CN102030345A - Preparation method of cell-grade anhydrous lithium iodide - Google Patents
Preparation method of cell-grade anhydrous lithium iodide Download PDFInfo
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- CN102030345A CN102030345A CN 201110025920 CN201110025920A CN102030345A CN 102030345 A CN102030345 A CN 102030345A CN 201110025920 CN201110025920 CN 201110025920 CN 201110025920 A CN201110025920 A CN 201110025920A CN 102030345 A CN102030345 A CN 102030345A
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- lithium iodide
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Abstract
The invention discloses a preparation method of a cell-grade anhydrous lithium iodide. The preparation method is as follows: mixing and stirring lithium salt and hydroiodic acid; filtering, evaporating, crystallizing and separating, obtaining acicular crystal of lithium iodide trihydrate; then carrying out pre-drying and vacuum drying; and finally obtaining the cell-grade anhydrous lithium iodide. For the preparation method, the preparation process is simple, the material is cheap and is easy to obtain, the preparation cost is low, and in the whole synthetic process, no organic solvent is adopted, is non-toxic, and is green and environment-friendly. In the anhydrous lithium iodide prepared by the invention, the water content is lower than 0.02%, and the quality is equivalent to that of imported products.
Description
Technical field
The invention belongs to chemical field, relate to a kind of preparation method of lithium salts, specifically, relate to a kind of preparation method of battery-grade anhydrous lithium iodide.
Background technology
Lithium iodide is a kind of important chemical reagent, has the attention that yield height, stable reaction, selectivity advantages of higher are subjected to chemical boundary as catalyzer in Synthetic Organic Chemistry.And battery-grade anhydrous lithium iodide is a kind of high value added product as the ionogen of battery, has been widely used in now the power material of schrittmacher, and it has high-energy, low-loss, the life-span is long and good seal performance, can prevent advantage such as body fluid inflow.
The lithium iodide of white crystals is a kind of very active compound, sees light or is exposed to oxidized generation free-iodine in the air for a long time, and color reddens, and makes purity drop.In addition, lithium iodide is deliquescence very easily, absorbs the water in air branch purity is reduced greatly.
Prepare low-moisture lithium iodide and be always the difficult point in this product synthesis technique, this also is the major cause of this product scale operation of restriction.
At present, mainly contain about the preparation method of lithium iodide: liquefied ammonia medium method, medium-acetone method, ether medium method etc., but aforesaid method exist device complexity, expensive raw material price, condition be difficult to control, productive rate low, with defective such as separation of by-products difficulty.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defective of prior art, and a kind of preparation method of battery-grade anhydrous lithium iodide is provided.Adopt aqua-solution method, hydroiodic acid HI and basic lithium salts react, and obtain low moisture lithium iodide product through pervaporation, crystallization, drying again, and whole process does not adopt any organic solvent.
The battery-grade anhydrous lithium iodide product moisture content that the present invention obtains is lower than 0.02%.
For solving easily oxidized and deliquescence problem of anhydrous lithium iodide, the invention provides a kind of preparation method of battery-grade anhydrous lithium iodide, said method comprising the steps of:
Lithium salts and hydroiodic acid HI mixing stirring, filtration, evaporation, crystallization, separate three water lithium iodide needle crystals, predrying again and vacuum-drying finally obtains battery-grade anhydrous lithium iodide.
Concrete steps are:
Lithium salts is slowly added in the hydroiodic acid HI, and the mol ratio of hydroiodic acid HI and lithium add-on is 1:1; Stir filtering solution; Evaporation concentration filtrate to 150 ℃ on electric furnace is placed the naturally cooling crystallization; Filtering separation crystallization liquid gets three water lithium iodide needle crystals; Reclaim mother liquor.
Under 60 ℃ three water lithium iodide needle crystals were carried out predrying 3 hours in baking oven, attached water and the free-iodine of removing crystal surface obtain white crystals;
White crystals contained put into vacuum drying oven in the drying basin, elevated temperature to 200 ℃, vacuum tightness is not less than 5000Pa, and material was carried out vacuum-drying 24 hours, obtains the anhydrous lithium iodide product of white needles.
Described lithium salts is a Quilonum Retard or a hydronium(ion) oxidation lithium.Crystallization liquid is after separating, and mother liquor returns in the synthetic lithium iodide solution and reuses.
Described anhydrous lithium iodide moisture content is lower than 0.02%.
The present invention adopts traditional aqua-solution method, and hydroiodic acid HI and basic lithium salts react, and obtains low moisture lithium iodide product through pervaporation, crystallization, drying again, and whole process does not adopt any organic solvent.
Thereby the present invention has the following advantages compared to existing technology:
1, the present invention adopts evaporation, crystalline method, effectively removes the content of foreign ion in the solution, has improved the purity of lithium iodide product; Adopt water as the reaction medium environmentally safe simultaneously.
2, the present invention adopts the airtight vacuum drying, and the equal and atmospheric isolation of the drying of product and packing effectively prevents the product oxidation, and final moisture is lower than 0.02%.
3, preparation process of the present invention is simple, and raw material is cheap and easy to get, and preparation cost is low.
