimental situation of anhydrous, anaerobic is provided.
Preferably, one end of this transition connecting pipe is connected with this glove box by a middle adpting flange that is provided with a sealing blind, the other end is communicated with flange by one and is connected with the inlet end of this vacuum tube furnace, this molten salt electrochemical experimental apparatus also comprises an air extractor, when being communicated with this glove box, this air extractor is not communicated with this transition connecting pipe, while being communicated with this transition connecting pipe, with this glove box, be not communicated with, thereby by this air extractor, this molten salt electrochemical experimental apparatus is bled and the tonifying Qi operation, the gas that is about to this melten salt electriochemistry reaction generation is extracted out from this molten salt electrochemical experimental apparatus, and be disconnected each other be provided with the adpting flange sealing of a sealing blind by this centre between this transition connecting pipe and this glove box in the process of bleeding after, so the inert gas in this glove box can only be supplemented in this vacuum tube furnace by this air extractor.
Preferably, this air extractor comprises one first path, an alternate path and a vavuum pump, these the first path two ends are connected with this vavuum pump and this transition connecting pipe respectively, these alternate path two ends are connected with this first path and this glove box respectively, and the delivery position of this first path and this alternate path is provided with one for switching the reversal valve of this first path and this alternate path.Utilize reversal valve, just can guarantee to bleed and two kinds of operations of tonifying Qi only can be carried out a kind ofly at one time, the gas of having avoided molten salt react ion to produce mixes mutually with the inert gas in glove box.
Preferably, molten salt electrochemical experimental apparatus also comprises the adpting flange that is provided with a sealing blind in the middle of, the blind end of this adpting flange and this vacuum tube is tightly connected, thus can do not affect under the prerequisite of glove box normal operation to vacuum tube furnace opened, the operations such as cleaning and dismounting and change.
Positive progressive effect of the present invention is: molten salt electrochemical experimental apparatus of the present invention utilizes the atmosphere of inert gas in glove box, can be for the high-temperature molten salt electrochemistry experiment provides experimental situation anhydrous, anaerobic, this experimental provision also possesses the function of molten salt electrolyte being carried out to predissolve exhaust bubble and recrystallization purifying.Simultaneously, the design of transition connecting pipe make this experimental provision can also do not affect under the prerequisite of glove box normal operation to boiler tube opened, the operations such as cleaning and dismounting and change.
The accompanying drawing explanation
The structure chart of the molten salt electrochemical experimental apparatus that Fig. 1 is the first embodiment of the present invention.
The structure chart of the molten salt electrochemical experimental apparatus that Fig. 2 is the second embodiment of the present invention.
The specific embodiment
Provide preferred embodiment of the present invention below in conjunction with accompanying drawing, to describe technical scheme of the present invention in detail.
The first embodiment:
As shown in Figure 1, the molten salt electrochemical experimental apparatus of the present embodiment comprise a glove box 1, a transition connecting pipe 2, a vacuum tube furnace 3, two be communicated with flange 4 and an adpting flange 5, the centre of this adpting flange 5 is provided with a sealing blind, thereby can will be connected to two devices sealing mutually at these adpting flange 5 two ends.
Wherein, this transition connecting pipe 2 is communicated with flange 4 by two and is connected with the inlet end of this glove box 1 and this vacuum tube furnace 3 respectively, and the blind end of this vacuum tube furnace 3 also is tightly connected with another sealing flange 5, herein inlet end namely the inert gas in this glove box 1 enter that end that this vacuum tube furnace 3 passes through, blind end is exactly that end corresponding with inlet end.
And be full of inert gas in this glove box 1, by this transition connecting pipe 2, make inert gas enter this vacuum tube furnace 3, for the reaction of the melten salt electriochemistry in this vacuum tube furnace 3 provides experimental situation anhydrous, anaerobic.Wherein, be provided with the vertical furnace tube 31 identical with the fused salt tube furnace of traditional confession melten salt electriochemistry reaction in this vacuum tube furnace 3, outside is provided with the encircling type resistance furnace 32 that hot environment is provided for melten salt electriochemistry reaction, and just is placed in the constant temperature working region that this encircling type resistance furnace 32 produces in this vertical furnace tube 31 for the melten salt electriochemistry pond of melten salt electriochemistry reaction.
