CN102807236A - Method for preparing lithium nitrate - Google Patents
Method for preparing lithium nitrate Download PDFInfo
- Publication number
- CN102807236A CN102807236A CN2011101456643A CN201110145664A CN102807236A CN 102807236 A CN102807236 A CN 102807236A CN 2011101456643 A CN2011101456643 A CN 2011101456643A CN 201110145664 A CN201110145664 A CN 201110145664A CN 102807236 A CN102807236 A CN 102807236A
- Authority
- CN
- China
- Prior art keywords
- lithium nitrate
- lithium
- product
- solution
- hydroxide monohydrate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 238000000034 method Methods 0.000 title claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000047 product Substances 0.000 claims abstract description 28
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 3
- 239000012265 solid product Substances 0.000 claims abstract description 3
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 24
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 23
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 23
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid group Chemical group C(C(=O)O)(=O)O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 21
- 238000002425 crystallisation Methods 0.000 claims description 18
- 239000012452 mother liquor Substances 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 235000006408 oxalic acid Nutrition 0.000 claims description 7
- 238000001556 precipitation Methods 0.000 claims description 7
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 4
- QDWNJWYHGDYFOG-UHFFFAOYSA-N [N+](=O)(O)[O-].[Li] Chemical compound [N+](=O)(O)[O-].[Li] QDWNJWYHGDYFOG-UHFFFAOYSA-N 0.000 claims description 3
- ZWWCURLKEXEFQT-UHFFFAOYSA-N dinitrogen pentoxide Inorganic materials [O-][N+](=O)O[N+]([O-])=O ZWWCURLKEXEFQT-UHFFFAOYSA-N 0.000 claims description 3
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000006200 vaporizer Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 37
- 238000001704 evaporation Methods 0.000 abstract description 16
- 238000001816 cooling Methods 0.000 abstract description 6
- 238000010790 dilution Methods 0.000 abstract description 3
- 239000012895 dilution Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000010413 mother solution Substances 0.000 abstract description 2
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 abstract 6
- 238000001914 filtration Methods 0.000 abstract 1
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000012716 precipitator Substances 0.000 abstract 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 15
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 15
- 239000011575 calcium Substances 0.000 description 15
- 229910052791 calcium Inorganic materials 0.000 description 15
- 239000011777 magnesium Substances 0.000 description 15
- 229910052749 magnesium Inorganic materials 0.000 description 15
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- 239000010935 stainless steel Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 9
- 239000011591 potassium Substances 0.000 description 9
- 229910052700 potassium Inorganic materials 0.000 description 9
- 239000011734 sodium Substances 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 230000008020 evaporation Effects 0.000 description 8
- 239000000498 cooling water Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 210000003298 dental enamel Anatomy 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for preparing lithium nitrate. The method comprises the following steps: (1) adding nitric acid at the weight concentration of 40-98 percent into pure water, adding lithium carbonate or lithium hydroxide for neutralization reaction, neutralizing by using lithium hydroxide until the pH is 7+/-0.5, obtaining a lithium nitrate solution, adding a precipitator, and filtering; (2) sending the lithium nitrate solution obtained in the step (1) into an evaporator, and evaporating until the temperature of the solution is 150+/-10DEG C; (3) cooling a product obtained in the step (2) to the temperature of 50+/-10DEG C, and crystallizing; and (4) performing solid-liquid separation on a product obtained in the step (3), collecting the separated solid product, namely hemihydrated lithium nitrate, and drying in vacuum to obtain an anhydrous lithium nitrate product. By the method, product cost is low, energy consumption is low, operation conditions are mild, and a mother solution can be recycled without being added with a great amount of water for dilution.
Description
Technical field
The present invention relates to a kind of method of producing lithium nitrate.
Technical background
Lithium nitrate is a kind of lithium salts chemical commonly used, in lithium-ion battery electrolytes, is able in recent years add and uses.
Usually, lithium nitrate prepares with following method: Quilonum Retard or Lithium Hydroxide MonoHydrate and nitric acid are reacted, then the solution evaporation of handling well, crystallization, separation, drying are obtained anhydrous nitric acid lithium product.
