CN106315655A - Method for producing high-purity lanthanum carbonate - Google Patents
Method for producing high-purity lanthanum carbonate Download PDFInfo
- Publication number
- CN106315655A CN106315655A CN201610605195.1A CN201610605195A CN106315655A CN 106315655 A CN106315655 A CN 106315655A CN 201610605195 A CN201610605195 A CN 201610605195A CN 106315655 A CN106315655 A CN 106315655A
- Authority
- CN
- China
- Prior art keywords
- lanthanum carbonate
- carbonate
- production method
- filtrate
- solution
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/247—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for producing high-purity lanthanum carbonate. The method comprises the following steps that 1, lanthanum carbonate is added into water to form a mixed solution; 2, concentrated nitric acid is added into the mixed solution obtained in the step 1 to be dissolved, the pH value is adjusted to range from 1.5 to 2 with ammonium hydroxide, the pH is adjusted to range from 4 to 4.5 with cerous carbonate after heating, and an acid solution is obtained; 3, the acid solution obtained in the step 2 is filtered, and filtrate is obtained; 4, the filtrate in the step 3 is concentrated; 5, the concentrated solution obtained in the step 4 is placed in a crystallizing disc to be naturally crystallized, and centrifugal dewatering is carried out; 6, water is added into crystals obtained after centrifugation in the step 5, and dissolving and diluting are carried out; 7, the solution obtained after being treated in the step 6 is heated to 50 DEG C, an ammonium bicarbonate solution is added slowly and then fast for sedimentation, and still standing is carried out after sedimentation is completed; 8, the sediment obtained after being treated in the step 7 is washed, and then centrifugal dewatering and packaging are carried out.
Description
Technical field
The invention belongs to Rare Earth Production field, be specifically related to the production method of a kind of high-purity lanthanum carbonate.
Background technology
The main uses of lanthanum carbonate is: produce lanthanum compound, such as lanthana, Lanthanum (III) nitrate etc., produces the PVC such as petroleum catalyst
Auxiliary agent etc..Also it is the medicine of a kind of novel anti-hyperphosphatemia with efficient phosphorus binding ability of discovered in recent years simultaneously.
Only have several factories at present and can produce this product, but the product impurity content of these manufacturer production is higher, has after dissolving
Machine thing content weight, it is impossible to fully meet user's requirement.
Summary of the invention
It is an object of the present invention to provide the production method of a kind of high-purity lanthanum carbonate, solve existing lanthanum carbonate product impurity content
Higher problem.
The technical scheme is that the production method of a kind of high-purity lanthanum carbonate, step is as follows:
(1), lanthanum carbonate is added to the water formation mixed liquor；
(2), in the mixed liquor that step (1) obtains, add concentrated nitric acid dissolving, and with ammonia adjustment pH value to 1.5-2, add
Adjust pH to 4-4.5 with cerous carbonate again after heat, obtain acid solution；
(3), the acid solution obtained in step (2) is filtrated to get filtrate；
(4), the filtrate in step (3) being concentrated, striking point solution concentration is calculated as 720-750 grams per liter by cerium oxide,
PH value 1-1.5；
(5), the concentrated solution obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifuge dehydration；
(6), the crystal after centrifugal in step (5) it is dissolved in water and dilutes, making la concn be calculated as 70g/ by oxide
L；
(7), after step (6) processes, the solution that obtains is heated to 50 DEG C, use the slowest after fast mode add bicarbonate
Ammonium salt solution precipitates, and stands after having precipitated；
(8), by the precipitation washing after step (7) process, it is then centrifuged for dehydration, packaging.
Further, in step (1), the weight ratio of lanthanum carbonate and water is 1 1.5.
Further, in step (2), the method for heating is: be heated to boiling, keeps more than 30min.
Further, in step (3), the method for filtration is: first with 200 mesh filter-cloth filterings, then the micropore with aperture 1-5um
Filter filters.
Further, in step (7), ammonium bicarbonate soln concentration is 100g/L.
Further, in step (7), refer to soon after elder generation is slow: first drip and rapidly join in time having a large amount of crystal to occur, precipitation
After completing, pH value is 6-7.
The present invention compared with prior art has the advantage that
1, in the present invention, use and first concentrate, then the mode of spontaneous nucleation, most metal ion can be removed.
2, in the present invention, using the slowest rear fast mode to add ammonium hydrogen carbonate, the lanthanum carbonate crystal particle diameter obtained is big, product
Specific surface area is little, and the metal ion of absorption is few.
