CN106915763A - A kind of high-purity anhydrous lanthanum chloride preparation technology - Google Patents
A kind of high-purity anhydrous lanthanum chloride preparation technology Download PDFInfo
- Publication number
- CN106915763A CN106915763A CN201710301962.4A CN201710301962A CN106915763A CN 106915763 A CN106915763 A CN 106915763A CN 201710301962 A CN201710301962 A CN 201710301962A CN 106915763 A CN106915763 A CN 106915763A
- Authority
- CN
- China
- Prior art keywords
- container
- lanthanum chloride
- crystal
- vacuum
- warming
- 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
- C01F17/253—Halides
- C01F17/271—Chlorides
-
- 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 belongs to anhydrous lanthanum chloride preparing technical field, a kind of high-purity anhydrous lanthanum chloride preparation technology is disclosed, comprised the following steps successively：S1：Lanthanum carbonate is crushed, addition diluted hydrochloric acid dissolution is untill gained mixed liquor ph is 2~3；S2：It is filtrated to get lanthanum chloride mixing stoste；S3：Lanthanum chloride is mixed into stoste to be put into container, then to container vacuum-pumping, until vacuum is 0.08Pa~0.28Pa in container, then distillation is proceeded by, vapo(u)rizing temperature is 100~130 degrees Celsius, when plane of crystal not rewetting in container, stop distillation, remaining crystal is lanthanum chloride crystal in container；S4：Vacuum state in holding container, injects ethanol liquid, and continuation is heated to container, is warming up to 70 DEG C, and constant temperature 2 hours obtains LaCl33H2O crystal；160 DEG C are warming up to again, and constant temperature obtains LaCl3H2O crystal in 2 hours；250 DEG C are warming up to again, and constant temperature obtains anhydrous lanthanum chloride in 4 hours.The present invention is simple to operate, and reaction is easily controlled, can the more convenient anhydrous lanthanum chloride crystal for obtaining higher purity.
Description
Technical field
The present invention relates to anhydrous lanthanum chloride preparing technical field, specifically refer to a kind of high-purity anhydrous lanthanum chloride and prepare work
Skill.
Background technology
Due to the strong moisture pick-up properties of anhydrous lanthanum chloride, the lanthanum chloride product that we obtain at present generally includes anhydrous chlorination
Lanthanum and many chloride hydrate lanthanum compounds, the purity of anhydrous lanthanum chloride is not high.
In order to remove the presence of anhydrous lanthanum chloride product reclaimed water as far as possible, it is necessary to be heated to anhydrous lanthanum chloride product.
But, due to anhydrous lanthanum chloride strong moisture pick-up properties in itself, even so, the purity of anhydrous lanthanum chloride is also typically merely able to reach
To 90% or so, it is impossible to further purification.
The content of the invention
It is an object of the invention to：Overcome the deficiencies in the prior art, there is provided a kind of high-purity anhydrous lanthanum chloride preparation technology.
The present invention is simple to operate, and reaction is easily controlled, can the more convenient anhydrous lanthanum chloride crystal for obtaining higher purity.
The present invention is achieved through the following technical solutions：
A kind of high-purity anhydrous lanthanum chloride preparation technology, comprises the following steps successively：
S1：After lanthanum carbonate is crushed, diluted hydrochloric acid dissolution is gradually dropped, with stirring during instillation, when straight carbonic acid
After lanthanum powder dissolves substantially, continuation instills watery hydrochloric acid untill gained mixed liquor ph is 2~3；
S2：The acidity acidity mixed solution obtained in filtration step S1, obtains lanthanum chloride mixing stoste；
S3：Lanthanum chloride is mixed into stoste to be put into container, then to container vacuum-pumping, until vacuum is in container
0.08Pa~0.28Pa, then proceeds by distillation, and vapo(u)rizing temperature is 100~130 degrees Celsius, when plane of crystal is no longer in container
During moistening, stop distillation, remaining crystal is lanthanum chloride crystal in container；
S4：Vacuum state in holding container, injects ethanol liquid, and continuation is heated to container, is warming up to 70 DEG C, constant temperature
2 hours, obtain LaCl33H2O crystal；160 DEG C are warming up to again, and constant temperature obtains LaCl3H2O crystal in 2 hours；It is warming up to again
250 DEG C, constant temperature obtains anhydrous lanthanum chloride in 4 hours.
As a preferred mode, in step s 2, selected filter screen is 1000 mesh.
