CN1204621A - Production process technology and device of granular lithium chloride - Google Patents
Production process technology and device of granular lithium chloride Download PDFInfo
- Publication number
- CN1204621A CN1204621A CN 97107592 CN97107592A CN1204621A CN 1204621 A CN1204621 A CN 1204621A CN 97107592 CN97107592 CN 97107592 CN 97107592 A CN97107592 A CN 97107592A CN 1204621 A CN1204621 A CN 1204621A
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- Prior art keywords
- drying
- licl
- lithium chloride
- prilling tower
- pressure
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 title claims abstract description 148
- 238000005516 engineering process Methods 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000005243 fluidization Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001694 spray drying Methods 0.000 claims abstract 2
- 230000008676 import Effects 0.000 claims 1
- 238000004886 process control Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 15
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052744 lithium Inorganic materials 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000003595 mist Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000005469 granulation Methods 0.000 abstract description 2
- 230000003179 granulation Effects 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 abstract 3
- 239000012452 mother liquor Substances 0.000 abstract 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000013067 intermediate product Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 238000003860 storage Methods 0.000 description 19
- 239000006260 foam Substances 0.000 description 15
- 239000007921 spray Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 238000007664 blowing Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 2
- 239000003245 coal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- Glanulating (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a drying process technology and a drying device for lithium chloride, and relates to the preparation of chemical raw materials. In the production of lithium chloride, an intermediate product lithium chloride mother liquor is required to be prepared into particles, the process adopts a fluidization spray drying technology, the mother liquor with the concentration of 150-320 g/l is atomized through a nozzle under the action of compressed air, the atomized mother liquor is quantitatively sprayed into a granulation tower, seed crystals in the tower attach fine mist into granules, and the granules with the particle size of phi 1-8 mm are prepared by drying the granules under the action of hot air, wherein the water content is less than 0.5%. The process can be used for large-scale industrial production, the direct yield reaches 92%, and the process can be directly used for producing metal lithium by an electrolytic method and used as other chemical raw materials.
Description
The invention belongs to the preparation field of industrial chemicals, be specifically related to the preparation of granular lithium chloride.
Fused salt electrolysis process is adopted in the production of metallic lithium usually, is preparing with this method in the process of metallic lithium, and granular lithium chloride is used as raw material and a large amount of the use; In addition, it also is widely used in making in the welding auxiliary material, in industry such as organic synthesis, electronics, medicine application is arranged also.But need the work in-process lithium chloride solution of Chemical Manufacture is carried out drying and dehydrating, make particle or powder lithium chloride; This process adopts electric furnace heat nickel pot parch usually, and shortcoming is that turnout is little, intermittent operation, and labor strength is big, and energy consumption is big, the cost height, and product contains the block that differs in size, and make water content inhomogeneous, be unfavorable for preparing metallic lithium and other application.
The objective of the invention is provides plant-scale Technology and device for the drying of lithium chloride, overcomes shortcomings such as nickel pot parch turnout is little, satisfies the needs of industrial-scale production metallic lithium.
The present invention is achieved by following technical measures, in prilling tower 1, add lithium chloride crystal seed (LiCl powder) 17, under the effect of vacuum fan 10, make LiCl crystal seed 17 fluidisations in the prilling tower 1 through foam eluting column 5, cyclonic separator 2 and suspension settlement chamber 15, when hot blast temperature reaches 350 ℃, with concentration in the header tank 3 is that LiCl solution about 300g/l makes its atomizing under the compressed-air actuated effect by nozzle 12 through strainer 8 and under meter 9 in pressing empty injector, and quantitatively sprays in the prilling tower 1; The LiCl solution mist that sprays is attached on the LiCl crystal seed 17, and warm air is rapidly with moisture evaporation, and (granular lithium chloride of φ 1～8mm), product is discharged into product storage tank 14 through sieve plate 13 from prilling tower 1 bottom to obtain certain particle size through concentrated, crystallization, drying.Tail gas is taken away from top of tower through the suspension settlement chamber that enlarges 15, and the bottom that enters foam eluting column 5 through cyclonic separator 2 enters atmosphere by vacuum fan 10 again after drip washing purifies.The particulate that reclaims from cyclonic separator 2 returns prilling tower 1 through powder diverting valve 11 under compressed-air actuated effect, or collects powder storage tank 16 separately as product (when needing powder-product).Through foam eluting columns 5 and tail gas counter current contact from cyclonic separator 2, the fine powder lithium chloride in the tail gas is dissolved in the solution lithium chloride dilute solution, makes lithium chloride dilute solution enrichment from header tank 4.The lithium chloride dilute solution flows into storage tank 7, squeezes into high-order storage tank 4 with pump 6; Through repeatedly circulation, when the lithium chloride concentration in the storage tank 7 reaches about 300g/l, squeeze into header tank 3 with pump 6, confession production particle LiCl usefulness, header tank 3 and header tank 4 all have upflow tube to receive storage tank 7.