Be connected with this glove box 1 because this transition connecting pipe 2 is communicated with flange 4 by this, in this case, can stretch in the melten salt electriochemistry pond and carry out electro-chemical test by the hole on this connection flange 4 by a measurement electrode.
The second embodiment:
As shown in Figure 2, the molten salt electrochemical experimental apparatus of the present embodiment comprises that a glove box 1, a transition connecting pipe 2, a vacuum tube furnace 3, are communicated with flange 4, two adpting flanges 5 and air extractors 6.And the difference of the present embodiment and the first embodiment is: the molten salt electrochemical experimental apparatus of the present embodiment also comprises an air extractor 6, and this transition connecting pipe 2 is tightly connected with this glove box 1 by an adpting flange 5.
Wherein this air extractor comprises one first path 61, an alternate path 62, a vavuum pump 63 and a reversal valve 64.The two ends of this first path 61 are connected with this vavuum pump 63 and this transition connecting pipe 2 respectively, these alternate path 62 two ends are connected with this first path 61 and this glove box 1 respectively, and this first path 61 is provided with for switching this reversal valve 64 of this first path 61 and this alternate path 62 with the delivery position of this alternate path 62.Like this, this air extractor 6 will not be communicated with this transition connecting pipe 2 when being communicated with this glove box 1, while being communicated with this transition connecting pipe 2, with this glove box 1, be not communicated with,
By this air extractor 6, just can be bled and the tonifying Qi operation to this molten salt electrochemical experimental apparatus, the gas that is about to this melten salt electriochemistry reaction generation is extracted out from this molten salt electrochemical experimental apparatus, and this transition connecting pipe 2 is disconnected each other after being tightly connected by this adpting flange 5 with this glove box 1 in the process of bleeding, so the inert gas in this glove box can only be supplemented in this vacuum tube furnace 3 through this transition connecting pipe 2 by this air extractor 6, thereby reacts experimental situation anhydrous, anaerobic is provided for melten salt electriochemistry.Utilize this reversal valve 64, just can guarantee to bleed and two kinds of operations of tonifying Qi only can be carried out a kind ofly at one time, the gas of having avoided molten salt react ion to produce mixes mutually with the inert gas in glove box 1.
Utilizing 6 pairs of these vacuum tube furnaces 3 of this air extractor constantly to be bled operates and the operation that stops bleeding after reaching the certain vacuum degree, just can be in this vacuum tube furnace 3 keep the vacuum constant during intensification heating for dissolving fused salt solid, and the operation of being bled every now and then, will guarantee the fused salt solid dissolve fully and bubble also arrange fully into.Simultaneously, after the fused salt solid dissolves fully, by these 3 insulation a period of times of vacuum tube furnace, then utilize the temperature control program to the slow segmentation cooling of this vacuum tube furnace 3, will make molten salt electrolyte obtain purifying in the process of cooling recrystallization.
Wherein, in the molten salt electrochemical experimental apparatus of the present embodiment, owing to adopting an adpting flange 5 to be sealed between this transition connecting pipe 2 and this glove box 1, just can guarantee that the inert gas in this glove box 1 is not subject to air impact.Like this, just can open successively the adpting flange 5 of the blind end of encircling type resistance furnace 32, this vacuum tube furnace 3, inwall to this vacuum tube furnace 3 is swept cleaning, seal the adpting flange 5 of this blind end after having cleaned, encircling type resistance furnace 32 again closes, and utilize the tonifying Qi 3 times of repeatedly bleeding of 6 pairs of these vacuum tube furnaces 3 of this air extractor, and just completed the cleaning operation of vacuum tube furnace 3 boiler tubes, and also similar with cleaning operation for the disassembling section step of the boiler tube of vacuum tube furnace 3.