3, the lanthanum carbonate purity that the production method of the present invention produces is the highest, TREO >=45% of lanthanum carbonate, La2O3/TREO
>=99.95%, Fe, Ca, Na, K, Pb, Zn, Mn, Al, Cu, Ni, Co, Cr ＜ 1ppm.
Detailed description of the invention
Embodiment 1
(1), 1 part of lanthanum carbonate is joined formation mixed liquor in 1.5 parts of pure water；
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and adjust back pH to 1.8 with ammonia, be heated to
Boiling, after 30 minutes, then with cerous carbonate readjustment pH to 4.3 to acid solution；
(3) it is, that 200 mesh filter clothes carry out being filtrated to get filtrate by the acid solution obtained in step (2) by aperture；
(4), the filtrate that step (3) obtains is carried out microfilter (aperture 4um) and be filtrated to get filtrate；
(5), the filtrate in (4) being concentrated, striking point solution concentration is calculated as 740 grams per liters, pH=1.3 by cerium oxide；
(6), the solution in step (5) is put into spontaneous nucleation in crystallizing pan, and centrifuge dehydration；
(7), the crystal in step (6) being dissolved in water and diluted, la concn is calculated as 70 grams per liter post-heating by oxide and arrives
50 degrees Celsius
(8), by the solution in step (7), the slowest rear fast mode is used to add the carbon that finite concentration is 100 grams per liters
Acid hydrogen ammonium salt solution precipitates, and stands 1 hour after having precipitated；
(9), the precipitation in step (8) is washed 5 times, be centrifuged dehydration, packaging.
Embodiment 2
(1), 1 part of lanthanum carbonate is joined formation mixed liquor in 2 parts of pure water；
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and adjust back pH to 1.5 with ammonia, be heated to
Boiling, after 30 minutes, then with cerous carbonate readjustment pH to 4 to acid solution；
(3) it is, that 200 mesh filter clothes carry out being filtrated to get filtrate by the acid solution obtained in step (2) by aperture；
(4), the filtrate that step (3) obtains is carried out microfilter (aperture 1um) and be filtrated to get filtrate；
(5), the filtrate in (4) being concentrated, striking point solution concentration is calculated as 720 grams per liters, pH=1 by cerium oxide；
(6), the solution in step (5) is put into spontaneous nucleation in crystallizing pan, and centrifuge dehydration；
(7), the crystal in step (6) being dissolved in water and diluted, la concn is calculated as 70 grams per liter post-heating by oxide and arrives
50 degrees Celsius
(8), by the solution in step (7), the slowest rear fast mode is used to add the carbon that finite concentration is 100 grams per liters
Acid hydrogen ammonium salt solution precipitates, and stands 1 hour after having precipitated；
(9), the precipitation in step (8) is washed 5 times, be centrifuged dehydration, packaging.
Embodiment 3
(1), 1 part of lanthanum carbonate is joined formation mixed liquor in 1 part of pure water；
(2) mixed liquor, by step (1) obtained adds concentrated nitric acid dissolve, and adjust back pH to 2 with ammonia, be heated to boiling
Rise, after 30 minutes, then with cerous carbonate readjustment pH4.5 to acid solution；
(3) it is, that 200 mesh filter clothes carry out being filtrated to get filtrate by the acid solution obtained in step (2) by aperture；
(4), the filtrate that step (3) obtains is carried out microfilter (aperture 5um) and be filtrated to get filtrate；
(5), the filtrate in (4) being concentrated, striking point solution concentration is calculated as 750 grams per liters, pH=1.5 by cerium oxide；
(6), the solution in step (5) is put into spontaneous nucleation in crystallizing pan, and centrifuge dehydration；
(7), the crystal in step (6) being dissolved in water and diluted, la concn is calculated as 70 grams per liter post-heating by oxide and arrives
50 degrees Celsius
(8), by the solution in step (7), the slowest rear fast mode is used to add the carbon that finite concentration is 100 grams per liters
Acid hydrogen ammonium salt solution precipitates, and stands 1 hour after having precipitated；
(9), the precipitation in step (8) is washed 5 times, be centrifuged dehydration, packaging.
Embodiment described above only have expressed the detailed description of the invention of the application, and it describes more concrete and detailed, but also
Therefore the restriction to the application protection domain can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, on the premise of conceiving without departing from technical scheme, it is also possible to make some deformation and improvement, these broadly fall into this
The protection domain of application.