The major defect of this method is: product cost is high; Streams flux and energy consumption are higher in the production process; Can only use HP steam or electrical heating device in the evaporative process; Operational condition is harsh; Have relatively high expectations to what equipment, separating medium, operator safety were protected; Mother liquor must add more water dilution could continue the circulation cycle use.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing lithium nitrate, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
(1) adding weight concentration in the pure water is the nitric acid of 40-98%, adds Quilonum Retard or Lithium Hydroxide MonoHydrate and carries out neutralization reaction, and using Lithium Hydroxide MonoHydrate to be neutralized to pH then is 7 ± 0.5, obtains lithium nitrate solution, adds precipitation agent, filters;
The weight ratio of component is: the nitric acid of 65-98%: water: Quilonum Retard or Lithium Hydroxide MonoHydrate=1: 0.32～1: 0.35～0.67;
Add precipitation agent, precipitated calcium, magnesium, sulfate radical foreign matter;
Described precipitation agent is selected from oxalic acid, ammonium oxalate, hydrated barta or barium carbonate etc.;
Precipitation agent: Quilonum Retard or Lithium Hydroxide MonoHydrate=1: 100～1000, weight ratio;
(2) lithium nitrate solution that step (2) is obtained is sent into vaporizer, and the temperature that is evaporated to solution is 150 ℃ ± 10 ℃;
(3) product that step (2) is obtained is cooled to 50 ℃ ± 10 ℃, crystallization;
(4) with the product solid-liquid separation of step (3), collecting isolated solid product, is half water lithium nitrate, and vacuum-drying promptly obtains anhydrous nitric acid lithium product;
Drying pressure is-0.02～-0.092 MPa, and drying temperature is 100～180 ℃; Drying temperature needs strict control, just can not dissolve, phenomenon such as caking;
The lithium nitrate mother liquor that solid-liquid separation obtains returns step (1), recycles.
Method of the present invention, product cost is low, and energy consumption is lower, and operational condition is gentle, and mother liquor must not add more water dilution, just can continue circulation cycle and use.
Embodiment
The following example is only being explained the present invention, and does not limit the scope of the invention.
Embodiment 1
Used Quilonum Retard and Lithium Hydroxide MonoHydrate are technical grade, and its content is 99.0-99.5%, and the content of major impurity content such as sodium, potassium, calcium, magnesium, sulfate radical is 20-1000ppm, and used nitric acid is technical grade, and content is 98%.
(1) adds pure water 1500Kg in the 5M3 enamel reaction still, open induced draft fan, add nitric acid 1500Kg, add technical grade Quilonum Retard 800Kg under stirring, add the back and stirred 30 minutes, adjust solution PH=7 ± 0.5, need Lithium Hydroxide MonoHydrate 70Kg approximately with Lithium Hydroxide MonoHydrate;
(2) add 2.13Kg oxalic acid, add the 4.01Kg hydrated barta, precipitated calcium, magnesium, sulfate radical foreign matter.
(3) solution is filtered with plate-and-frame filter press;
(4) will filter good solution and join in the 3M3 stainless steel evaporating kettle, and stir down and boil, evaporate with being steam heated to, preferred, add in the centre and to filter good lithium nitrate solution, control liquid level well, evaporating terminal temperature is 150 ℃ ± 10 ℃;
(5) will evaporate good lithium nitrate solution and be cooled to 60 ℃, separate out half water lithium nitrate crystallization;
(6) lithium nitrate solution that crystallisation by cooling is good carries out solid-liquid separation with whizzer, obtains 703Kg half water lithium nitrate crystallization, and the mother liquor that obtains adds the 150Kg pure water and deposits for use;
(7) isolated half water lithium nitrate wet feed carries out drying with 1.5M3 stainless steel bipyramid Vacuumdrier, opens revolution, and the steam heating material is opened by the open vacuum system, and final drying temperature is 125 ℃, and the drying machine vacuum pressure is-0.092 Mpa;
Dried lithium nitrate is cooled under 35 ℃, obtains powdered anhydrous lithium nitrate product;
Adopt the method for Shanghai City company standard regulation to detect, moisture content weight content 0.08%, important foreign matter contents such as sodium, potassium, calcium, magnesium, sulfate radical are all less than 100ppm, and product quality is much better than general industry level product standard.
