CN101471446A - Low-melting-point high-conductivity molten salt electrolyte and preparation method thereof - Google Patents
Low-melting-point high-conductivity molten salt electrolyte and preparation method thereof Download PDFInfo
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- CN101471446A CN101471446A CN 200710304285 CN200710304285A CN101471446A CN 101471446 A CN101471446 A CN 101471446A CN 200710304285 CN200710304285 CN 200710304285 CN 200710304285 A CN200710304285 A CN 200710304285A CN 101471446 A CN101471446 A CN 101471446A
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Abstract
The invention relates to a molten salt electrolyte and the preparation method thereof. The molten salt electrolyte contains LiCl (purity equal to or larger than 97.0%) 19.0 to 28.5 wt%, KCl (purity equal to or larger than 99.8%) 21.5 to 33.0 wt%, LiBr (purity equal to or larger than 98.0%) 11.5 to 21.0 wt%; KBr (purity equal to or larger than 99.0%) 9.8 to 19.5 wt%, LiF (purity equal to or larger than 99.0%) 1.5 to 8.5 wt% and KF (purity equal to or larger than 99.0%) 4.0 to 14.5 wt%. The molten salt electrolyte has a melting point of 275 to 286 DEG C, conductivity of 1.18 to 1.25 S*cm<-1>, and water content not more than 0.5%.
Description
Technical field
The present invention relates to a kind of low-melting-point high-conductivity molten salt electrolyte and preparation method thereof, particularly a kind of molten salt electrolyte that is used for military thermal cell and preparation method thereof.
Background technology
Thermal cell is molten salt electrolyte battery or thermally activated battery again, is a kind of reserve type battery.It is compared with general chemical cell, make electrolyte owing to adopt fuse salt, has unique advantage: reliability height, activationary time short (≤0.5 second), period of storage long (10-15 or longer), internal resistance is little, can discharge by heavy current pulse, be not subjected to the influence of ambient temperature and installation direction during use, have the good mechanical performance, be the battery that uses most convenient in the current military battery, be widely used in guided missile, dispense armament systems such as device and nuclear weapon.
The performance of thermal cell plays crucial effects to the use and the storge quality of armament systems.Molten salt electrolyte performance quality has directly determined the quality of battery performance, reduce molten salt electrolyte fusing point, improve its conductance and thermal stability is one of important channel of improving the thermal cell performance.
Though at present domestic and international scientific worker has carried out a large amount of bases and application study to the molten salt electrolyte of low melting point, high conductivity, but the low-melting-point high-conductivity electrolyte system is imperfection very still, be mainly reflected in: though fusing point has lowered, but conductivity and stability are still not high, still need further study.
The main at present LiCl-KCl eutectic salt system that uses of the domestic high specific energy of developing, high-power, long-life thermal cell, its molten salt system, its fusing point is 352 ℃, conductivity is 0.95Scm
-1, press for the molten salt system of development low melting point high conductivity, to satisfy China's weaponry with the needs of novel thermal cell to the molten-salt electrolysis material.
Summary of the invention
One of purpose of the present invention provides a kind of molten salt electrolyte with low-melting-point high-conductivity and Heat stability is good.
Above-mentioned purpose of the present invention reaches by the following technical programs:
A kind of molten salt electrolyte is characterized in that this molten salt electrolyte comprises: LiCl (purity 〉=97.0%): 19.0-28.5 weight %; KCl (purity 〉=99.8%): 21.5-33.0 weight %; LiBr (purity 〉=98.0%): 11.5-21.0 weight %; KBr (purity 〉=99.0%): 9.8-19.5 weight %; LiF (purity 〉=99.0%): 1.5-8.5 weight % and KF (purity 〉=99.0%): 4.0-14.5 weight %.
A kind of optimal technical scheme is characterized in that: the water content of described molten salt electrolyte≤0.5%.
Another object of the present invention provides a kind of preparation method of above-mentioned molten salt electrolyte.
Above-mentioned purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of molten salt electrolyte, its step is as follows:
(1) choose LiCl, KCl, LiBr, KBr, LiF and KF, carry out vacuum dehydration respectively, dewater to water content≤0.5%, weigh batching mixes or is ground to material fully mixing in proportion;
(2) step (1) gained mixture is placed crucible, slowly be heated to 120 ℃-200 ℃, be incubated 1-3 hour, to remove the moisture in the material, be warming up to 650-850 ℃ then, material melting during this period, volatile ingredient wherein fully volatilizees and removes, stop heating, nature or forced cooling are to room temperature;
(3) the material piece in the taking-up crucible is 1-3mm with crusher in crushing to average particle size earlier, and being crushed to particle mean size with ceramic pulverizer again is below the 150 μ m, promptly gets product.
