CN104973617A - Preparation method of anhydrous lanthanum chloride - Google Patents
Preparation method of anhydrous lanthanum chloride Download PDFInfo
- Publication number
- CN104973617A CN104973617A CN201510378814.3A CN201510378814A CN104973617A CN 104973617 A CN104973617 A CN 104973617A CN 201510378814 A CN201510378814 A CN 201510378814A CN 104973617 A CN104973617 A CN 104973617A
- Authority
- CN
- China
- Prior art keywords
- crystal
- filtrate
- preparation
- lanthanum chloride
- obtains
- 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
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a preparation method of anhydrous lanthanum chloride. The preparation method comprises following steps: 1, lanthanum carbonate powder is dissolved in dilute hydrochloric acid until pH value is detected to be 2-3, and stirring reaction is carried out for 1 to 5h; 2, an obtained solution is filtered so as to remove impurities; 3, an obtained mixed solution is subjected to millipore filtration so as to obtain a filtrate; 4, the filtrate is subjected to evaporative concentration; 5, an obtained product is cooled on a crystallizing pan to 20 DEG C, and is subjected to 12 to 24h of nature crystallization; 6, an obtained filter liquor is filtered so as to obtain a crystal, and the crystal is delivered into a centrifugal hydroextractor for 20 to 60min of dehydration so as to obtain an intermediate product; 7, the intermediate product is delivered into a non-oxidation drying oven, is heated to 70 DEG C, and is subjected to thermal insulation for 2h so as to obtain LaCl3*3H2O crystal, is heated to 160 DEG C, and is subjected to thermal insulation for 2h so as to obtain LaCl3*H2O crystal, and then is heated to 250 DEG C, and is subjected to thermal insulation for 4h so as to obtain anhydrous lanthanum chloride. Beneficial effects of the preparation method are that: reaction processes are simple, and are convenient to control; production period is short; a clear transparent solution can be obtained via dissolving of the obtained finished product, and impurity content is low.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of preparation method of anhydrous lanthanum chloride.
Background technology
Lanthanum trichloride comprises anhydrous lanthanum chloride and many chloride hydrate lanthanum compound.Lanthanum trichloride, mainly as preparing catalyst of cracking petroleum, also can make the raw material extracting single rare earth product or smelt lanthanum rich norium.
The preparation method of current Lanthanum trichloride is mainly obtained at the hydrochloric acid system of methyl alcohol by lanthanum trioxide and hydrochloric acid, and also in HCl atmosphere, many hydrated lanthanum chloride intensifications are dewatered and obtain, and also obtains 300 degrees Celsius of reactions under protective atmosphere by lanthanum trioxide and ammonium chloride.But these methods all have the following disadvantages: 1, reaction process is too complicated, and reaction conditions is not easily controlled, be not suitable for producing in enormous quantities.2, generating period is long; 3, finished product solubleness is low, and solution is not as clear as crystal.
Summary of the invention
Goal of the invention: the present invention is directed to above-mentioned prior art Problems existing and make improvement, namely the invention discloses a kind of preparation method of anhydrous lanthanum chloride.
Technical scheme: a kind of preparation method of anhydrous lanthanum chloride, comprises the following steps:
(1), by 1 part of Phosbloc powder form acidic solution with after 2 ~ 4 parts of diluted hydrochloric acid dissolutions, then drip appropriate dilute hydrochloric acid in oxytropism solution until the PH of acidic solution is 2 ~ 3, stirring reaction 1 ~ 5 hour;
(2) filtering and impurity removing
The mixed solution of precipitation will be also had by obtaining filtrate after 1000 object screen filtrations in step (1);
(3) micro-filtration
The filtrate of step (2) is added after millipore filter carries out micro-filtration and obtains filtrate;
(4) evaporation concentration
The filtrate of step (3) is heated to 150 DEG C, is incubated and obtains concentrated solution in 5 ~ 7 hours;
(5) crystallisation by cooling
The concentrated solution of step (4) is cooled to 20 DEG C, and crystallization is filtered and is obtained Neodymium trichloride crystal for 12 ~ 18 hours;
(6), by the filtrate in step (5) obtain crystal, and put into centrifuge dehydration 20 ~ 60min through crystal and remove after mother liquor and obtain intermediate product;
(7), by the intermediate product that step (6) obtains put into the non-oxidation baking oven being full of rare gas element and be warming up to 70 DEG C, constant temperature 2 hours, obtains LaCl
33H
2o crystal; Be warming up to 160 DEG C again, constant temperature obtains LaCl in 2 hours
3h
2o crystal; Be warming up to 250 DEG C again, namely constant temperature obtain anhydrous lanthanum chloride in 4 hours.