Embodiment 2
Used Quilonum Retard and Lithium Hydroxide MonoHydrate are technical grade, and its content is 99-99.5%, and the content of major impurity content such as sodium, potassium, calcium, magnesium, sulfate radical is 20-1000ppm, and used nitric acid is technical grade, and content is 98%.
(1) adds pure water 1500Kg in the 5M3 enamel reaction still, open induced draft fan, add nitric acid 1500Kg, add technical grade Quilonum Retard 800Kg under stirring, add the back and stirred 30 minutes, adjust solution PH=7 ± 0.5, need Lithium Hydroxide MonoHydrate 70Kg approximately with Lithium Hydroxide MonoHydrate;
(2) add 2.05Kg oxalic acid, add the 3.88Kg hydrated barta, precipitated calcium, magnesium, sulfate radical foreign matter.
(3) solution is released in the storage tank, filters with pressure filter with the mother liquor merging of embodiment 1.
(4) will filter good solution and join in the 3M3 stainless steel evaporating kettle, and stir down and boil with being steam heated to, and evaporate, the centre is added and is filtered good lithium nitrate solution, controls liquid level well, and evaporating terminal temperature is 150 ℃ ± 10 ℃.
(5) lithium nitrate solution that evaporation is good is cooled to 40 ℃, separates out half water lithium nitrate crystallization, wherein contains a small amount of anhydrous crystal.
(6) lithium nitrate solution that crystallisation by cooling is good carries out solid-liquid separation with whizzer, obtains 1100Kg half water lithium nitrate crystallization; The mother liquor that obtains adds the 250Kg pure water and deposits for use.
(7) isolated half water lithium nitrate wet feed carries out drying with 1.5M3 stainless steel bipyramid Vacuumdrier, and final drying temperature is 125 ℃, and dryer inner pressure is-0.092 Mpa.The lithium nitrate that oven dry is good is cooled under 35 ℃ with recirculated cooling water, obtains powdered anhydrous lithium nitrate product.
Adopt the method for Shanghai City company standard regulation to detect, water content 0.08%, important foreign matter contents such as sodium, potassium, calcium, magnesium, sulfate radical are all less than 100ppm, and product quality is much better than general industry level product standard.
(8) repeat said process reject mother liquor when foreign matter content is near the mark.Total yield is 93.5%.
Embodiment 3
Used Quilonum Retard and Lithium Hydroxide MonoHydrate are analytical pure, and its content is 99.5-99.9%, the content of major impurity content such as sodium, potassium, calcium, magnesium, sulfate radical are less than 100ppm, and used nitric acid is analytical pure, and content is 98%.
(1) adds pure water 1500Kg in the 5M3 enamel reaction still, open induced draft fan, add nitric acid 1500Kg, add analytical pure Quilonum Retard 800Kg under stirring, add the back and stirred 30 minutes, adjust solution PH=7 ± 0.5, need Lithium Hydroxide MonoHydrate 70Kg approximately with Lithium Hydroxide MonoHydrate;
(2) add 0.25Kg oxalic acid, adding 0.43Kg hydrated barta, precipitated calcium, magnesium, sulfate radical foreign matter.
(3) solution is released in the storage tank, filters with plate-and-frame filter press.
(4) will filter good solution and join in the 3M3 stainless steel evaporating kettle, and stir down and boil, open induced draft fan with being steam heated to; Vapor pressure is controlled at 0.3-0.5Mpa, evaporates, and the centre is added and filtered good lithium nitrate solution; Control liquid level well, the evaporation terminal point is controlled at 150 ℃ ± 10 ℃.
(5) lithium nitrate solution that evaporation is good is cooled to 60 ℃ with recirculated cooling water, separates out half water lithium nitrate crystallization, wherein contains a small amount of anhydrous crystal.