Get prepared fuse salt a little, place crucible, be heated to fusing, its fusing point is determined in range estimation, or uses derivatograph to measure its fusing point.Use digital electric bridge to measure its conductivity.Use thermogravimetric analyzer to measure its water content.
Above-mentioned batching, preparation and measuring process are all carried out in the dry environment of relative humidity (RH)≤2%.
Beneficial effect:
The fusing point of molten salt electrolyte of the present invention is 275-286 ℃, and conductivity is 1.18-1.25Scm
-1, its water content is no more than 0.5%.
The present invention will be further described below by embodiment, but and do not mean that limiting the scope of the invention.
Embodiment
Embodiment 1
A kind of low melting point, high-conductivity molten salt electrolyte, ingredient groups becomes: LiCl (purity 〉=97.0%): 23.8 weight %, KCl (purity 〉=99.8%): 31.0 weight %, LiBr (purity 〉=98.0%): 17.3 weight %, KBr (purity 〉=99.0%): 15.6 weight %, LiF (purity 〉=99.0%): 4.8 weight % and KF weight (purity 〉=99.0%): 7.5 weight %.Raw material reagent all uses vacuum drying chamber 85 ℃ of following vacuumizes 2 hours, weighing in the dry environment of RH≤2%, with agate mortar be ground to full and uniform after, put into melting furnace, slowly be warming up to 250 ℃, the material that mixes is further dewatered, be warming up to 700 ℃ then, under this temperature, be incubated 2h, stop heating, cool to room temperature.The fused salt that obtains is carried out fragmentation and grinding, obtain low melting point of the present invention, high conductivity molten salt electrolyte.
Above process is all carried out in the dry environment of RH≤2%.
Use derivatograph to measure its fusing point.Use digital electric bridge to measure its conductivity.Use thermogravimetric analyzer to measure its water content.The fusing point of gained molten salt electrolyte is 275 ℃, and conductivity is 1.22Scm
-1, its water content is 0.22%.
Embodiment 2
A kind of low melting point, high-conductivity molten salt electrolyte, ingredient groups becomes: LiCl (purity 〉=97.0%): 24.5 weight %, KCl (purity 〉=99.8%): 31.9 weight %, LiBr (purity 〉=98.0%): 15.1 weight %, KBr (purity 〉=99.0%): 15.6 weight %, LiF (purity 〉=99.0%): 4.7 weight % and KF (purity 〉=99.0%): 8.2 weight %.Raw material reagent all uses vacuum drying chamber 90 ℃ of following vacuumizes 1.5 hours, weighing in the dry environment of RH≤2%, with agate mortar be ground to full and uniform after, put into melting furnace, slowly be warming up to 270 ℃, the material that mixes is further dewatered, be warming up to 720 ℃ then, under this temperature, be incubated 2.5h, stop heating, cool to room temperature.The fused salt that obtains is carried out fragmentation and grinding, obtain low melting point of the present invention, high conductivity molten salt electrolyte.
Above process is all carried out in the dry environment of RH≤2%.
Use derivatograph to measure its fusing point.Use digital electric bridge to measure its conductivity.Use thermogravimetric analyzer to measure its water content.The fusing point of gained fused salt is 282 ℃, and conductivity is 1.18Scm
-1, its water content is 0.18%.
Embodiment 3
A kind of low melting point, high-conductivity molten salt electrolyte, ingredient groups becomes: LiCl (purity 〉=97.0%): 26.8 weight %, KCl (purity 〉=99.8%): 29.3 weight %, LiBr (purity 〉=98.0%): 17.3 weight %, KBr (purity 〉=99.0%): LiF (purity 〉=99.0%) 12.7%: 3.8 weight % and KF (purity 〉=99.0%): 10.1 weight %.Raw material reagent all uses vacuum drying chamber 110 ℃ of following vacuumizes 2.5 hours, weighing in the dry environment of RH≤2%, with agate mortar be ground to full and uniform after, put into melting furnace, slowly be warming up to 290 ℃, the material that mixes is further dewatered, be warming up to 740 ℃ then, under this temperature, be incubated 2h, stop heating, cool to room temperature.The fused salt that obtains is carried out fragmentation and grinding, obtain low melting point of the present invention, high conductivity molten salt electrolyte.
