CN114634198A - Preparation method of high-purity anhydrous lanthanum chloride - Google Patents
Preparation method of high-purity anhydrous lanthanum chloride Download PDFInfo
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- CN114634198A CN114634198A CN202210335816.4A CN202210335816A CN114634198A CN 114634198 A CN114634198 A CN 114634198A CN 202210335816 A CN202210335816 A CN 202210335816A CN 114634198 A CN114634198 A CN 114634198A
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- Prior art keywords
- preparation
- lacl
- heating
- lanthanum chloride
- anhydrous lanthanum
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 title claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 8
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims description 15
- 239000007787 solid Substances 0.000 claims description 7
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000012805 post-processing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- JEROREPODAPBAY-UHFFFAOYSA-N [La].ClOCl Chemical compound [La].ClOCl JEROREPODAPBAY-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- 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
- C01F17/265—Fluorides
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention is suitable for the technical field of anhydrous lanthanum chloride production, and provides a preparation method of high-purity anhydrous lanthanum chloride, which comprises the following steps: s1, preparation of La2O3A solution; s2 preparation of Lacl3·7H2O；S3，Lacl3·7H2O, dehydrating; s4, post-treatment, the invention provides a preparation method of high-purity anhydrous lanthanum chloride, firstly, La2O3Adding into deionized water, heating and stirring, adding hydrochloric acid, and concentrating at high temperature to obtain Lacl3·7H2O, then to Lacl3·7H2And (2) dehydrating O, adding ammonium chloride in proportion, mixing, and performing post-treatment in a high-temperature environment, wherein compared with the prior art, the anhydrous lanthanum chloride in the product obtained by the anhydrous lanthanum chloride preparation method has the problems of low purity, incapability of meeting the use requirement, high preparation cost and complex operation, the Lacl obtained by the method is provided3High purity and preparation methodSimple, convenient operation and low cost.
Description
Technical Field
The invention relates to the technical field of anhydrous lanthanum chloride production, and particularly relates to a preparation method of high-purity anhydrous lanthanum chloride.
Background
The anhydrous lanthanum chloride is reddish or gray deliquescent crystal or blocky solid, can be dissolved in water, can generate lanthanum hydroxide or lanthanum oxychloride precipitate when being subjected to alkali, has neutral aqueous solution, and can be used for preparing petroleum cracking catalysts, extracting single rare earth products, smelting lanthanum-rich mixed rare earth metals and the like.
The anhydrous lanthanum chloride in the product obtained by the existing anhydrous lanthanum chloride preparation method has low purity, can not meet the use requirement, and has high preparation cost and complex operation.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity anhydrous lanthanum chloride, and aims to solve the problems that in the prior art, the purity of anhydrous lanthanum chloride in a product obtained by the preparation method of anhydrous lanthanum chloride is low, the use requirement cannot be met, the preparation cost is high, and the operation is complex.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of high-purity anhydrous lanthanum chloride comprises the following steps:
s1, preparation of La2O3Solution:
la2O3Adding into deionized water, heating, stirring and dissolving;
s2 preparation of Lacl3·7H2O：
Adding hydrochloric acid, adjusting pH, heating to 100 deg.C, and concentrating to obtain Lacl3·7H2O；
S3，Lacl3·7H2O, dehydration:
mixing Lacl3·7H2Placing the O in a vacuum drying oven, heating to 80 ℃, keeping constant temperature for drying for 8h, then heating to 160 ℃, keeping constant temperature for drying for 8h, finally heating to 200 ℃, keeping constant temperature for drying for 4 h;
s4, post-processing:
mixing the solid matter in the S3 and ammonium chloride according to a certain proportion, heating to 300 ℃ in a vacuum environment, keeping the constant temperature for 60-90 min to obtain the Lacl3。
Preferably, the temperature in the S1 is raised to 50-60 ℃.
Preferably, the mass fraction of hydrochloric acid in the S2 is 30%.
Preferably, the pH value of the S2 is adjusted to 2-3.
Preferably, the mass ratio of the solid matters to the ammonium chloride in the S4 is 4-5: 1.