(6) lithium nitrate solution that crystallisation by cooling is good carries out solid-liquid separation with whizzer, obtains 700Kg half water lithium nitrate crystallization; The mother liquor that obtains adds the 150Kg pure water and deposits for use.
(7) isolated half water lithium nitrate wet feed carries out drying with 1.5M3 stainless steel bipyramid Vacuumdrier, opens revolution, and the steam heating material is opened by the open vacuum system, and final drying temperature is 125 ℃, and the dryer inner vacuum pressure is-0.092 Mpa.The lithium nitrate that oven dry is good is cooled under 35 ℃ with recirculated cooling water, obtains powdered anhydrous lithium nitrate product.
Moisture content weight content 0.08%, important foreign matter contents such as sodium, potassium, calcium, magnesium, sulfate radical are all less than 20ppm, and product quality is much better than 99.9% product standard.
Embodiment 4
Press the method for embodiment 2, replace industrial raw material with the analytical pure raw material, carry out Recycling Mother Solution, reject mother liquor when foreign matter content is near the mark, total yield are 94.2%
Embodiment 5
Used Quilonum Retard and Lithium Hydroxide MonoHydrate are technical grade, and its content is 99-99.5%, and the content of major impurity content such as sodium, potassium, calcium, magnesium, sulfate radical is 20-1000ppm, and used nitric acid is technical grade, and content is 65%.
(1) adds pure water 740Kg in the 5M3 enamel reaction still, open induced draft fan, add nitric acid 2260Kg, add technical grade Quilonum Retard 800Kg under stirring, add the back and stirred 30 minutes, adjust solution PH=7 ± 0.5, need Lithium Hydroxide MonoHydrate 70Kg approximately with Lithium Hydroxide MonoHydrate;
(2) add 2.11Kg oxalic acid, adding 3.65Kg hydrated barta, precipitated calcium, magnesium, sulfate radical foreign matter.
(3) solution is released in the storage tank, filters with plate-and-frame filter press.
(4) will filter good solution and join in the 3M3 stainless steel evaporating kettle, and stir down and boil, open induced draft fan with being steam heated to; Vapor pressure is controlled at 0.3-0.5Mpa, evaporates, and the centre is added and filtered good lithium nitrate solution; Control liquid level well, the evaporation terminal point is controlled at 150 ℃ ± 10 ℃.
(5) lithium nitrate solution that evaporation is good is cooled to 50 ℃ with recirculated cooling water, separates out half water lithium nitrate crystallization, wherein contains a small amount of anhydrous crystal.
(6) lithium nitrate solution that crystallisation by cooling is good carries out solid-liquid separation with whizzer, obtains 707Kg half water lithium nitrate crystallization; The mother liquor that obtains adds the 150Kg pure water and deposits for use.
(7) isolated half water lithium nitrate wet feed carries out drying with 1.5M3 stainless steel bipyramid Vacuumdrier, opens revolution, and the steam heating material is opened by the open vacuum system, and final drying temperature is 125 ℃, and the dryer inner vacuum pressure is-0.092 Mpa.The lithium nitrate that oven dry is good is cooled under 35 ℃ with recirculated cooling water, obtains powdered anhydrous lithium nitrate product.
Water content 0.08%, important foreign matter contents such as sodium, potassium, calcium, magnesium, sulfate radical are all less than 100ppm, and product quality is much better than general industry level product standard.
Embodiment 6
(1) adds pure water 740Kg in the 5M3 enamel reaction still, open induced draft fan, add 65% technical grade nitric acid 2260Kg; Stir and add technical grade Quilonum Retard 800Kg down; Add the back and stirred 30 minutes,, need Lithium Hydroxide MonoHydrate 70Kg approximately with industrial stage monohydrate lithium hydroxide adjustment solution PH=7 ± 0.5.
(2) add 2.02Kg oxalic acid, adding 3.57Kg hydrated barta, precipitated calcium, magnesium, sulfate radical foreign matter.