Claims (6)
1. the production method of a high-purity lanthanum carbonate, it is characterised in that step is as follows:
(1), lanthanum carbonate is added to the water formation mixed liquor；
(2), in the mixed liquor that step (1) obtains, concentrated nitric acid dissolving is added, and with ammonia adjustment pH value to 1-1.5, after heating
Adjust pH to 4-4.5 with cerous carbonate again, obtain acid solution；
(3), the acid solution obtained in step (2) is filtrated to get filtrate；
(4), the filtrate in step (3) being concentrated, striking point solution concentration is calculated as 720-750 grams per liter, pH value by cerium oxide
1-1.5；
(5), the concentrated solution obtained in step (4) is put into spontaneous nucleation in crystallizing pan, and centrifuge dehydration；
(6), the crystal after centrifugal in step (5) it is dissolved in water and dilutes, making la concn be calculated as 70g/L by oxide；
(7), after step (6) processes, the solution that obtains is heated to 50 DEG C, use the slowest after fast mode to add ammonium hydrogen carbonate molten
Liquid precipitates, and stands after having precipitated；
(8), by the precipitation washing after step (7) process, it is then centrifuged for dehydration, packaging.
The production method of a kind of high-purity lanthanum carbonate the most according to claim 1, it is characterised in that in step (1), carbonic acid
The weight ratio of lanthanum and water is 1 1.5.
The production method of a kind of high-purity lanthanum carbonate the most according to claim 1, it is characterised in that in step (2), heating
Method be: be heated to boiling, keep more than 30min.
The production method of a kind of high-purity lanthanum carbonate the most according to claim 1, it is characterised in that in step (3), filters
Method be: first with 200 mesh filter-cloth filterings, then filter with the microfilter of aperture 1-5um.
The production method of a kind of high-purity lanthanum carbonate the most according to claim 1, it is characterised in that in step (7), carbonic acid
Hydrogen ammonium salt solution concentration is 100g/L.
The production method of a kind of high-purity lanthanum carbonate the most according to claim 1, it is characterised in that in step (7), the slowest
After refer to soon: first dripping and rapidly join in time having a large amount of crystal to occur, having precipitated rear pH value is 6-7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610605195.1A CN106315655A (en) | 2016-07-28 | 2016-07-28 | Method for producing high-purity lanthanum carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610605195.1A CN106315655A (en) | 2016-07-28 | 2016-07-28 | Method for producing high-purity lanthanum carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106315655A true CN106315655A (en) | 2017-01-11 |
Family
ID=57740067
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610605195.1A Pending CN106315655A (en) | 2016-07-28 | 2016-07-28 | Method for producing high-purity lanthanum carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106315655A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217712A (en) * | 2018-04-13 | 2018-06-29 | 四川沃耐稀新材料科技有限公司 | A kind of production method of the big grain size cerous carbonate of high-purity |
| CN108423703A (en) * | 2018-06-20 | 2018-08-21 | 乐山沃耐稀电子材料有限公司 | A kind of production method of fine grain shape cerous carbonate |
| CN108530289A (en) * | 2018-06-20 | 2018-09-14 | 乐山沃耐稀电子材料有限公司 | A kind of preparation method of lanthanum acetate |
| CN111115675A (en) * | 2018-10-11 | 2020-05-08 | 有研稀土新材料股份有限公司 | High-purity light lanthanum carbonate or lanthanum oxide and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012505A (en) * | 2007-02-05 | 2007-08-08 | 常州华南化工有限公司 | Method for preparing ultra-thin highly-pure lanthanum oxide by beneficiated lanthanum |
| CN101481131A (en) * | 2009-02-20 | 2009-07-15 | 包头市金蒙稀土有限责任公司 | Preparation of high purity cerous carbonate with high total amount of rare earth |
| CN104473963A (en) * | 2014-12-24 | 2015-04-01 | 厦门科明达科技有限公司 | Preparation method of rare earth chemical drug lanthanum carbonatechewable tablets |
| CN104925844A (en) * | 2015-06-11 | 2015-09-23 | 乐山沃耐稀电子材料有限公司 | Method for refining high-purity cerium carbonate |
