CN103058231B - Method for preparing anhydrous lithium bromide - Google Patents
Method for preparing anhydrous lithium bromide Download PDFInfo
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- CN103058231B CN103058231B CN201210417698.8A CN201210417698A CN103058231B CN 103058231 B CN103058231 B CN 103058231B CN 201210417698 A CN201210417698 A CN 201210417698A CN 103058231 B CN103058231 B CN 103058231B
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Abstract
The invention discloses a method for preparing anhydrous lithium bromide by drying in an atmospheric environment, shortening drying time and reducing energy consumption and production cost, and the method comprises the following steps of: (1) active carbon decolouration: adding 3 thousandths of active carbon to a lithium bromide solution, stirring for 0.5-1.5 hours for decolouration, and then carrying out pressure filtration to obtain a fine lithium bromide solution; (2) evaporation and concentration: evaporating and concentrating the fine lithium bromide solution till the concentration of lithium bromide is between 30 percent and 50 percent; (3) spray drying: firstly regulating the inlet air temperature of a spray drying instrument to 250-350 DEG C, the outlet air temperature to 170-200 DEG C, previously spraying for 10-20 minutes by using pure water, carrying out the spray drying on the lithium bromide solution through the spray drying instrument, controlling the airflow rate of the spray drying instrument at 3000 cubic meters/hour and the flow rate of a peristaltic pump at 150 liters/hour; and (4) cooling packaging: blowing dehumidified and cooled dry cold air into the discharge port of the spray drying instrument, and controlling the relative humidity of the dry cold air to be less than 5 percent and the temperature to be less than 20 DEG C.
Description
Technical field
The present invention relates to the technical field of chemical industry, relate in particular to a kind of method of preparing anhydrous lithium bromide.
Background technology
Anhydrous lithium bromide molecular formula is LiBr, and the production method of existing anhydrous lithium bromide mainly contains three kinds: neutralisation, bromination iron processes and urea reduction method, briefly introduce as follows.1, neutralisation: adopt Hydrogen bromide and Lithium hydroxide to carry out neutralization reaction and obtain lithium-bromide solution, then through evaporation concentration, the dry anhydrous lithium bromide that obtains; 2, bromination iron processes: this method makes lithium-bromide solution taking iron filings, bromine and Quilonum Retard as raw material, then through evaporation concentration, the dry anhydrous lithium bromide that obtains; 3, urea reduction method: it is that raw material makes lithium-bromide solution that this method adopts urea, Quilonum Retard and bromine, then through evaporation concentration, the dry anhydrous lithium bromide product that obtains.
Obtain water content low, the anhydrous lithium bromide product that whiteness is good, drying mode is crucial, the drying means of preparing at present anhydrous lithium bromide has three major types: 1, organic solvent method, as building medium organic solvent (1,2-, bis-D) and the lithium-bromide solution azeotropic dehydration under 130 DEG C/10.67kPa used, king obtains 98.5% anhydrous lithium bromide solid; 2, nitrogen protection method, as the employings such as J.LIVINGSTON obtain anhydrous lithium bromide solid 160 DEG C of above dry several talentes under nitrogen protection; 3, boulton process, as the employings such as I.S.YAFFE 350 DEG C of dry anhydrous lithium bromide solids that just obtain for 96 hours under vacuum condition.
Above method has all adopted under protective medium or vacuum environment and has been dried and prepares anhydrous lithium bromide, drying conditions harshness, and time of drying is longer, is difficult for realizing industrialization.Tradition anhydrous lithium bromide drying process adopts the major cause of harsh drying conditions to be, anhydrous lithium bromide solid has strong absorptive, as at air drying, still can absorb a small amount of airborne moisture content and become tawny in drying process.Avoid anhydrous lithium bromide to reuptake moisture content and variable color, traditional technology adopt isolated air (as under rare gas element or organic solvent protection or dry under vacuum state) method.
Summary of the invention
For overcoming the defect of prior art, the technical problem to be solved in the present invention has been to provide a kind of method of preparing anhydrous lithium bromide that can be dried in atmospheric environment, shorten time of drying, reduce energy consumption and production costs.