A kind of preferred version as a kind of in the present invention preparation method of anhydrous lanthanum chloride: in step (1), the particle diameter of Phosbloc powder is 100 ~ 800 orders.
A kind of preferred version as a kind of in the present invention preparation method of anhydrous lanthanum chloride: the dilute hydrochloric acid massfraction in step (1) lower than 20% hydrochloric acid.
A kind of preferred version as a kind of in the present invention preparation method of anhydrous lanthanum chloride: in step (2), the aperture of the filtering net of millipore filter is 0.5 ~ 1 μm.
A kind of preferred version as a kind of in the present invention preparation method of anhydrous lanthanum chloride: the concentration of the filtrate that step (2) obtains is not less than 200g/L.
Beneficial effect: the preparation method of a kind of anhydrous lanthanum chloride disclosed by the invention has following beneficial effect:
1, reaction process is simple, and reaction process is controlled, is applicable to producing in enormous quantities;
2, with short production cycle;
3, finished product dissolution rate is high.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of a kind of anhydrous lanthanum chloride disclosed by the invention.
Embodiment:
Below the specific embodiment of the present invention is described in detail.
The number of present specification all refers to mass fraction.
Specific embodiment 1
A preparation method for anhydrous lanthanum chloride, comprises the following steps:
(1), by 1 part of Phosbloc powder form acidic solution with after 2 parts of diluted hydrochloric acid dissolutions, then drip appropriate dilute hydrochloric acid in oxytropism solution until the PH of acidic solution is after 2, stirring reaction 1 hour;
(2) filtering and impurity removing
The mixed solution of precipitation will be also had by obtaining filtrate after 1000 object screen filtrations in step (1);
(3) micro-filtration
The filtrate of step (2) is added after millipore filter carries out micro-filtration and obtains filtrate;
(4) evaporation concentration
The filtrate of step (3) is heated to 150 DEG C, is incubated and obtains concentrated solution in 5 hours;
(5) crystallisation by cooling
The concentrated solution of step (4) is cooled to 20 DEG C, and crystallization is filtered and is obtained Neodymium trichloride crystal for 12 hours;
(6), by the filtrate in step (5) obtain crystal, and put into the centrifuge 20min that dewaters through crystal and remove after mother liquor and obtain intermediate product;
(7), by the intermediate product that step (6) obtains put into the non-oxidation baking oven being full of rare gas element and be warming up to 70 DEG C, constant temperature 2 hours, obtains LaCl
33H
2o crystal; Be warming up to 160 DEG C again, constant temperature obtains LaCl in 2 hours
3h
2o crystal; Be warming up to 250 DEG C again, namely constant temperature obtain anhydrous lanthanum chloride in 4 hours.
In the present embodiment, in step (1), the particle diameter of Phosbloc powder is 100 orders.
In the present embodiment, the dilute hydrochloric acid massfraction in step (1) is the hydrochloric acid of 20%.
In the present embodiment, in step (2), the aperture of the filtering net of millipore filter is 0.5 μm.
In the present embodiment, the concentration of the filtrate that step (2) obtains is 200g/L.
Specific embodiment 2
A preparation method for anhydrous lanthanum chloride, comprises the following steps:
(1), by 1 part of Phosbloc powder form acidic solution with after 4 parts of diluted hydrochloric acid dissolutions, then drip appropriate dilute hydrochloric acid in oxytropism solution until the PH of acidic solution is after 3, stirring reaction 5 hours;
(2) filtering and impurity removing
The mixed solution of precipitation will be also had by obtaining filtrate after 1000 object screen filtrations in step (1);
(3) micro-filtration
The filtrate of step (2) is added after millipore filter carries out micro-filtration and obtains filtrate;
(4) evaporation concentration
The filtrate of step (3) is heated to 150 DEG C, is incubated and obtains concentrated solution in 7 hours;
(5) crystallisation by cooling
The concentrated solution of step (4) is cooled to 20 DEG C, and crystallization is filtered and is obtained Neodymium trichloride crystal for 18 hours;
(6), by the filtrate in step (5) obtain crystal, and put into centrifuge dehydration 20 ~ 60min through crystal and remove after mother liquor and obtain intermediate product;
(7), by the intermediate product that step (6) obtains put into the non-oxidation baking oven being full of rare gas element and be warming up to 70 DEG C, constant temperature 2 hours, obtains LaCl
33H
2o crystal; Be warming up to 160 DEG C again, constant temperature obtains LaCl in 2 hours
3h
2o crystal; Be warming up to 250 DEG C again, namely constant temperature obtain anhydrous lanthanum chloride in 4 hours.
In the present embodiment, in step (1), the particle diameter of Phosbloc powder is 800 orders.
In the present embodiment, the dilute hydrochloric acid massfraction in step (1) is the hydrochloric acid of 18%.
