CN102229435A - Synthetic method for lithium iodide for cell and preparation method for electrolyte of lithium iodide - Google Patents
Synthetic method for lithium iodide for cell and preparation method for electrolyte of lithium iodide Download PDFInfo
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- CN102229435A CN102229435A CN2010105819834A CN201010581983A CN102229435A CN 102229435 A CN102229435 A CN 102229435A CN 2010105819834 A CN2010105819834 A CN 2010105819834A CN 201010581983 A CN201010581983 A CN 201010581983A CN 102229435 A CN102229435 A CN 102229435A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to a synthetic method for lithium iodide for cells and a preparation method for an electrolyte of lithium iodide, belonging to the filed of batteries. The synthetic method for lithium iodide comprises the following steps: using lithium hydroxide or lithium carbonate and hydroiodic acid as raw materials to prepare a crude product of lithium iodide; dissolving the crude product of lithium iodide in an organic solvent in a glove box and adjusting the pH value of the solution to between 1 and 6; carrying out filtering; carrying out reduced pressure distillation for 0.5 to 50 hours; cooling the product of the distillation to normal temperature so as to obtain battery-grade white solid lithium iodide. The organic electrolyte of lithium iodide is obtained by dissolving the synthesized lithium iodide in an organic solvent. The synthesized battery-grade lithium iodide in the invention has a high purity and low moisture, and can be utilized for injection into cells after addition into an organic solvent without dewatering.
Description
Technical field
The present invention relates to technical field of lithium batteries, relate in particular to the preparation method of a kind of battery and electrolytic solution synthetic with lithium iodide.
Background technology
Usually lithium iodide has three crystal water, be heated to 73 ℃ and lose a part crystal water, lose two molecular crystal water to 80 ℃, the 3rd crystal water is difficult to remove, and the preparation lithium iodide often is being mingled with a large amount of impurity such as Lithium Oxide 98min, Quilonum Retard, elemental iodine etc. in the industrial and laboratory; And last crystal water of lithium iodide often removes not thoroughly, has in the lithium iodide electrolytic solution that causes preparing out that insolubles, moisture are higher, color is reddish black.
Chinese literature " preparation of high-purity lithium iodide "--Xinzhou teacher training school journal--Zhao Zhigang, appoint bright--2002 (2) [1] and " new preparation method of anhydrous lithium iodide "--yellow pivot, Tong Zhiping, Tian Baozhi--chemical reagent---1991,13 (5) [2] discloses the preparation method of two kinds of lithium iodides.Its technical scheme is respectively: prepare lithium iodide 2Li+2NH by metallic lithium and ammonium iodide
4↑=2LiI+NH
3+ H
2↑ and sodium iodide and the method for lithium chloride in anhydrous propanone prepare lithium iodide LiC1+NaI → LiI+NaC1 ↓.But, the reaction unit complexity of these two kinds of methods, severe reaction conditions is difficult to control; The price of metallic lithium is higher simultaneously, and lithium iodide purity of producing and moisture content are difficult to satisfy the requirement of electrolytic solution; The electrolytic solution moisture height that makes contains insolubles, and color is dark, influences the chemical property of battery.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of battery and electrolytic solution synthetic with lithium iodide, the technical problem of its solution is the lithium iodide of preparing by the inventive method and the organic electrolyte cost is low, moisture is low, purity height, process optimization and good stability.