Technical scheme of the present invention is: this method of preparing anhydrous lithium bromide, comprises the following steps:
(1) activated carbon decolorizing: toward the gac that adds solution quality 3 ‰ in lithium-bromide solution, stir and decolour for 0.5～1.5 hour, then press filtration obtains smart lithium-bromide solution;
(2) evaporation concentration: the smart lithium-bromide solution evaporation concentration that step (1) is obtained to lithium bromide concentration is between 30%-50%;
(3) spraying is dry: the lithium-bromide solution after utilizing spraying drying instrument to step (2) evaporation concentration is sprayed to be dried and obtained anhydrous lithium bromide, first the entrance wind-warm syndrome of adjustable spraying drying instrument is 250-350 DEG C, outlet wind-warm syndrome 170-200 DEG C, with the pre-spray of pure water 10～20 minutes, lithium-bromide solution is sprayed dry by spraying drying instrument again, the air flow quantity of controlling spraying drying instrument is 3000 cubes ms/h, and peristaltic pump flow is 150 ls/h;
(4) cooling packing: the discharge port at spraying drying instrument blasts the dry freezing air through dehumidifying and cooling, make the quick cooling packing of anhydrous lithium bromide powder of ejection, prevent that anhydrous lithium bromide from absorbing moisture content and causing product water content to raise, control the relative humidity < 5% of dry air, 20 DEG C of temperature <.
The inventor finds through great many of experiments; in atmospheric environment; be at high temperature lithiumbromide powder by lithium-bromide solution evaporation drying fast; then quick cooling packing; just can obtain that whiteness is good, the anhydrous lithium bromide product of water content low (<0.25%); overcome traditional technology must be under rare gas element or organic solvent protection or under vacuum state the shortcoming of dry lithiumbromide, shortened time of drying, reduced energy consumption and production cost.
Embodiment
This method of preparing anhydrous lithium bromide, comprises the following steps:
(1) activated carbon decolorizing: toward the gac that adds solution quality 3 ‰ in lithium-bromide solution, stir and decolour for 0.5～1.5 hour, then press filtration obtains smart lithium-bromide solution;
(2) evaporation concentration: the smart lithium-bromide solution evaporation concentration that step (1) is obtained to lithium bromide concentration is between 30%-50%;
(3) spraying is dry: the lithium-bromide solution after utilizing spraying drying instrument to step (2) evaporation concentration is sprayed to be dried and obtained anhydrous lithium bromide, first the entrance wind-warm syndrome of adjustable spraying drying instrument is 250-350 DEG C, outlet wind-warm syndrome 170-200 DEG C, with the pre-spray of pure water 10～20 minutes, by spraying drying instrument, lithium-bromide solution is sprayed dry, the air flow quantity of controlling spraying drying instrument is 3000m again
3/ h (cube m/h), peristaltic pump flow be 150L/h (l/h);
(4) cooling packing: the discharge port at spraying drying instrument blasts the dry freezing air through dehumidifying and cooling, make the quick cooling packing of anhydrous lithium bromide powder of ejection, prevent that anhydrous lithium bromide from absorbing moisture content and causing product water content to raise, control the relative humidity < 5% of dry air, 20 DEG C of temperature <.
The inventor finds through great many of experiments; in atmospheric environment; be at high temperature lithiumbromide powder by lithium-bromide solution evaporation drying fast; then quick cooling packing; just can obtain that whiteness is good, the anhydrous lithium bromide product of water content low (<0.25%); overcome traditional technology must be under rare gas element or organic solvent protection or under vacuum state the shortcoming of dry lithiumbromide, shortened time of drying, reduced energy consumption and production cost.
Preferably, described lithium-bromide solution is the thick lithium-bromide solution that adopts neutralisation to prepare.
Preferably, described lithium-bromide solution is the thick lithium-bromide solution that adopts urea reduction method to prepare.
Preferably, described lithium-bromide solution is to adopt the standby thick lithium-bromide solution of iron bromide legal system.
Below provide several specific embodiments.