| CN105502470A (en) * | 2015-12-31 | 2016-04-20 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Preparation method of low-impurity-entrainment lanthanum carbonate or cerium lanthanum carbonate |
-
2016
- 2016-07-28 CN CN201610605195.1A patent/CN106315655A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012505A (en) * | 2007-02-05 | 2007-08-08 | 常州华南化工有限公司 | Method for preparing ultra-thin highly-pure lanthanum oxide by beneficiated lanthanum |
| CN101481131A (en) * | 2009-02-20 | 2009-07-15 | 包头市金蒙稀土有限责任公司 | Preparation of high purity cerous carbonate with high total amount of rare earth |
| CN104473963A (en) * | 2014-12-24 | 2015-04-01 | 厦门科明达科技有限公司 | Preparation method of rare earth chemical drug lanthanum carbonatechewable tablets |
| CN104925844A (en) * | 2015-06-11 | 2015-09-23 | 乐山沃耐稀电子材料有限公司 | Method for refining high-purity cerium carbonate |
| CN105502470A (en) * | 2015-12-31 | 2016-04-20 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Preparation method of low-impurity-entrainment lanthanum carbonate or cerium lanthanum carbonate |
Non-Patent Citations (1)
| Title |
|---|
| 张继光: "《催化剂制备过程技术》", 31 August 2011 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217712A (en) * | 2018-04-13 | 2018-06-29 | 四川沃耐稀新材料科技有限公司 | A kind of production method of the big grain size cerous carbonate of high-purity |
| CN108423703A (en) * | 2018-06-20 | 2018-08-21 | 乐山沃耐稀电子材料有限公司 | A kind of production method of fine grain shape cerous carbonate |
| CN108530289A (en) * | 2018-06-20 | 2018-09-14 | 乐山沃耐稀电子材料有限公司 | A kind of preparation method of lanthanum acetate |
| CN111115675A (en) * | 2018-10-11 | 2020-05-08 | 有研稀土新材料股份有限公司 | High-purity light lanthanum carbonate or lanthanum oxide and preparation method thereof |
| CN111115675B (en) * | 2018-10-11 | 2023-03-10 | 有研稀土新材料股份有限公司 | High-purity light lanthanum carbonate or lanthanum oxide and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103145187B (en) | Production technology of harmless high-purity vanadium pentoxide | |
| CN106315655A (en) | Method for producing high-purity lanthanum carbonate | |
| CN103789550B (en) | The recovery method of vanadium potassium silicon in spent vanadium catalyst | |
| CN106335920A (en) | Production technology of low-chlorine cerium carbonate | |
| JP5406386B2 (en) | Method for producing manganese sulfate monohydrate | |
| CN102491419B (en) | Method for comprehensively recycling waste vanadium catalyst | |
| CN102502823B (en) | Preparation method for preparing high-tap density ammonium poly-vanadate | |
| CN102337409A (en) | Method for recovering vanadium from dephosphorization bottom flow residues | |
| CN102730757A (en) | Method for preparing high purity vanadium pentoxide through using ammonium metavanadate | |
| CN102531054A (en) | Purification method of ammonium metavanadate and preparation method of high-purity vanadium pentoxide | |
| CN104760996A (en) | Low-temperature crystallization method of ammonium polyvanadate | |
| CN103402909B (en) | Make UO3And/or U3O8It is converted into hydration UO4Method | |
| CN104843789A (en) | Method for purifying vanadium pentoxide | |
| CN105366722B (en) | The method of normal temperature extraction production high purity vanadic anhydride | |
| CN105016371A (en) | Preparation method of electronic grade ceric sulfate | |
| CN102602993A (en) | Method for recovering zirconium element from zirconium oxychloride crystallized mother liquor raffinate | |
| CN106044838B (en) | Production technology of low-sulfur lanthanum hydroxide | |
| CN104925844A (en) | Method for refining high-purity cerium carbonate | |
| CN102442700A (en) | Method for preparing high-purity spherical niobium oxide by peroxidizing precipitation | |
| CN110028088B (en) | Preparation method of battery-grade lithium carbonate | |
| CN108423703A (en) | A kind of production method of fine grain shape cerous carbonate | |
| CN103708566B (en) | Method for improving filtering performance of ferrous sulfate | |
| CN103667706B (en) | The separating and purifying method of gold in a kind of plation waste material | |
| CN110423893A (en) | The method that titanium tetrachloride purification tailings prepares vanadic sulfate | |
| CN106277022A (en) | A kind of production method of electronic-grade sulfuric acid cerium ammonium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170111 |
|
| RJ01 | Rejection of invention patent application after publication |