A kind of battery lithium iodide preparation method comprises being prepared as follows step:
The thick product preparation of step 1 lithium iodide
1.1 with lithium hydroxide or Quilonum Retard and hydriodic acid aqueous solution is reaction raw materials, raw material addition ratio 1: 1, and control drips feed rate remains between 30 ℃-70 ℃ temperature of reaction;
1.2 with a hydronium(ion) oxidation lithium or hydroiodic acid HI regulating step 1.1 gained solution pH values is 1-6, makes solution be the water white transparency state;
1.3 step 1.2 gained solution is removed by filter impurity;
1.4 mother liquid obtained decompression of step 1.3 added thermal distillation, and keep-uping pressure is warming up to 80 ℃-150 ℃ under the condition of-0.1MPa, insulation 0.5h-50h;
1.5 step 1.4 products therefrom is cooled to normal temperature, charge into nitrogen protection, obtain the crude product that lithium iodide white is mingled with light yellow solid;
The preparation of step 2 anhydrous lithium iodide
2.1 in being full of the glove box of high pure nitrogen the thick product of lithium iodide is dissolved in the organic solvent, the hydriodic acid aqueous solution 1-200 of dropping 45% drips, and stirs;
2.2 step 2.1 gained solution is removed by filter impurity;
2.3 in glove box, mother liquid obtained decompression of step 2.2 added thermal distillation, keep-ups pressure after being warming up to 150 ℃-300 ℃ under the condition of-0.1MPa constant temperature 0.5h-50h;
2.4 step 2.3 products therefrom is cooled to normal temperature, charge into nitrogen protection, obtain the anhydrous lithium iodide white solid.
Further, the organic solvent of described dissolving crude product is alcohols or ethers.
Further, described alcohols is at least a in methyl alcohol, ethanol, propyl alcohol, Virahol or the butanols; Described ethers is at least a in ether, methyl ethyl ether, ethylene glycol monoemethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether, dioxolane or the dioxane.
The present invention also comprises a kind of battery method for preparation of lithium iodide organic electrolytic solution, comprises being prepared as follows step:
Step 1 is used the electrolytic solution organic solvent
Molecular sieve precipitation makes organic solvent moisture content be lower than 10ppm;
Step 2 is refrigerated to 0 ℃-10 ℃ with the electrolytic solution organic solvent;
Step 3 will be dissolved in the electrolytic solution organic solvent according to the anhydrous lithium iodide that the described battery of claim 1-3 is prepared with the lithium iodide preparation method, obtains lithium iodide organic electrolytic solution.
Further, described organic electrolyte is made up of organic solvent and lithium iodide; Wherein, organic solvent is two or more the mixture in glycol dimethyl ether, diethylene glycol dimethyl ether, dioxolane, dioxane, propylene carbonate, methylcarbonate, Methyl ethyl carbonate or the diethyl carbonate.
Further, described battery with lithium iodide organic electrolytic solution preparation be at dew point less than under-40 ℃, the environment of oxygen level less than 2ppm, the lithium iodide finished product be dissolved in prepare in the organic electrolyte solvent.
The preparation method of the battery that provides of the present invention and electrolytic solution synthetic with lithium iodide has the following advantages: the anhydrous lithium iodide of preparing by this technology and the organic electrolyte cost is low, moisture is low, purity height, process optimization, good stability and cheap.
Embodiment
Several embodiments of the present invention are described below, further understand the present invention.
Embodiment 1
Get a hydronium(ion) oxidation lithium 42g (1mol) in there-necked flask, adding 42g deoxygenation distilled water is partly dissolved a hydronium(ion) oxidation lithium, stirring becomes suspension, slowly drips 45% hydriodic acid aqueous solution 300g (1mol HI), make temperature be controlled at＜45 ℃ scope in; Dropwise the back and stirred 10 minutes, regulate between the above-mentioned solution pH value 3-4, make solution be water white transparency with a hydronium(ion) oxidation lithium and hydroiodic acid HI; Gained solution is carried out suction filtration, leach after the impurity, mother liquor is carried out underpressure distillation, keep-up pressure, be warming up to 180 ℃, be incubated 20 minutes at-0.1MPa with Rotary Evaporators; Product is cooled to normal temperature, charges into nitrogen protection, obtain the crude product that lithium iodide white is mingled with light yellow solid.
In being full of the glove box of high pure nitrogen, thick product is dissolved in Virahol and alcoholic acid mixes among the dark liquid 500ml, its volume ratio 10: 1, the hydriodic acid aqueous solution 5g of dropping 45% stirs the elimination insolubles, in glove box, mother liquor is reduced pressure then and add thermal distillation with Rotary Evaporators, pressure condition is-0.1MPa, after temperature rises to 250 ℃, and constant temperature 0.5 hour; Product is cooled to normal temperature, charges into the high pure nitrogen protection, obtain the anhydrous lithium iodide white solid.Weighing output in glove box, calculated yield reaches 98.5%.