Embodiment 1:
Toward the gac that adds 3 ‰ in lithium-bromide solution, stir 0.5h and decolour, then press filtration obtains smart lithium-bromide solution; Be 30% by smart lithium-bromide solution evaporation concentration to lithium bromide concentration again, utilize the lithium-bromide solution of spraying drying instrument after to evaporation concentration spray to be dried and obtain anhydrous lithium bromide product.First the entrance wind-warm syndrome of adjustable spraying drying instrument is 250 DEG C, 170 DEG C of outlet wind-warm syndrome.With the pre-spray of pure water 10 minutes, and then it is dry that 1500L lithium-bromide solution is sprayed, and the air flow quantity of controlling spraying drying instrument is 3000m
3/ h, peristaltic pump flow is 100L/h, obtains 576kg anhydrous lithium bromide.
Embodiment 2:
Toward the gac that adds 3 ‰ in lithium-bromide solution, stir 1h and decolour, then press filtration obtains smart lithium-bromide solution; Be 40% by smart lithium-bromide solution evaporation concentration to lithium bromide concentration again, utilize the lithium-bromide solution of spraying drying instrument after to evaporation concentration spray to be dried and obtain anhydrous lithium bromide product.First the entrance wind-warm syndrome of adjustable spraying drying instrument is 300 DEG C, 190 DEG C of outlet wind-warm syndrome.With the pre-spray of pure water 15 minutes, and then it is dry that 1500L lithium-bromide solution is sprayed, and the air flow quantity of controlling spraying drying instrument is 3000m
3/ h, peristaltic pump flow is 100L/h, obtains 768kg anhydrous lithium bromide.
Embodiment 3:
Toward the gac that adds 3 ‰ in lithium-bromide solution, stir 1.5h and decolour, then press filtration obtains smart lithium-bromide solution; Be 50% by smart lithium-bromide solution evaporation concentration to lithium bromide concentration again, utilize the lithium-bromide solution of spraying drying instrument after to evaporation concentration spray to be dried and obtain anhydrous lithium bromide product.First the entrance wind-warm syndrome of adjustable spraying drying instrument is 350 DEG C, 200 DEG C of outlet wind-warm syndrome.With the pre-spray of pure water 20 minutes, and then it is dry that 1500L lithium-bromide solution is sprayed, and the air flow quantity of controlling spraying drying instrument is 3000m
3/ h, peristaltic pump flow is 100L/h, obtains 960kg anhydrous lithium bromide.
Table 1 is the experimental result of above three kinds of embodiment.
Table 1
| Sequence number | Main content (%) | H 2O is less than (%) | Whiteness |
| 1 | 99.56 | 0.22 | 90 |
| 2 | 99.62 | 0.26 | 95 |
| 3 | 99.59 | 0.23 | 88 |
The above; it is only preferred embodiment of the present invention; not the present invention is done to any pro forma restriction, any simple modification, equivalent variations and modification that every foundation technical spirit of the present invention is done above embodiment, all still belong to the protection domain of technical solution of the present invention.
Claims (4)
1. a method of preparing anhydrous lithium bromide, is characterized in that: comprise the following steps:
(1) activated carbon decolorizing: toward the gac that adds solution quality 3 ‰ in lithium-bromide solution, stir and decolour for 0.5～1.5 hour, then press filtration obtains smart lithium-bromide solution;
(2) evaporation concentration: the smart lithium-bromide solution evaporation concentration that step (1) is obtained to lithium bromide concentration is between 30%-50%;
(3) spraying is dry: the lithium-bromide solution after utilizing spraying drying instrument to step (2) evaporation concentration is sprayed to be dried and obtained anhydrous lithium bromide, first the entrance wind-warm syndrome of adjustable spraying drying instrument is 250-350 DEG C, outlet wind-warm syndrome 170-200 DEG C, with the pre-spray of pure water 10～20 minutes, lithium-bromide solution is sprayed dry by spraying drying instrument again, the air flow quantity of controlling spraying drying instrument is 3000 cubes ms/h, and peristaltic pump flow is 150 ls/h;
(4) cooling packing: the discharge port at spraying drying instrument blasts the dry freezing air through dehumidifying and cooling, make the quick cooling packing of anhydrous lithium bromide powder of ejection, prevent that anhydrous lithium bromide from absorbing moisture content and causing product water content to raise, control the relative humidity < 5% of dry air, 20 DEG C of temperature <.