Processing parameter:
LiCl crystal seed height: 280～400mm (the quiet height of bed);
LiCl seed size: φ 0.5～6mm;
Hot blast inlet temperature: 300～450 ℃;
Hot-blast pressure: 2.0～4.0kPa (adjustable);
Trunnion pressure :-50～-150Pa;
LiCl strength of solution: 150～320g/l;
Material spray pressure: 0.1～0.4MPa;
Fluidized layer temperature: 170～250 ℃;
Blowing pressure reduction: 2.0～3.8kPa;
The foam column top hole pressure :-1.0～-2.5kPa;
Foam column temperature out: 70～100 ℃.
The present invention is applicable to the granular lithium chloride of industrial-scale production φ 1～8, by the parameters such as concentration, straying quatity, hot-blast pressure, temperature of control lithium chloride solution, can obtain the lithium chloride of variable grain size, and grain graininess is adjustable.The suitable warm air that adopts fluidizing furnace to burn the coal generation of this technology comes the fluidized drying lithium chloride, and production cost is than low with electric furnace nickel pot parch.
Open fluidizing furnace, make hot blast reach use temperature, mix up the blast and the wind speed of hot blast, send into prilling tower 1 continuously and stably; It is standby that the lithium chloride solution for preparing in the LiCl solution storage tank 7 is sent into header tank 3 with pump 6.Start vacuum fan 10, adjust compressed air pressure, mix up the flow that sprays into of lithium chloride solution with under meter 9, when each monitoring instrument indicate reach controlled variable after, carry out the material spray fluidization granulation.The product particle lithium chloride draws off from the prilling tower bottom.Tail gas enters atmosphere through the powder of cyclonic separator 2 except that deentrainment behind foam eluting column 5 washing, purifyings, the lithium chloride dilute solution flows into storage tank 7 behind header tank 4 process foam eluting columns 5 enrichments.When the lithium chloride solution concentration in the storage tank 7 reaches about 300g/l, squeeze into header tank 3 with pump 6.
Fig. 1 is a granular lithium chloride production process equipment schema;
Fig. 2 is the nozzle synoptic diagram.
Embodiment 1:
In storage tank 7, add LiOHH
2O uses water dissolution, adds hydrochloric acid, is mixed with the LiCl solution of concentration 246g/l, and it is standby to squeeze into header tank 3 with pump 6.
In prilling tower 1, add the LiCl crystal seed, make the crystal seed height reach 300mm; Open fluidizing furnace, make hot blast reach 385 ℃, mix up the blast and the wind speed of hot blast; Start vacuum fan 10, hot blast is sent in the prilling tower 1, make LiCl crystal seed 17 fluidisations in the prilling tower 1.With the concentration in the header tank 3 be the LiCl solution of 246g/l through strainer 8 and under meter 9, in pressing empty injector 18, make its atomizing under the compressed-air actuated effect by nozzle 12, and quantitatively spray in the prilling tower 1.The LiCl solution mist that sprays is attached on the crystal seed, and warm air through concentrated, crystallization, drying, obtains the particle LiCl that particle diameter is about φ 3mm rapidly with moisture evaporation.Product is discharged into product storage tank 14 through sieve plate 13 from the prilling tower bottom.Tail gas is taken away from top of tower through suspension settlement chamber 15, enters foam eluting column 5 through cyclonic separator 2, and drip washing enters atmosphere by vacuum fan 10 after purifying.The particulate that reclaims from cyclonic separator 2 returns prilling tower 1 through powder diverting valve 11 under compressed-air actuated effect.