As a preferred mode, in step s3, vacuum is 0.08Pa in container.
As a preferred mode, in step s3, vacuum is 0.18Pa in container.
As a preferred mode, in step S3, vacuum is 0.28Pa in container.
The present invention compared with prior art, with advantages below and beneficial effect：The present invention is simple to operate, the reaction easily palm
Control, can the more convenient anhydrous lanthanum chloride crystal for obtaining higher purity.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Specific embodiment
Further described in detail below in conjunction with the accompanying drawings, but embodiments of the present invention not limited to this：
Embodiment 1：
Referring to Fig. 1, a kind of high-purity anhydrous lanthanum chloride preparation technology is comprised the following steps successively：
S1：After lanthanum carbonate is crushed, diluted hydrochloric acid dissolution is gradually dropped, with stirring during instillation, when straight carbonic acid
After lanthanum powder dissolves substantially, continuation instills watery hydrochloric acid untill gained mixed liquor ph is 2~3；
S2：The acidity acidity mixed solution obtained in filtration step S1, obtains lanthanum chloride mixing stoste；
S3：Lanthanum chloride is mixed into stoste to be put into container, then to container vacuum-pumping, distillation is then proceeded by, distilled
Temperature is 100 degrees Celsius, when plane of crystal not rewetting in container, stops distillation, and remaining crystal is lanthanum chloride in container
Crystal；
S4：Vacuum state in holding container, injects ethanol liquid, and continuation is heated to container, is warming up to 70 DEG C, constant temperature
2 hours, obtain LaCl33H2O crystal；160 DEG C are warming up to again, and constant temperature obtains LaCl3H2O crystal in 2 hours；It is warming up to again
250 DEG C, constant temperature obtains anhydrous lanthanum chloride in 4 hours.
As a preferred mode, in step s 2, selected filter screen is 1000 mesh.
As a preferred mode, in step s3, vacuum is 0.08Pa in container.
Embodiment 2：
A kind of high-purity anhydrous lanthanum chloride preparation technology, comprises the following steps successively：
S1：After lanthanum carbonate is crushed, diluted hydrochloric acid dissolution is gradually dropped, with stirring during instillation, when straight carbonic acid
After lanthanum powder dissolves substantially, continuation instills watery hydrochloric acid untill gained mixed liquor ph is 2~3；
S2：The acidity acidity mixed solution obtained in filtration step S1, obtains lanthanum chloride mixing stoste；
S3：Lanthanum chloride is mixed into stoste to be put into container, then to container vacuum-pumping, distillation is then proceeded by, distilled
Temperature is 110 degrees Celsius, when plane of crystal not rewetting in container, stops distillation, and remaining crystal is lanthanum chloride in container
Crystal；
S4：Vacuum state in holding container, injects ethanol liquid, and continuation is heated to container, is warming up to 70 DEG C, constant temperature
2 hours, obtain LaCl33H2O crystal；160 DEG C are warming up to again, and constant temperature obtains LaCl3H2O crystal in 2 hours；It is warming up to again
250 DEG C, constant temperature obtains anhydrous lanthanum chloride in 4 hours.
As a preferred mode, in step s 2, selected filter screen is 1000 mesh.
As a preferred mode, in step s3, vacuum is 0.18Pa in container.
Embodiment 3：
A kind of high-purity anhydrous lanthanum chloride preparation technology, comprises the following steps successively：
S1：After lanthanum carbonate is crushed, diluted hydrochloric acid dissolution is gradually dropped, with stirring during instillation, when straight carbonic acid
After lanthanum powder dissolves substantially, continuation instills watery hydrochloric acid untill gained mixed liquor ph is 2~3；
S2：The acidity acidity mixed solution obtained in filtration step S1, obtains lanthanum chloride mixing stoste；
S3：Lanthanum chloride is mixed into stoste to be put into container, then to container vacuum-pumping, distillation is then proceeded by, distilled
Temperature is 130 degrees Celsius, when plane of crystal not rewetting in container, stops distillation, and remaining crystal is lanthanum chloride in container
Crystal；
S4：Vacuum state in holding container, injects ethanol liquid, and continuation is heated to container, is warming up to 70 DEG C, constant temperature
2 hours, obtain LaCl33H2O crystal；160 DEG C are warming up to again, and constant temperature obtains LaCl3H2O crystal in 2 hours；It is warming up to again
250 DEG C, constant temperature obtains anhydrous lanthanum chloride in 4 hours.
As a preferred mode, in step s 2, selected filter screen is 1000 mesh.