Embodiment
Embodiment 1
Take by weighing massfraction and be about 42% new system hydroiodic acid HI 455.2g, pour in the beaker, and use magnetic stirrer, slowly add Quilonum Retard 56g, stir and obtained lithium iodide solution in 1 hour.
Filter, filtrate evaporation concentration filtrate to 150 ℃ on electric furnace is placed the naturally cooling crystallization; Filtering separation crystallization liquid gets three water lithium iodide needle crystals; Reclaim mother liquor.
Under 60 ℃ three water lithium iodide needle crystals were carried out predrying 3 hours in baking oven, attached water and the free-iodine of removing crystal surface obtain white crystals.
White crystals contained put into vacuum drying oven in the drying basin, elevated temperature to 200 ℃, vacuum tightness is not less than 5000Pa, and material was carried out vacuum-drying 24 hours, obtains the anhydrous lithium iodide product of white needles.In glove box, pack.
Mother liquor returns in the synthetic lithium iodide solution and reuses.
Embodiment 2
Take by weighing massfraction and be about 42% new system hydroiodic acid HI 455.2g, pour in the beaker, and use magnetic stirrer, slowly add a hydronium(ion) oxidation lithium 62.6g, stir and obtained lithium iodide solution in 1 hour.
Filter, filtrate evaporation concentration filtrate to 150 ℃ on electric furnace is placed the naturally cooling crystallization; Filtering separation crystallization liquid gets three water lithium iodide needle crystals; Reclaim mother liquor.
In baking oven three water lithium iodide needle crystals were carried out predrying 3 hours under 60 ℃, attached water and the free-iodine of removing crystal surface obtain white crystals.
White crystals contained put into vacuum drying oven in the drying basin, elevated temperature to 200 ℃, vacuum tightness is not less than 5000Pa, and material was carried out vacuum-drying 24 hours, obtains the anhydrous lithium iodide product of white needles.In glove box, pack.
Mother liquor returns in the synthetic lithium iodide solution and reuses.
Embodiment 3
Take by weighing massfraction and be about new system hydroiodic acid HI 455.2g about 42%, pour in the beaker, and use magnetic stirrer, slowly add Quilonum Retard 54g, add the about 1.3g of a hydronium(ion) oxidation lithium again, continue to stir and obtained lithium iodide solution in 1 hour.
Filtering solution gets filtrate; Evaporation concentration filtrate to 150 ℃ on electric furnace is placed the naturally cooling crystallization; Filtering separation crystallization liquid gets three water lithium iodide needle crystals; Reclaim mother liquor.
Under 60 ℃ three water lithium iodide needle crystals were carried out predrying 3 hours in baking oven, attached water and the free-iodine of removing crystal surface obtain white crystals.
White crystals contained put into vacuum drying oven in the drying basin, elevated temperature to 200 ℃, vacuum tightness is not less than 5000Pa, and material was carried out vacuum-drying 24 hours, obtains the anhydrous lithium iodide product of white needles.In glove box, pack.
Mother liquor returns in the synthetic lithium iodide solution and reuses.
The anhydrous lithium iodide moisture content of embodiment 1-embodiment 3 preparations is lower than 0.02%, and is suitable with the imported product quality.Its cost is well below imported product.
It should be noted that at last: obviously, the foregoing description only is for example of the present invention clearly is described, and is not the qualification to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (5)
1. the preparation method of a battery-grade anhydrous lithium iodide is characterized in that, said method comprising the steps of:
Lithium salts and hydroiodic acid HI mix stir, filter evaporation, crystallization, separate three water lithium iodide needle crystals, predrying again and vacuum-drying finally obtains battery-grade anhydrous lithium iodide.
2. the preparation method of battery-grade anhydrous lithium iodide as claimed in claim 1 is characterized in that, concrete steps are:
Lithium salts is slowly added in the hydroiodic acid HI, and the mol ratio of hydroiodic acid HI and lithium add-on is 1:1; Stir filtering solution; Evaporation concentration filtrate to 150 ℃ on electric furnace is placed the naturally cooling crystallization; Filtering separation crystallization liquid gets three water lithium iodide needle crystals; Reclaim mother liquor;
Under 60 ℃ three water lithium iodide needle crystals were carried out predrying 3 hours in baking oven, attached water and the free-iodine of removing crystal surface obtain white crystals;
White crystals contained put into vacuum drying oven in the drying basin, elevated temperature to 200 ℃, vacuum tightness is not less than 5000Pa, and material was carried out vacuum-drying 24 hours, obtains the anhydrous lithium iodide product of white needles.
3. the preparation method of battery-grade anhydrous lithium iodide as claimed in claim 1, it is characterized in that: described lithium salts is a Quilonum Retard or a hydronium(ion) oxidation lithium.
4. the preparation method of battery-grade anhydrous lithium iodide as claimed in claim 2 is characterized in that: crystallization liquid is after separating, and mother liquor returns in the synthetic lithium iodide solution and reuses.
5. the preparation method of battery-grade anhydrous lithium iodide as claimed in claim 2, it is characterized in that: described anhydrous lithium iodide moisture content is lower than 0.02%.