Above process is all carried out in the dry environment of RH≤2%.
Use derivatograph to measure its fusing point.Use digital electric bridge to measure its conductivity.Use thermogravimetric analyzer to measure its water content.The fusing point of gained fused salt is 286 ℃, and conductivity is 1.25Scm
-1, its water content is 0.33%.
Claims (3)
1, a kind of molten salt electrolyte is characterized in that this molten salt electrolyte comprises: LiCl:19.0-28.5 weight %; KCl:21.5-33.0 weight %; LiBr:11.5-21.0 weight %; KBr:9.8-19.5 weight %; LiF:1.5-8.5 weight % and KF:4.0-14.5 weight %.
2, molten salt electrolyte according to claim 1 is characterized in that: the water content of described molten salt electrolyte≤0.5%.
3, the preparation method of molten salt electrolyte according to claim 1 and 2, its step is as follows:
(1) choose LiCl, KCl, LiBr, KBr, LiF and KF, carry out vacuum dehydration respectively, dewater to water content≤0.5%, weigh batching mixes or is ground to material fully mixing in proportion;
(2) step (1) gained mixture is placed crucible, slowly be heated to 120 ℃-200 ℃, be incubated 1-3 hour, to remove the moisture in the material, be warming up to 650-850 ℃ then, material melting during this period, volatile ingredient wherein fully volatilizees and removes, stop heating, nature or forced cooling are to room temperature;
(3) the material piece in the taking-up crucible is 1-3mm with crusher in crushing to average particle size earlier, and being crushed to particle mean size with ceramic pulverizer again is below the 150 μ m, promptly gets product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102148353A (en) * | 2010-02-10 | 2011-08-10 | 上海空间电源研究所 | Special modified negative pole material for thermal battery and preparation method thereof |
| CN106328966A (en) * | 2016-08-25 | 2017-01-11 | 中南大学 | Thermal battery electrolyte containing metal particles and preparation method and application of thermal battery electrolyte |
| CN107895795A (en) * | 2017-12-06 | 2018-04-10 | 贵州梅岭电源有限公司 | A kind of thermal cell superelevation electrode potential positive electrode and preparation method thereof |
| CN107978767A (en) * | 2017-12-06 | 2018-05-01 | 贵州梅岭电源有限公司 | A kind of thermal cell sulfenyl electrolyte preparation method |
| CN109841821A (en) * | 2019-03-18 | 2019-06-04 | 贵州梅岭电源有限公司 | A kind of high potential high-power type thermal cell positive electrode and preparation method thereof |
| CN110212208A (en) * | 2019-04-30 | 2019-09-06 | 中国电子科技集团公司第十八研究所 | Electrolyte material for storage thermal battery |
-
2007
- 2007-12-26 CN CN 200710304285 patent/CN101471446A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102148353A (en) * | 2010-02-10 | 2011-08-10 | 上海空间电源研究所 | Special modified negative pole material for thermal battery and preparation method thereof |
| CN106328966A (en) * | 2016-08-25 | 2017-01-11 | 中南大学 | Thermal battery electrolyte containing metal particles and preparation method and application of thermal battery electrolyte |
| CN106328966B (en) * | 2016-08-25 | 2019-04-09 | 中南大学 | A kind of thermal battery electrolyte of containing metal particle and its preparation method and application |
| CN107895795A (en) * | 2017-12-06 | 2018-04-10 | 贵州梅岭电源有限公司 | A kind of thermal cell superelevation electrode potential positive electrode and preparation method thereof |
| CN107978767A (en) * | 2017-12-06 | 2018-05-01 | 贵州梅岭电源有限公司 | A kind of thermal cell sulfenyl electrolyte preparation method |
| CN107895795B (en) * | 2017-12-06 | 2020-09-11 | 贵州梅岭电源有限公司 | Ultrahigh electrode potential positive electrode material for thermal battery and preparation method thereof |
| CN109841821A (en) * | 2019-03-18 | 2019-06-04 | 贵州梅岭电源有限公司 | A kind of high potential high-power type thermal cell positive electrode and preparation method thereof |
| CN110212208A (en) * | 2019-04-30 | 2019-09-06 | 中国电子科技集团公司第十八研究所 | Electrolyte material for storage thermal battery |
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