Preparation LiCl dilute solution is squeezed into header tank 4 with it in storage tank 7, and through foam eluting column 5 and tail gas counter current contact from cyclonic separator 2, the fine powder LiCl in the tail gas is dissolved in the solution, makes LiCl dilute solution enrichment.The LiCl dilute solution flows in the storage tank 7, squeezes into header tank 4 with pump 6.Through repeatedly circulation, when the LiCl concentration in the storage tank 7 reaches about 250g/l, squeeze into header tank 3, for production particle LiCl usefulness with pump 6.
Processing parameter:
LiCl crystal seed height: 300mm;
LiCl seed size: φ 2～5mm, 50%; ﹠amp; #60 φ 2mm, 50%;
Hot blast temperature: 385 ℃;
Hot-blast pressure: 3.75kPa; Revert pipe blast: 0.28MPa; Trunnion pressure :-100Pa; LiCl strength of solution: 246g/l material spray flow: 430l/h; Material spray pressure: 0.28MPa; Fluidized layer temperature: 180～210 ℃; Blowing pressure reduction: 3.5kPa; Foam column top hole pressure :-1.9kPa foam column temperature out: 85～90 ℃; The particle LiCl epigranular of output is about φ 3mm, and hourly output is about 100kg.Embodiment 2: add LiOHH in storage tank 7
2O uses water dissolution, adds hydrochloric acid, is mixed with the LiCl solution of concentration 176g/l, and it is standby to squeeze into header tank 3 with pump 6.
In prilling tower 1, add the LiCl powder and make crystal seed, make the crystal seed height reach 320mm; Open fluidizing furnace, make hot blast reach 392 ℃, mix up the blast and the wind speed of hot blast; Start vacuum fan 10, hot blast is sent in the prilling tower 1, make LiCl crystal seed 17 fluidisations in the prilling tower 1.With the concentration in the header tank 3 be the LiCl solution of 176g/l through strainer 8 and under meter 9, in pressing empty injector, make its atomizing under the compressed-air actuated effect by nozzle 12, spray in the prilling tower 1 by the flow of 420l/h.The LiCl solution mist that sprays is attached on the crystal seed, and warm air through concentrated, crystallization, drying, obtains the particle LiCl that particle diameter is about φ 1mm rapidly with moisture evaporation.Product is discharged into product storage tank 14 through sieve plate 13 from the prilling tower bottom.Tail gas is taken away from top of tower through suspension settlement chamber 15, enters foam eluting column 5 through cyclonic separator 2, and drip washing enters atmosphere by vacuum fan 10 after purifying.The particulate of adding from cyclonic separator 2 returns prilling tower 1 through powder diverting valve 11 under compressed-air actuated effect.
Preparation LiCl dilute solution is squeezed into header tank 4 with it in storage tank 7, and through foam eluting column 5 and tail gas counter current contact from cyclonic separator 2, the fine powder LiCl in the tail gas is soluble in water, becomes the LiCl dilute solution to flow in the storage tank 7, squeezes into header tank 4 with pump 6.Through repeatedly circulation, when the concentration of LiCl reaches about 170g/l in the storage tank 7, squeeze into header tank 3, for production particle LiCl usefulness with pump 6.
Processing parameter:
LiCl crystal seed height: 320mm;
LiCl seed size: φ 2.5～6mm, 60%mm; φ 0.5～2.5mm, 40%;
Hot blast temperature: 392 ℃;
Hot-blast pressure: 3.7kPa;
Revert pipe blast: 0.3MPa;
Trunnion pressure :-100Pa;
LiCl strength of solution: 176g/l;
Material spray flow: 420l/h;
Material spray pressure: 0.35MPa;
Fluidized layer temperature: 180～210 ℃;
Blowing pressure reduction: 3.3kPa;
Foam eluting column top hole pressure :-1.8kPa;
Foam column drip washing temperature out: 85～90 ℃;
The particle LiCl epigranular of output is about φ 1mm, and hourly output is about 70kg.