At dew point less than under-40 ℃, the environment of oxygen level less than 2ppm, preparation dioxolane, glycol dimethyl ether, propylene carbonate organic solvent, its volume ratio is 1: 1: 1, uses
Molecular sieve precipitation when moisture is reduced to 10ppm, seals and is refrigerated to-10 ℃, adds the lithium iodide of above-mentioned preparation then, and concentration is 1mo l/L, obtains lithium iodide organic electrolytic solution after shaking up.Obtain experimental data such as following table:
| Moisture | Placed 0 day | Placed 20 days |
| ?23ppm | Water white transparency | Water white transparency |
Embodiment 2
According to the lithium iodide of preparing among the embodiment 1, less than under-40 ℃, the environment of oxygen level less than 2ppm, preparation dioxolane, glycol dimethyl ether, diethylene glycol dimethyl ether volume ratio are 1: 1: 1 solvent, use at dew point
Molecular sieve precipitation, moisture is reduced to 10ppm, and sealing is refrigerated to-10 ℃, adds the lithium iodide of above-mentioned preparation then, and concentration is 1mol/L, obtains lithium iodide organic electrolytic solution after shaking up.Obtain experimental data such as following table:
| Moisture | Placed 0 day | Placed 20 days |
| 21ppm | Water white transparency | Water white transparency |
Embodiment 3
Get a hydronium(ion) oxidation lithium 168g (4mol) in there-necked flask, adding 168g deoxygenation distilled water is partly dissolved a hydronium(ion) oxidation lithium, stirring becomes suspension, slowly drips 45% hydriodic acid aqueous solution 1200g (4mol HI), make temperature be controlled at＜45 ℃ scope in; Dropwise the back and stirred 15 minutes, regulate between the above-mentioned solution pH value 3-4, make solution be water white transparency with a hydronium(ion) oxidation lithium and hydroiodic acid HI; Gained solution is carried out suction filtration, leach after the impurity, with Rotary Evaporators mother liquor is carried out underpressure distillation, the condition that keep-ups pressure is-0.1MPa, is warming up to 180 ℃, is incubated 30 minutes; Product is cooled to normal temperature, charges into nitrogen protection, obtain the crude product that lithium iodide white is mingled with faint yellow solid.
In being full of the glove box of high pure nitrogen, thick product is dissolved among Virahol and the alcoholic acid mixing solutions 2000ml, its volume ratio 10: 3, the hydriodic acid aqueous solution 10g of dropping 45% stirs the elimination insolubles, in glove box, mother liquor is carried out underpressure distillation then with Rotary Evaporators, pressure condition is-0.1MPa, after temperature rises to 250 ℃, and constant temperature 0.5 hour; Product is cooled to normal temperature, charges into the high pure nitrogen protection, obtain the anhydrous lithium iodide white solid.Weighing output in glove box, calculated yield reaches 98%.