In the present embodiment, in step (2), the aperture of the filtering net of millipore filter is 1 μm.
In the present embodiment, the concentration of the filtrate that step (2) obtains is 230g/L.
Specific embodiment 3
A preparation method for anhydrous lanthanum chloride, comprises the following steps:
(1), by 1 part of Phosbloc powder form acidic solution with after 3 parts of diluted hydrochloric acid dissolutions, then drip appropriate dilute hydrochloric acid in oxytropism solution until the PH of acidic solution is after 2.5, stirring reaction 3 hours;
(2) filtering and impurity removing
The mixed solution of precipitation will be also had by obtaining filtrate after 1000 object screen filtrations in step (1);
(3) micro-filtration
The filtrate of step (2) is added after millipore filter carries out micro-filtration and obtains filtrate;
(4) evaporation concentration
The filtrate of step (3) is heated to 150 DEG C, is incubated and obtains concentrated solution in 6 hours;
(5) crystallisation by cooling
The concentrated solution of step (4) is cooled to 20 DEG C, and crystallization is filtered and is obtained Neodymium trichloride crystal for 15 hours;
(6), by the filtrate in step (5) obtain crystal, and put into the centrifuge 30min that dewaters through crystal and remove after mother liquor and obtain intermediate product;
(7), by the intermediate product that step (6) obtains put into the non-oxidation baking oven being full of rare gas element and be warming up to 70 DEG C, constant temperature 2 hours, obtains LaCl
33H
2o crystal; Be warming up to 160 DEG C again, constant temperature obtains LaCl in 2 hours
3h
2o crystal; Be warming up to 250 DEG C again, namely constant temperature obtain anhydrous lanthanum chloride in 4 hours.
In the present embodiment, in step (1), the particle diameter of Phosbloc powder is 400 orders.
In the present embodiment, the dilute hydrochloric acid massfraction in step (1) is the hydrochloric acid of 15%.
In the present embodiment, in step (2), the aperture of the filtering net of millipore filter is 0.8 μm.
In the present embodiment, the concentration of the filtrate that step (2) obtains is 230g/L.
Above embodiments of the present invention are elaborated.But the present invention is not limited to above-mentioned embodiment, in the ken that art those of ordinary skill possesses, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (5)
1. a preparation method for anhydrous lanthanum chloride, is characterized in that, comprises the following steps:
(1), by 1 part of Phosbloc powder form acidic solution with after 2 ~ 4 parts of diluted hydrochloric acid dissolutions, then drip appropriate dilute hydrochloric acid in oxytropism solution until the PH of acidic solution is 2 ~ 3, stirring reaction 1 ~ 5 hour;
(2) filtering and impurity removing
The mixed solution of precipitation will be also had by obtaining filtrate after 1000 object screen filtrations in step (1);
(3) micro-filtration
The filtrate of step (2) is added after millipore filter carries out micro-filtration and obtains filtrate;
(4) evaporation concentration
The filtrate of step (3) is heated to 150 DEG C, is incubated and obtains concentrated solution in 5 ~ 7 hours;
(5) crystallisation by cooling
The concentrated solution of step (4) is cooled to 20 DEG C, and crystallization is filtered and is obtained Neodymium trichloride crystal for 12 ~ 18 hours;
(6), by the filtrate in step (5) obtain crystal, and put into centrifuge dehydration 20 ~ 60min through crystal and remove after mother liquor and obtain intermediate product;
(7), by the intermediate product that step (6) obtains put into the non-oxidation baking oven being full of rare gas element and be warming up to 70 DEG C, constant temperature 2 hours, obtains LaCl
33H
2o crystal; Be warming up to 160 DEG C again, constant temperature obtains LaCl in 2 hours
3h
2o crystal; Be warming up to 250 DEG C again, namely constant temperature obtain anhydrous lanthanum chloride in 4 hours.
2. the preparation method of a kind of anhydrous lanthanum chloride according to claim 1, is characterized in that, in step (1), the particle diameter of Phosbloc powder is 100 ~ 800 orders.
3. the preparation method of a kind of anhydrous lanthanum chloride according to claim 1, is characterized in that, the dilute hydrochloric acid massfraction in step (1) lower than 20% hydrochloric acid.
4. the preparation method of a kind of anhydrous lanthanum chloride according to claim 1, is characterized in that, in step (2), the aperture of the filtering net of millipore filter is 0.5 ~ 1 μm.