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| CN 201110025920 CN102030345A (en) | 2011-01-25 | 2011-01-25 | Preparation method of cell-grade anhydrous lithium iodide |
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| CN 201110025920 CN102030345A (en) | 2011-01-25 | 2011-01-25 | Preparation method of cell-grade anhydrous lithium iodide |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013103851A (en) * | 2011-11-11 | 2013-05-30 | Nippon Chem Ind Co Ltd | Lithium iodide anhydrate, method for producing lithium iodide anhydrate, solid electrolyte and lithium ion battery |
| CN103523805A (en) * | 2013-10-22 | 2014-01-22 | 瓮福（集团）有限责任公司 | Method for preparing high-purity lithium iodide trihydrate and co-producing lithium sulfate |
| JP2014065637A (en) * | 2012-09-26 | 2014-04-17 | Nippo Kagaku Kk | Method of producing lithium iodide aqueous solution and use thereof |
| JP2014065638A (en) * | 2012-09-26 | 2014-04-17 | Nippo Kagaku Kk | Method of producing lithium iodide aqueous solution and use thereof |
| CN104261440A (en) * | 2014-09-18 | 2015-01-07 | 新疆有色金属研究所 | Battery-grade anhydrous lithium iodide and preparation method thereof |
| CN105098203A (en) * | 2015-08-10 | 2015-11-25 | 惠州亿纬锂能股份有限公司 | Preparation method for electrolyte used for lithium-ferrous disulfide battery |
| CN109553118A (en) * | 2018-12-19 | 2019-04-02 | 江西赣锋锂业股份有限公司 | A kind of method of industrial production anhydrous lithium hydroxide ball |
| JP2019089673A (en) * | 2017-11-14 | 2019-06-13 | 伊勢化学工業株式会社 | Method for producing inorganic iodine anhydrous compound and lump thereof |
| CN110182829A (en) * | 2019-06-11 | 2019-08-30 | 新疆有色金属研究所 | A kind of industrialized process for preparing of cell-grade anhydrous lithium iodide |
| CN110230917A (en) * | 2019-06-17 | 2019-09-13 | 新疆骏强科技发展有限公司 | Device for drying anhydrous lithium iodide and preparation method of anhydrous lithium iodide |
| CN113735140A (en) * | 2021-07-02 | 2021-12-03 | 湖北百杰瑞新材料股份有限公司 | Preparation method of anhydrous lithium iodide |
-
2011
- 2011-01-25 CN CN 201110025920 patent/CN102030345A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《原子能科学技术》 19601231 张振等 碘化锂（铊）单晶的制备 1-5 , 第3期 2 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013103851A (en) * | 2011-11-11 | 2013-05-30 | Nippon Chem Ind Co Ltd | Lithium iodide anhydrate, method for producing lithium iodide anhydrate, solid electrolyte and lithium ion battery |
| JP2014065637A (en) * | 2012-09-26 | 2014-04-17 | Nippo Kagaku Kk | Method of producing lithium iodide aqueous solution and use thereof |
| JP2014065638A (en) * | 2012-09-26 | 2014-04-17 | Nippo Kagaku Kk | Method of producing lithium iodide aqueous solution and use thereof |
| CN103523805A (en) * | 2013-10-22 | 2014-01-22 | 瓮福（集团）有限责任公司 | Method for preparing high-purity lithium iodide trihydrate and co-producing lithium sulfate |
| CN104261440B (en) * | 2014-09-18 | 2016-02-17 | 新疆有色金属研究所 | Cell-grade anhydrous lithium iodide and preparation method thereof |
| CN104261440A (en) * | 2014-09-18 | 2015-01-07 | 新疆有色金属研究所 | Battery-grade anhydrous lithium iodide and preparation method thereof |
| CN105098203A (en) * | 2015-08-10 | 2015-11-25 | 惠州亿纬锂能股份有限公司 | Preparation method for electrolyte used for lithium-ferrous disulfide battery |
| JP2019089673A (en) * | 2017-11-14 | 2019-06-13 | 伊勢化学工業株式会社 | Method for producing inorganic iodine anhydrous compound and lump thereof |
| JP7098306B2 (en) | 2017-11-14 | 2022-07-11 | 伊勢化学工業株式会社 | Method for producing inorganic iodine compound anhydride, and lumps |
| CN109553118A (en) * | 2018-12-19 | 2019-04-02 | 江西赣锋锂业股份有限公司 | A kind of method of industrial production anhydrous lithium hydroxide ball |
| CN110182829A (en) * | 2019-06-11 | 2019-08-30 | 新疆有色金属研究所 | A kind of industrialized process for preparing of cell-grade anhydrous lithium iodide |
| CN110230917A (en) * | 2019-06-17 | 2019-09-13 | 新疆骏强科技发展有限公司 | Device for drying anhydrous lithium iodide and preparation method of anhydrous lithium iodide |
| CN113735140A (en) * | 2021-07-02 | 2021-12-03 | 湖北百杰瑞新材料股份有限公司 | Preparation method of anhydrous lithium iodide |
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Application publication date: 20110427 |