As a preferred mode, in step s3, vacuum is 0.28Pa in container.
Embodiment 4：
The difference gained anhydrous lanthanum chloride product purity of testing example 1~3, its data such as following table.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Control group | |
| Product purity | 98% | 96% | 95% | 90% |
The present invention is simple to operate, and reaction is easily controlled, can the more convenient anhydrous lanthanum chloride crystal for obtaining higher purity.
The above, is only presently preferred embodiments of the present invention, not does any formal limitation to the present invention, it is every according to
Any simple modification, the equivalent variations made to above example according to technical spirit of the invention, each fall within protection of the invention
Scope.
Claims (5)
1. a kind of high-purity anhydrous lanthanum chloride preparation technology, it is characterised in that comprise the following steps successively：
S1：After lanthanum carbonate is crushed, diluted hydrochloric acid dissolution is gradually dropped, with stirring during instillation, when straight lanthanum carbonate powder
After last basic dissolving, continuation instills watery hydrochloric acid untill gained mixed liquor ph is 2~3；
S2：The acidity acidity mixed solution obtained in filtration step S1, obtains lanthanum chloride mixing stoste；
S3：By lanthanum chloride mix stoste be put into container, then to container vacuum-pumping, until in container vacuum be 0.08Pa~
0.28Pa, then proceeds by distillation, and vapo(u)rizing temperature is 100~130 degrees Celsius, when plane of crystal not rewetting in container,
Stop distillation, remaining crystal is lanthanum chloride crystal in container；
S4：Vacuum state in holding container, injects ethanol liquid, and continuation is heated to container, is warming up to 70 DEG C, and constant temperature 2 is small
When, obtain LaCl33H2O crystal；160 DEG C are warming up to again, and constant temperature obtains LaCl3H2O crystal in 2 hours；250 are warming up to again
DEG C, constant temperature obtains anhydrous lanthanum chloride in 4 hours.
2. a kind of high-purity anhydrous lanthanum chloride preparation technology according to claim 1, it is characterised in that：In step s 2,
Selected filter screen is 1000 mesh.
3. a kind of high-purity anhydrous lanthanum chloride preparation technology according to claim 1, it is characterised in that：In step s3,
Vacuum is 0.08Pa in container.
4. a kind of high-purity anhydrous lanthanum chloride preparation technology according to claim 1, it is characterised in that：In step s3,
Vacuum is 0.18Pa in container.