5. the preparation method of a kind of anhydrous lanthanum chloride according to claim 1, is characterized in that, the concentration of the filtrate that step (2) obtains is not less than 200g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510378814.3A CN104973617A (en) | 2015-07-01 | 2015-07-01 | Preparation method of anhydrous lanthanum chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510378814.3A CN104973617A (en) | 2015-07-01 | 2015-07-01 | Preparation method of anhydrous lanthanum chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104973617A true CN104973617A (en) | 2015-10-14 |
Family
ID=54270649
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510378814.3A Pending CN104973617A (en) | 2015-07-01 | 2015-07-01 | Preparation method of anhydrous lanthanum chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104973617A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044838A (en) * | 2016-07-28 | 2016-10-26 | 乐山沃耐稀电子材料有限公司 | Production technology of low-sulfur lanthanum hydroxide |
| CN106495199A (en) * | 2016-10-18 | 2017-03-15 | 清远市嘉禾稀有金属有限公司 | A kind of preparation method of granule lanthanum chloride crystal |
| 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 |
| 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 |
| CN110092404A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of preparation method of anhydrous neodymium chloride |
| CN112867695A (en) * | 2018-10-26 | 2021-05-28 | 住友化学株式会社 | Method for producing hydrous lanthanum carbonate |
| 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 |
|---|---|---|---|---|
| CN1539739A (en) * | 2003-10-30 | 2004-10-27 | 北京交通大学 | Chemical coprecipitation method for synthesizing, powder material of terrae rare salt of normal niobic acid |
| 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 |
-
2015
- 2015-07-01 CN CN201510378814.3A patent/CN104973617A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1539739A (en) * | 2003-10-30 | 2004-10-27 | 北京交通大学 | Chemical coprecipitation method for synthesizing, powder material of terrae rare salt of normal niobic acid |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 陈红兵等: "LaCl3:Ce3+晶体生长用无水氯化镧的制备", 《人工晶体学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044838A (en) * | 2016-07-28 | 2016-10-26 | 乐山沃耐稀电子材料有限公司 | Production technology of low-sulfur lanthanum hydroxide |
| CN106495199A (en) * | 2016-10-18 | 2017-03-15 | 清远市嘉禾稀有金属有限公司 | A kind of preparation method of granule lanthanum chloride crystal |
| 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 |
| 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 |
| CN110092404A (en) * | 2018-01-28 | 2019-08-06 | 蒋盼盼 | A kind of preparation method of anhydrous neodymium chloride |
| CN112867695A (en) * | 2018-10-26 | 2021-05-28 | 住友化学株式会社 | Method for producing hydrous lanthanum carbonate |
| 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 |
|---|---|---|
| CN104973617A (en) | Preparation method of anhydrous lanthanum chloride | |
| CN102502823B (en) | Preparation method for preparing high-tap density ammonium poly-vanadate | |
| CN103361486B (en) | Method for extracting high purity scandium oxide and titanium from waste acid solution containing scandium and titanium | |
| CN100469696C (en) | Method for preparing battery-stage anhydrous lithium chloride | |
| CN109180749B (en) | Method for preparing high-purity N-acetylneuraminic acid hydrate by using supersaturation crystallization method | |
| CN103555937B (en) | Two sections of sedimentations refine platinum technique | |
| CN102863004A (en) | Purification and preparation method of high-purity scandium oxide | |
| CN104944459A (en) | Preparation method of anhydrous neodymium chloride | |
| CN103922954A (en) | Method for preparing glycine zinc chelate | |
| CN105016373A (en) | Method for producing copper chloride through waste etching liquid containing copper | |
| CN109231180B (en) | Method for preparing high-purity barium dihydrogen phosphate | |
| CN102320585A (en) | Method for direct production of industrial-grade ammonium biphosphate by wet-process phosphoric acid | |
| CN108609635A (en) | A kind of method prepared by potassium nitrate | |
| CN102828036B (en) | Method of preparing potassium metavanadate solution from vanadium slag | |
| CN103896232B (en) | Raffinate twice neutralisation prepares the method for industrial grade monoammonium phosphate | |
| CN104386751A (en) | Ultra-high-purity tantalum oxide and method for preparing same | |
| CN103641150A (en) | Method for preparing low-calcium high-purity lanthanum oxide by one-step extraction | |
| CN108409554B (en) | Synthetic method of iridium acetate | |
| CN103265072A (en) | Method for crystallizing zirconium oxychloride | |
| CN102633292A (en) | Method for preparing copper sulphate by using copper sponge without roasting and evaporating | |
| CN102417207A (en) | Process for preparing ammonium dimolybdate crystal by using sulfuric acid and molybdenum calcine | |
| CN106629809B (en) | Method for purifying coarse scandium oxide | |
| CN104557685A (en) | Method for producing nicotinic acid by using nicotinamide mother solution | |
| CN102731340B (en) | Preparation method of demethyl aureomycin hydrochloride | |
| CN111592042B (en) | Method for preparing high-purity vanadium pentoxide by ammonium-free vanadium precipitation of vanadium liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | 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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151014 |