Although more than described the specific embodiment of the present invention, it will be understood by those of skill in the art that these only illustrate, protection scope of the present invention is limited by appended claims.Those skilled in the art, under the prerequisite that does not deviate from principle of the present invention and essence, can make various changes or modifications to these embodiments, but these changes and modification all fall into protection scope of the present invention.
Claims (4)
1. a molten salt electrochemical experimental apparatus, this molten salt electrochemical experimental apparatus comprises a vacuum tube furnace, it is characterized in that, and this molten salt electrochemical experimental apparatus also comprises that one is full of the glove box of inert gas, and this glove box is connected with the inlet end of this vacuum tube furnace;
This molten salt electrochemical experimental apparatus also comprises a transition connecting pipe, and this transition connecting pipe is arranged between the inlet end of this glove box and this vacuum tube furnace, and with the inlet end of this glove box and this vacuum tube furnace, be connected respectively;
The adpting flange that one end of this transition connecting pipe is provided with a sealing blind by a centre is connected with this glove box, the other end is communicated with flange by one and is connected with the inlet end of this vacuum tube furnace, this molten salt electrochemical experimental apparatus also comprises an air extractor, be not communicated with this transition connecting pipe when this air extractor is communicated with this glove box, be not communicated with this glove box while being communicated with this transition connecting pipe.
2. molten salt electrochemical experimental apparatus as claimed in claim 1, is characterized in that, the two ends of this transition connecting pipe are communicated with flange by one respectively and are connected with the inlet end of this glove box and this vacuum tube furnace.
3. molten salt electrochemical experimental apparatus as claimed in claim 1, it is characterized in that, this air extractor comprises one first path, an alternate path and a vavuum pump, these the first path two ends are connected with this vavuum pump and this transition connecting pipe respectively, these alternate path two ends are connected with this first path and this glove box respectively, and the delivery position of this first path and this alternate path is provided with one for switching the reversal valve of this first path and this alternate path.
4. molten salt electrochemical experimental apparatus as described as any one in claim 1-3, is characterized in that, molten salt electrochemical experimental apparatus also comprises the adpting flange that is provided with a sealing blind in the middle of, and the blind end of this adpting flange and this vacuum tube furnace is tightly connected.
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| CN 201210003346 CN102553664B (en) | 2012-01-06 | 2012-01-06 | Molten salt electrochemical experimental apparatus |
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| CN 201210003346 CN102553664B (en) | 2012-01-06 | 2012-01-06 | Molten salt electrochemical experimental apparatus |
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| CN102553664B true CN102553664B (en) | 2013-12-18 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1246897A (en) * | 1997-02-04 | 2000-03-08 | 卡思英戈特斯有限公司 | Process for electrolytic production of metals |
| CN201024217Y (en) * | 2006-12-06 | 2008-02-20 | 北京有色金属研究总院 | Semi-continuous fused salt electrolytic refining device |
| CN101275251A (en) * | 2007-03-30 | 2008-10-01 | 北京有色金属研究总院 | Method for preparing titanium alloy by fused salt electrolysis |
| CN202460640U (en) * | 2012-01-06 | 2012-10-03 | 中国科学院上海应用物理研究所 | Electrochemistry experiment device for fused salt |
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2012
- 2012-01-06 CN CN 201210003346 patent/CN102553664B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1246897A (en) * | 1997-02-04 | 2000-03-08 | 卡思英戈特斯有限公司 | Process for electrolytic production of metals |
| CN201024217Y (en) * | 2006-12-06 | 2008-02-20 | 北京有色金属研究总院 | Semi-continuous fused salt electrolytic refining device |
| CN101275251A (en) * | 2007-03-30 | 2008-10-01 | 北京有色金属研究总院 | Method for preparing titanium alloy by fused salt electrolysis |
| CN202460640U (en) * | 2012-01-06 | 2012-10-03 | 中国科学院上海应用物理研究所 | Electrochemistry experiment device for fused salt |
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