5. a kind of high-purity anhydrous lanthanum chloride preparation technology according to claim 1, it is characterised in that：In step s3,
Vacuum is 0.28Pa in container.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710301962.4A CN106915763A (en) | 2017-05-02 | 2017-05-02 | A kind of high-purity anhydrous lanthanum chloride preparation technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710301962.4A CN106915763A (en) | 2017-05-02 | 2017-05-02 | A kind of high-purity anhydrous lanthanum chloride preparation technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106915763A true CN106915763A (en) | 2017-07-04 |
Family
ID=59567763
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710301962.4A Pending CN106915763A (en) | 2017-05-02 | 2017-05-02 | A kind of high-purity anhydrous lanthanum chloride preparation technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106915763A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107857288A (en) * | 2017-11-29 | 2018-03-30 | 中铝广西国盛稀土开发有限公司 | A kind of preparation method of the lanthanum chloride of good dispersion |
| CN114477265A (en) * | 2020-11-13 | 2022-05-13 | 南京正济医药研究有限公司 | Preparation method of lanthanum carbonate tetrahydrate |
| CN114634198A (en) * | 2022-03-31 | 2022-06-17 | 山东金能环保科技有限公司 | Preparation method of high-purity anhydrous lanthanum chloride |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037216A (en) * | 2006-03-14 | 2007-09-19 | 宁波大学 | Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method |
| CN102502757A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous lanthanum chloride or cerium chloride by programmed heating method |
| CN104973617A (en) * | 2015-07-01 | 2015-10-14 | 乐山沃耐稀电子材料有限公司 | Preparation method of anhydrous lanthanum chloride |
-
2017
- 2017-05-02 CN CN201710301962.4A patent/CN106915763A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037216A (en) * | 2006-03-14 | 2007-09-19 | 宁波大学 | Preparation technique of anhydrous lanthanum chloride by chlorination baking dehydration method |
| CN102502757A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous lanthanum chloride or cerium chloride by programmed heating method |
| CN104973617A (en) * | 2015-07-01 | 2015-10-14 | 乐山沃耐稀电子材料有限公司 | Preparation method of anhydrous lanthanum chloride |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107857288A (en) * | 2017-11-29 | 2018-03-30 | 中铝广西国盛稀土开发有限公司 | A kind of preparation method of the lanthanum chloride of good dispersion |
| CN114477265A (en) * | 2020-11-13 | 2022-05-13 | 南京正济医药研究有限公司 | Preparation method of lanthanum carbonate tetrahydrate |
| CN114477265B (en) * | 2020-11-13 | 2023-11-03 | 南京正济医药研究有限公司 | Preparation method of lanthanum carbonate tetrahydrate |
| CN114634198A (en) * | 2022-03-31 | 2022-06-17 | 山东金能环保科技有限公司 | Preparation method of high-purity anhydrous lanthanum chloride |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100357183C (en) | Preparation method of anhydrous cerium chloride | |
| CN106915763A (en) | A kind of high-purity anhydrous lanthanum chloride preparation technology | |
| CN104003445B (en) | A kind of method of producing high-dissolvability Ammonium Heptamolybdate | |
| CN103011807B (en) | Method for preparing strontium titanate powder | |
| CN107758715A (en) | A kind of method for preparing high-crystallinity high-purity boehmite | |
| CN104445346B (en) | A kind of hydrothermal synthesis method of nano yttrium oxide powder | |
| CN103204823B (en) | Method for purifying 1, 2-benzisothiazole-3-ketone | |
| CN105016373A (en) | Method for producing copper chloride through waste etching liquid containing copper | |
| CN104513174A (en) | Cyclic utilization process and device for waste acid produced during production of dinitolmide | |
| CN102303941A (en) | Deep dealkalizing method of red mud in alumina factory | |
| CN103058246B (en) | A kind of calcium sulfate produces the method for high-purity calcium oxide | |
| CN102502756A (en) | Preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by programmed heating method | |
| CN105665748A (en) | Method for preparing high-purity superfine silver powder | |
| CN105776967A (en) | Preparation method for fiber needled felt-enhanced sodium metaaluminate-modified aerogel | |
| CN103088421B (en) | The method of chemosynthesis high-purity hexagonal monocrystal calcium fluoride | |
| WO2021036391A1 (en) | Method for removing humate and oxalate impurities in bayer liquor | |
| EP3954654A1 (en) | System and method for preparing ultrafine silica by leaching silicate ore using hydrogen chloride gas | |
| CN106397347A (en) | Method for producing irganox 565 | |
| CN103508974A (en) | Method for treating methyl 2-(aminosulfonyl)benzoate crystallization mother solution | |
| CN106430278B (en) | A kind of preparation method of high-pure anhydrous acetic acid scandium and High-purity Sc Oxide | |
| CN104928403B (en) | A kind of compound lime emulsifier and its preparation method and application | |
| CN109019633B (en) | Preparation method of large-particle sodium hydrogen fluoride | |
| CN107986315B (en) | The recovery method of mixed waste liquor | |
| CN104891517A (en) | Method for producing potassium borofluoride by utilizing lithium hexafluorophosphate recovery acid mixture | |
| CN103739700B (en) | A kind of sodium benzoate extracts the method for chorionic gonadotrophin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170704 |
|
| RJ01 | Rejection of invention patent application after publication |