2. the method for preparing anhydrous lithium bromide according to claim 1, is characterized in that: described lithium-bromide solution is the thick lithium-bromide solution that adopts neutralisation to prepare.
3. the method for preparing anhydrous lithium bromide according to claim 1, is characterized in that: described lithium-bromide solution is the thick lithium-bromide solution that adopts urea reduction method to prepare.
4. the method for preparing anhydrous lithium bromide claimed in claim 1, is characterized in that: described lithium-bromide solution is to adopt the standby thick lithium-bromide solution of iron bromide legal system.
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| CN201210417698.8A CN103058231B (en) | 2012-10-26 | 2012-10-26 | Method for preparing anhydrous lithium bromide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103508471A (en) * | 2013-09-28 | 2014-01-15 | 昆山市周市溴化锂溶液厂 | Method for refining anhydrous lithium bromide |
| DE102014226608A1 (en) * | 2014-01-03 | 2015-07-09 | Rockwood Lithium GmbH | Process for the preparation of zinc bromide and lithium bromide-containing aprotic solutions |
| EP3245658A1 (en) * | 2015-01-13 | 2017-11-22 | ABB Schweiz AG | Apparatus containing a dielectric insulation gas comprising an organofluorine compound |
| CN109205647A (en) * | 2018-09-21 | 2019-01-15 | 佛山市吉力达铝材科技有限公司 | A method of sodium metaaluminate is prepared using mould waste liquid is stewed |
| CN110182829B (en) * | 2019-06-11 | 2021-08-13 | 新疆有色金属研究所 | Industrial preparation method of battery-grade anhydrous lithium iodide |
| CN114212836A (en) * | 2021-12-31 | 2022-03-22 | 金川集团镍盐有限公司 | Preparation method of anhydrous nickel chloride powder material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1204621A (en) * | 1997-07-08 | 1999-01-13 | 国营建中化工总公司 | Technology and device for producing granular lithium chloride |
| WO2008069639A1 (en) * | 2006-12-07 | 2008-06-12 | Friesland Brands B.V. | Method and apparatus for spray drying and powder produced using said method |
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- 2012-10-26 CN CN201210417698.8A patent/CN103058231B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1204621A (en) * | 1997-07-08 | 1999-01-13 | 国营建中化工总公司 | Technology and device for producing granular lithium chloride |
| WO2008069639A1 (en) * | 2006-12-07 | 2008-06-12 | Friesland Brands B.V. | Method and apparatus for spray drying and powder produced using said method |
Non-Patent Citations (4)
| Title |
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| 杨金席.生产溴化锂新工艺的研究.《海盐与化工》.1996,全文. |
| 溴化锂的生产工艺综述;魏述彬等;《盐湖研究》;20060930;全文 * |
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| 魏述彬等.溴化锂的生产工艺综述.《盐湖研究》.2006,全文. |
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Effective date of registration: 20140813 Address after: 338004 No. 608, South hi tech Industrial Park, Jiangxi, Xinyu Applicant after: JIANGXI GANFENG LITHIUM Co.,Ltd. Address before: 338000, Jiangxi City, Jiangxi Province, Xinyu town Xinyu Gan Feng organic lithium Co., Ltd. Applicant before: XINYU GANFENG LITHIUM Co.,Ltd. |
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Address after: 338004 No. 608, Nanyuan Road, Xinyu national high tech Industrial Park, Jiangxi Province Patentee after: Jiangxi Ganfeng Lithium Industry Group Co.,Ltd. Address before: 338004 No. 608, Nanyuan Road, Xinyu national high tech Industrial Park, Jiangxi Province Patentee before: JIANGXI GANFENG LITHIUM Co.,Ltd. |