(3) solution is released in the storage tank, merges with the mother liquor that produces among the embodiment 5 and filter with plate-and-frame filter press.
(4) will filter good solution and join in the 3M3 stainless steel evaporating kettle, and stir down and boil, open induced draft fan with being steam heated to; Vapor pressure is controlled at 0.3-0.5Mpa, evaporates, and the centre is added and filtered good lithium nitrate solution; Control liquid level well, the evaporation terminal point is controlled at 150 ℃ ± 10 ℃.
(5) lithium nitrate solution that evaporation is good is cooled to 45 ℃ with recirculated cooling water, separates out half water lithium nitrate crystallization, wherein contains a small amount of anhydrous crystal.
(6) lithium nitrate solution that crystallisation by cooling is good carries out solid-liquid separation with whizzer, obtains 1109Kg half water lithium nitrate crystallization; The mother liquor that obtains adds the 250Kg pure water and deposits for use.
(7) isolated half water lithium nitrate wet feed carries out drying with 1.5M3 stainless steel bipyramid Vacuumdrier, and final drying temperature is 125 ℃, and the dryer inner vacuum pressure is-0.092 Mpa.The lithium nitrate that oven dry is good is cooled under 35 ℃ with recirculated cooling water, obtains powdered anhydrous lithium nitrate product.
Water content 0.08%, important foreign matter contents such as sodium, potassium, calcium, magnesium, sulfate radical are all less than 30ppm, and product quality is much better than general industry level product standard.
(8) repeat said process reject mother liquor when foreign matter content is near the mark.Total yield is 93%.
Embodiment 7～8
Press the method for embodiment 5,6 respectively, replace industrial raw material, obtain the result of embodiment 3, embodiment 4 equally respectively with the analytical pure raw material.
Claims (6)
1. the preparation method of lithium nitrate is characterized in that, comprises the steps:
(1) adding weight concentration in the pure water is the nitric acid of 40-98%, adds Quilonum Retard or Lithium Hydroxide MonoHydrate and carries out neutralization reaction, and using Lithium Hydroxide MonoHydrate to be neutralized to pH then is 7 ± 0.5, obtains lithium nitrate solution, adds precipitation agent, filters;
(2) lithium nitrate solution that step (1) is obtained is sent into vaporizer, and the temperature that is evaporated to solution is 150 ℃ ± 10 ℃;
(3) product that step (2) is obtained is cooled to 50 ℃ ± 10 ℃, crystallization;
(4) with the product solid-liquid separation of step (3), collecting isolated solid product, is half water lithium nitrate, and vacuum-drying promptly obtains anhydrous nitric acid lithium product.
2. method according to claim 1 is characterized in that, the weight ratio of component is:
The nitric acid of 40-98%: water: Quilonum Retard or Lithium Hydroxide MonoHydrate=1: 0～1: 0.23～0.67.
3. method according to claim 2 is characterized in that, the weight ratio of component is: preferred, and the nitric acid of 65-98%: water: Quilonum Retard or Lithium Hydroxide MonoHydrate=1: 0.32～1: 0.35～0.67.
4. method according to claim 1 is characterized in that described precipitation agent is selected from oxalic acid, ammonium oxalate, hydrated barta or barium carbonate etc.; Precipitation agent: Quilonum Retard or Lithium Hydroxide MonoHydrate=1: 100～1000, weight ratio.
5. method according to claim 1 is characterized in that, the lithium nitrate mother liquor that solid-liquid separation obtains returns step (1), recycles.