Claims (4)
1. a lithium chloride drying technique is characterized in that, this technology adopts fluidization and spray-drying technology, and its process control parameter is:
LiCl strength of solution: 150～320g/l;
Fluidized drying prilling tower (1) import hot blast temperature: 300～450 ℃;
The interior hot blast wind speed of fluidized drying prilling tower (1): 1.0～4.0m/s;
Hot-blast pressure: 2.0～4.0kPa;
LiCl solution nozzle flow: 300～450l/h;
LiCl solution nozzle pressure: 0.1～0.4MPa;
Particle LiCl water content :≤0.5%;
Particle LiCl particle diameter: φ 1～8mm.
2. according to the drying technique of claim 1, it is characterized in that the drying cartridge of this process using is equipped with: fluidized drying prilling tower (1), nozzle (12), press empty injector (18).
3. according to the drying technique of claim 1 or 2, it is characterized in that described fluidized drying prilling tower (1) bottom is provided with sieve plate (13), its percentage of open area is 20～30%, and the aperture is φ 3～6mm.
4. according to the drying-granulating Technology of claim 1 or 2, it is characterized in that the employed pressure pneumatics of the empty injector of described pressure (18) power is 0.1～0.4MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97107592 CN1204621A (en) | 1997-07-08 | 1997-07-08 | Production process technology and device of granular lithium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97107592 CN1204621A (en) | 1997-07-08 | 1997-07-08 | Production process technology and device of granular lithium chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1204621A true CN1204621A (en) | 1999-01-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97107592 Pending CN1204621A (en) | 1997-07-08 | 1997-07-08 | Production process technology and device of granular lithium chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1204621A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102371133A (en) * | 2010-08-20 | 2012-03-14 | 天津大沽化工股份有限公司 | Granulation method of sodium peroxide |
| CN103058231A (en) * | 2012-10-26 | 2013-04-24 | 新余赣锋有机锂有限公司 | Method for preparing anhydrous lithium bromide |
| CN101652170B (en) * | 2006-12-07 | 2013-06-05 | 菲仕兰品牌公司 | Method and apparatus for spray drying and powder produced using said method |
| CN103387242A (en) * | 2013-07-25 | 2013-11-13 | 天津长芦海晶集团有限公司 | Equipment and technology for recycling and reusing medicinal sodium chloride particulate matters |
| CN105014063A (en) * | 2015-07-17 | 2015-11-04 | 中国兵器科学研究院宁波分院 | Spray granulation device suitable for active powder and granulation method thereof |
| CN107362749A (en) * | 2012-03-14 | 2017-11-21 | 艾德凡斯化学公司 | The method and apparatus for being used to be granulated with Stress control |
-
1997
- 1997-07-08 CN CN 97107592 patent/CN1204621A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101652170B (en) * | 2006-12-07 | 2013-06-05 | 菲仕兰品牌公司 | Method and apparatus for spray drying and powder produced using said method |
| CN102371133A (en) * | 2010-08-20 | 2012-03-14 | 天津大沽化工股份有限公司 | Granulation method of sodium peroxide |
| CN102371133B (en) * | 2010-08-20 | 2013-09-11 | 天津大沽化工股份有限公司 | Granulation method of sodium peroxide |
| CN107362749A (en) * | 2012-03-14 | 2017-11-21 | 艾德凡斯化学公司 | The method and apparatus for being used to be granulated with Stress control |
| CN103058231A (en) * | 2012-10-26 | 2013-04-24 | 新余赣锋有机锂有限公司 | Method for preparing anhydrous lithium bromide |
| CN103058231B (en) * | 2012-10-26 | 2014-09-10 | 江西赣锋锂业股份有限公司 | Method for preparing anhydrous lithium bromide |
| CN103387242A (en) * | 2013-07-25 | 2013-11-13 | 天津长芦海晶集团有限公司 | Equipment and technology for recycling and reusing medicinal sodium chloride particulate matters |
| CN103387242B (en) * | 2013-07-25 | 2015-02-18 | 天津长芦海晶集团有限公司 | Equipment and technology for recycling and reusing medicinal sodium chloride particulate matters |
| CN105014063A (en) * | 2015-07-17 | 2015-11-04 | 中国兵器科学研究院宁波分院 | Spray granulation device suitable for active powder and granulation method thereof |
| CN105014063B (en) * | 2015-07-17 | 2017-03-29 | 中国兵器科学研究院宁波分院 | Suitable for the spray granulation plant of active powder |
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