At dew point less than under-40 ℃, the environment of oxygen level less than 2ppm, the organic solvent of preparation dioxolane, glycol dimethyl ether, propylene carbonate, its volume ratio is 1: 1: 1, uses
Molecular sieve precipitation, moisture is reduced to 10ppm, and sealing is refrigerated to-10 ℃, adds the lithium iodide of above-mentioned preparation then, and concentration is 0.8mol/L, obtains lithium iodide organic electrolytic solution after shaking up.Obtain experimental data such as following table:
| Moisture | Placed 0 day | Placed 20 days |
| 24ppm | Water white transparency | Water white transparency |
Comparative example 1
According to the lithium iodide of preparing among the embodiment 1, at dew point less than under-40 ℃, the environment of oxygen level less than 2ppm, preparation dioxolane, glycol dimethyl ether, diethylene glycol dimethyl ether mixed organic solvents (no antioxidant addn), its volume ratio is 1: 1: 1, uses
Molecular sieve precipitation, moisture is reduced to 10ppm, adds the lithium iodide of above-mentioned preparation then, and concentration is 1mol/L, obtains lithium iodide organic electrolytic solution after shaking up.Obtain experimental data such as following table:
| Moisture | Placed 0 day | Placed 20 days |
| 25ppm | Light yellow | Scarlet |
Comparative example 2
Anhydrous lithium iodide is available from last marine lithium Industrial Co., Ltd., at dew point less than under-40 ℃, the environment of oxygen level less than 2ppm, the mixed organic solvents of preparation dioxolane, glycol dimethyl ether, diethylene glycol dimethyl ether, its volume ratio is 1: 1: 1, uses
Molecular sieve precipitation, moisture is reduced to 10ppm, adds the lithium iodide of above-mentioned purchase then, and concentration is 1mol/L, obtains lithium iodide organic electrolytic solution after shaking up.Obtain experimental data such as following table:
| Moisture | Placed 0 day | Placed 20 days |
| 54ppm | Yellow | Scarlet |
Comparative example 3
Anhydrous lithium iodide is available from last marine lithium Industrial Co., Ltd., at dew point less than under-40 ℃, the environment of oxygen level less than 2ppm, the mixed organic solvents of preparation dioxolane, glycol dimethyl ether, diethylene glycol dimethyl ether, its volume ratio is 1: 1: 1, uses
Molecular sieve precipitation, moisture is reduced to 10ppm, and sealing is refrigerated to-10 ℃, adds the lithium iodide of above-mentioned purchase then, and concentration is 1mol/L, obtains lithium iodide organic electrolytic solution after shaking up.Obtain experimental data such as following table:
| Moisture | Placed 0 day | Placed 20 days |
| 56ppm | Water white transparency | Yellow |
In conjunction with the embodiments the present invention has been carried out exemplary description above; obvious realization of the present invention is not subjected to the restriction of aforesaid way; as long as the various improvement of having adopted method design of the present invention and technical scheme to carry out; or design of the present invention and technical scheme are directly applied to other occasion without improving, all in protection scope of the present invention.
Claims (6)
1. battery lithium iodide preparation method comprises being prepared as follows step:
The thick product preparation of step 1 lithium iodide
1.1 with lithium hydroxide or Quilonum Retard and hydriodic acid aqueous solution is reaction raw materials, raw material addition ratio 1: 1, and control drips feed rate remains between 30 ℃-70 ℃ temperature of reaction;
1.2 the pH value with a hydronium(ion) oxidation lithium or hydroiodic acid HI regulating step 1.1 gained solution is 1-6, makes solution be the water white transparency state;
1.3 step 1.2 gained solution is removed by filter impurity;
1.4 mother liquid obtained decompression of step 1.3 added thermal distillation, and keep-uping pressure is warming up to 80 ℃-150 ℃ under the condition of-0.1MPa, insulation 0.5h-50h;
1.5 step 1.4 products therefrom is cooled to normal temperature, charge into nitrogen protection, obtain lithium iodide white and be mingled with lurid crude product;
The preparation of step 2 anhydrous lithium iodide
2.1 in being full of the glove box of high pure nitrogen the thick product of lithium iodide is dissolved in the organic solvent, the hydriodic acid aqueous solution 1-200 of dropping 45% drips, and stirs;
2.2 step 2.1 gained solution is removed by filter impurity;
2.3 in glove box, carry out underpressure distillation with step 2.2 is mother liquid obtained, keep-up pressure after being warming up to 150 ℃-300 ℃ under the condition of-0.1MPa constant temperature 0.5h-50h;
2.4 step 2.3 products therefrom is cooled to normal temperature, charge into nitrogen protection, obtain the anhydrous lithium iodide white solid.
2. according to the described preparation method of claim 1, it is characterized in that: the organic solvent of described dissolving crude product is alcohols or ethers.
3. according to the described preparation method of claim 2, it is characterized in that: described alcohols is at least a in methyl alcohol, ethanol, propyl alcohol, Virahol or the butanols; Described ethers is at least a in ether, methyl ethyl ether, ethylene glycol monoemethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether, dioxolane or the dioxane.