The invention has at least the following beneficial effects:
the invention provides a high-purityThe preparation method of the anhydrous lanthanum chloride comprises the steps of firstly, preparing La2O3Adding into deionized water, heating and stirring, adding hydrochloric acid, and concentrating at high temperature to obtain Lacl3·7H2O, then to Lacl3·7H2And (3) dehydrating O, adding ammonium chloride in proportion, mixing, and performing post-treatment in a high-temperature environment, wherein compared with the prior art, the purity of anhydrous lanthanum chloride in the product obtained by the anhydrous lanthanum chloride preparation method is lower, the use requirement cannot be met, the preparation cost is higher, and the operation is complex, the method can be used for obtaining the Lacl3High purity, simple preparation method, convenient operation and low cost.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of high-purity anhydrous lanthanum chloride comprises the following steps:
s1, preparation of La2O3Solution:
la2O3Adding the mixture into deionized water, heating to 50-60 ℃, and stirring for dissolving;
s2 preparation of Lacl3·7H2O：
Adding 30% hydrochloric acid, adjusting pH to 3, heating to 100 deg.C, and concentrating to obtain Lacl3·7H2O；
S3，Lacl3·7H2O, dehydration:
mixing Lacl3·7H2Placing the O in a vacuum drying oven, heating to 80 ℃, keeping constant temperature for drying for 8h, then heating to 160 ℃, keeping constant temperature for drying for 8h, finally heating to 200 ℃, keeping constant temperature for drying for 4 h;
s4, post-processing:
mixing the solid substance in S3 with ammonium chloride at a mass ratio of 5:1, heating to 300 deg.C in vacuum environment, and holding the temperature for 60min to obtain Lacl3。
Example 2
A preparation method of high-purity anhydrous lanthanum chloride comprises the following steps:
s1, preparation of La2O3Solution:
la2O3Adding the mixture into deionized water, heating to 50-60 ℃, and stirring for dissolving;
s2 preparation of Lacl3·7H2O：
Adding hydrochloric acid with the mass fraction of 30%, adjusting the pH to 2, heating to 100 ℃, and concentrating to obtain Lacl3·7H2O；
S3，Lacl3·7H2O, dehydration:
mixing Lacl3·7H2Placing the O in a vacuum drying oven, heating to 80 ℃, keeping constant temperature for drying for 8h, then heating to 160 ℃, keeping constant temperature for drying for 8h, finally heating to 200 ℃, keeping constant temperature for drying for 4 h;
s4, post-processing:
mixing the solid matter in S3 with ammonium chloride at a mass ratio of 4:1, heating to 300 deg.C in vacuum environment, and holding the temperature for 90min to obtain Lacl3。
Comparative example 1
A preparation method of high-purity anhydrous lanthanum chloride comprises the following steps:
s1, preparation of La2O3Solution:
la2O3Adding the mixture into deionized water, heating to 50-60 ℃, and stirring for dissolving;
s2 preparation of Lacl3·7H2O：
Adding hydrochloric acid with the mass fraction of 30%, adjusting the pH to 2, heating to 100 ℃, and concentrating to obtain Lacl3·7H2O；
S3，Lacl3·7H2O, dehydration:
mixing Lacl3·7H2Placing O in a vacuum drying oven, heating to 80 deg.C, drying at constant temperature for 8 hr, heating to 160 deg.C, drying at constant temperature for 8 hr, heating to 200 deg.C, drying at constant temperature for 4 hr to obtain Lacl3。
The products obtained in examples 1-2 and comparative example 1 were tested, and Lacl in the product obtained in example 23The purity is highest and reaches 96 percent.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A preparation method of high-purity anhydrous lanthanum chloride is characterized by comprising the following steps:
s1, preparation of La2O3Solution:
la2O3Adding into deionized water, heating, stirring and dissolving;
s2 preparation of Lacl3·7H2O：
Adding hydrochloric acid, adjusting pH, heating to 100 deg.C, and concentrating to obtain Lacl3·7H2O；
S3，Lacl3·7H2O, dehydration:
mixing Lacl3·7H2Placing the O in a vacuum drying oven, heating to 80 ℃, keeping constant temperature for drying for 8h, then heating to 160 ℃, keeping constant temperature for drying for 8h, finally heating to 200 ℃, keeping constant temperature for drying for 4 h;
s4, post-processing:
mixing the solid matter in the S3 and ammonium chloride according to a certain proportion, heating to 300 ℃ in a vacuum environment, keeping the constant temperature for 60-90 min to obtain the Lacl3。
2. The method for preparing high-purity anhydrous lanthanum chloride according to claim 1, which is characterized in that: and heating the S1 to 50-60 ℃.
3. The method for preparing high-purity anhydrous lanthanum chloride according to claim 1, which is characterized in that: the mass fraction of the hydrochloric acid in the S2 is 30%.
4. The method for preparing high-purity anhydrous lanthanum chloride according to claim 1, which is characterized in that: and adjusting the pH value to 2-3 in the S2.
5. The method for preparing high-purity anhydrous lanthanum chloride according to claim 1, which is characterized in that: the mass ratio of the solid matters to the ammonium chloride in the S4 is 4-5: 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210335816.4A CN114634198A (en) | 2022-03-31 | 2022-03-31 | Preparation method of high-purity anhydrous lanthanum chloride |
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| CN202210335816.4A CN114634198A (en) | 2022-03-31 | 2022-03-31 | Preparation method of high-purity anhydrous lanthanum chloride |
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| CN114634198A true CN114634198A (en) | 2022-06-17 |
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| CN202210335816.4A Pending CN114634198A (en) | 2022-03-31 | 2022-03-31 | Preparation method of high-purity anhydrous lanthanum chloride |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1785814A (en) * | 2005-12-26 | 2006-06-14 | 包头市世博稀土冶金有限责任公司 | Preparation method of anhydrous cerium chloride |
| 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 |
| CN106915763A (en) * | 2017-05-02 | 2017-07-04 | 乐山沃耐稀电子材料有限公司 | A kind of high-purity anhydrous lanthanum chloride preparation technology |
| CN110040758A (en) * | 2019-04-16 | 2019-07-23 | 兰州大学 | A kind of preparation method of anhydrous rare-earth chlorination |
-
2022
- 2022-03-31 CN CN202210335816.4A patent/CN114634198A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1785814A (en) * | 2005-12-26 | 2006-06-14 | 包头市世博稀土冶金有限责任公司 | Preparation method of anhydrous cerium chloride |
| 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 |
| CN106915763A (en) * | 2017-05-02 | 2017-07-04 | 乐山沃耐稀电子材料有限公司 | A kind of high-purity anhydrous lanthanum chloride preparation technology |
| CN110040758A (en) * | 2019-04-16 | 2019-07-23 | 兰州大学 | A kind of preparation method of anhydrous rare-earth chlorination |
Non-Patent Citations (2)
| Title |
|---|
| 时文中;左春山;褚意新;徐启杰;: "氯化铵焙烧氯化氧化镧的热力学研究", 南阳理工学院学报, no. 06 * |
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Application publication date: 20220617 |