6. according to each described method of claim 1～5, it is characterized in that dry vacuum pressure-0.02～-0.095 MPa, drying temperature are 100～180 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101456643A CN102807236A (en) | 2011-06-01 | 2011-06-01 | Method for preparing lithium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101456643A CN102807236A (en) | 2011-06-01 | 2011-06-01 | Method for preparing lithium nitrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102807236A true CN102807236A (en) | 2012-12-05 |
Family
ID=47231128
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101456643A Pending CN102807236A (en) | 2011-06-01 | 2011-06-01 | Method for preparing lithium nitrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102807236A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2959463A (en) * | 1957-07-03 | 1960-11-08 | American Potash & Chem Corp | Process for manufacture of lithium nitrate |
| CN102030344A (en) * | 2009-09-25 | 2011-04-27 | 上海中锂实业有限公司 | Preparation method of lithium fluoride |
-
2011
- 2011-06-01 CN CN2011101456643A patent/CN102807236A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2959463A (en) * | 1957-07-03 | 1960-11-08 | American Potash & Chem Corp | Process for manufacture of lithium nitrate |
| CN102030344A (en) * | 2009-09-25 | 2011-04-27 | 上海中锂实业有限公司 | Preparation method of lithium fluoride |
Non-Patent Citations (2)
| Title |
|---|
| 胡庆福: "《镁化合物生产与应用》", 31 March 2004, 化学工业出版社化学与应用化学出版中心 * |
| 韩长日等: "《精细无机化学品制造技术》", 31 August 2008, 科学技术文献出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101993105B (en) | Method for preparing light calcium carbonate and co-producing ammonium sulfate from phosphogypsum | |
| CN108568135B (en) | Manganese sulfate evaporation crystallization equipment and process | |
| CN103588225A (en) | Method for producing food-grade potassium chloride through multistage flash evaporation, cooling and continuous crystallization | |
| CN108359815A (en) | A kind of preparation method containing vanadium solution | |
| CN102910676B (en) | Preparation method of high-purity vanadium pentoxide | |
| CN103539164A (en) | Method for refining sodium sulfate powder from chromium-containing mirabilite | |
| CN103351010B (en) | Preparation process of battery-grade lithium carbonate | |
| CN112939034B (en) | Method for preparing battery-grade anhydrous lithium hydroxide from industrial-grade lithium carbonate | |
| CN106377993B (en) | A method and device for removing SO2 from flue gas with pyrolusite slurry and its resource utilization | |
| CN118724031A (en) | A hydrogenation method for purifying industrial-grade lithium carbonate and a process for purifying industrial-grade lithium carbonate using the method | |
| CN106904642A (en) | A kind of magnesium processes treatment liquid containing ammonium sulfate technique waste water and the method for reclaiming magnesium sulfate | |
| CN105819469B (en) | A kind of method that PMIDA abraum salt is handled using high-temperature S removal | |
| CN101857212B (en) | Method for producing food-grade monoammonium phosphate with wet-process phosphoric acid | |
| CN111268704A (en) | Method and device for treating lithium precipitation mother liquor | |
| CN102267717B (en) | Process for preparing zinc sulfate by evaporation and crystallization | |
| CN104130105A (en) | Method for recycling ethanol during production of p-methyl sulfonyl phenyl ethyl serinate | |
| CN103539170B (en) | Method for producing magnesium sulfate and industrial-grade monoammonium phosphate by using tail solution from refining of wet process phosphoric acid by solvent extraction method | |
| CN104129811A (en) | Process for preparing zinc sulfate | |
| CN105293796A (en) | Method for co-production of sodalumite and gypsum through activated clay production mother liquid | |
| CN102807236A (en) | Method for preparing lithium nitrate | |
| CN114735724B (en) | Method for recycling low-water-content sodium bromide from wastewater | |
| CN101214980A (en) | Method for producing large particles of heptahydrate magnesium sulfate and monohydrate magnesium sulfate from magnesium sulfate solution | |
| CN216737932U (en) | Electrolytic waste residue and fluorine-containing wastewater treatment device for electrolytic fluorine production process | |
| CN103664242A (en) | Caustic sludge treatment method | |
| CN104163410A (en) | Method for preparing calcium phosphite from industrial sodium hypophosphite waste residues |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 201424 Shanghai city Fengxian District Zhelin town science Road No. 1158 Applicant after: Shanghai China Lithium Industrial Co., Ltd. Address before: Fengxian District Zhelin Town East Zhongxing Road 201424 Shanghai City No. 8 Applicant before: Shanghai China Lithium Industrial Co., Ltd. |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20121205 |