4. battery method for preparation of lithium iodide organic electrolytic solution comprises being prepared as follows step:
Step 1 is used the electrolytic solution organic solvent
Molecular sieve precipitation makes organic solvent moisture content be lower than 10ppm;
Step 2 is refrigerated to 0 ℃-10 ℃ with the electrolytic solution organic solvent;
Step 3 will be dissolved in the electrolytic solution organic solvent according to the anhydrous lithium iodide that the described battery of claim 1-3 is prepared with the lithium iodide preparation method, obtains lithium iodide organic electrolytic solution.
5. according to the described battery method for preparation of lithium iodide organic electrolytic solution of claim 4, it is characterized in that: described organic electrolyte is made up of organic solvent and lithium iodide; Wherein, organic solvent is two or more the mixture in glycol dimethyl ether, diethylene glycol dimethyl ether, dioxolane, dioxane, propylene carbonate, methylcarbonate, Methyl ethyl carbonate or the diethyl carbonate.
6. according to claim 4 or 5 described battery method for preparation of lithium iodide organic electrolytic solution, it is characterized in that: described battery with lithium iodide organic electrolytic solution preparation be at dew point less than under-40 ℃, the environment of oxygen level less than 2ppm, the lithium iodide finished product be dissolved in prepare in the organic electrolyte solvent.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103137981A (en) * | 2013-03-06 | 2013-06-05 | 潘群生 | Preparation method for anhydrous lithium iodide |
| JP2013256416A (en) * | 2012-06-13 | 2013-12-26 | Godo Shigen Sangyo Kk | Method of manufacturing lithium iodide anhydride |
| CN103943882A (en) * | 2014-03-27 | 2014-07-23 | 北京化学试剂研究所 | Preparation method of lithium battery electrolyte |
| CN104261441A (en) * | 2014-09-30 | 2015-01-07 | 湖北佳德新材料有限公司 | Preparation method of anhydrous lithium iodide |
| JP2015214472A (en) * | 2014-04-23 | 2015-12-03 | 出光興産株式会社 | Method for producing a dried lithium halide |
| CN107221703A (en) * | 2017-06-01 | 2017-09-29 | 合肥尚强电气科技有限公司 | Manufacturing process of electrolyte for emergency power supply equipment |
| CN114409527A (en) * | 2021-12-30 | 2022-04-29 | 新余赣锋锂业有限公司 | Preparation method of non-broken small-particle anhydrous lithium acetate |
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| CN101565192A (en) * | 2009-04-30 | 2009-10-28 | 上海新漫传感技术研究发展有限公司 | Methods for preparing anhydrous lithium iodide and scintillation crystal doped with lithium iodide |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013256416A (en) * | 2012-06-13 | 2013-12-26 | Godo Shigen Sangyo Kk | Method of manufacturing lithium iodide anhydride |
| CN103137981A (en) * | 2013-03-06 | 2013-06-05 | 潘群生 | Preparation method for anhydrous lithium iodide |
| CN103943882A (en) * | 2014-03-27 | 2014-07-23 | 北京化学试剂研究所 | Preparation method of lithium battery electrolyte |
| JP2015214472A (en) * | 2014-04-23 | 2015-12-03 | 出光興産株式会社 | Method for producing a dried lithium halide |
| CN104261441A (en) * | 2014-09-30 | 2015-01-07 | 湖北佳德新材料有限公司 | Preparation method of anhydrous lithium iodide |
| CN104261441B (en) * | 2014-09-30 | 2016-02-24 | 湖北百杰瑞新材料股份有限公司 | A kind of preparation method of anhydrous lithium iodide |
| CN107221703A (en) * | 2017-06-01 | 2017-09-29 | 合肥尚强电气科技有限公司 | Manufacturing process of electrolyte for emergency power supply equipment |
| CN114409527A (en) * | 2021-12-30 | 2022-04-29 | 新余赣锋锂业有限公司 | Preparation method of non-broken small-particle anhydrous lithium acetate |
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Application publication date: 20111102 |