CN110065963A - A kind of preparation method of anhydrous rare-earth chlorination - Google Patents
A kind of preparation method of anhydrous rare-earth chlorination Download PDFInfo
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- CN110065963A CN110065963A CN201910343112.XA CN201910343112A CN110065963A CN 110065963 A CN110065963 A CN 110065963A CN 201910343112 A CN201910343112 A CN 201910343112A CN 110065963 A CN110065963 A CN 110065963A
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- 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
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- 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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Abstract
The present invention provides a kind of anhydrous rare-earth chlorination (RECl3) preparation method.It is involved in the present invention to include: S1, using hydrochloric acid dissolve rare earth oxide to form rare-earth chloride solution to step；S2, ammonium chloride is added into dissolved rare-earth chloride solution；S3, in a heated condition fried dry obtain the solid mixture of rare earth-iron-boron and ammonium chloride containing the crystallization water；S4, the solid mixture after above-mentioned fried dry is transferred in sublimation apparatus, 390 DEG C are risen to from 80 DEG C by the way of gradient increased temperature, it carries out vacuumizing heating operation simultaneously, in vacuumizing heating process, the crystallization water of ammonium chloride and rare earth-iron-boron is successively removed, to obtain the anhydrous rare-earth chlorination of high-purity.Have a characteristic that production process is simple and safe, occur without side reaction, the anhydrous rare-earth chlorination of preparation purity is high, is conducive to large-scale production using the method for the invention.
Description
Technical field
The invention belongs to technical field of rare earth material preparation, prepare nothing by raw material of rare earth oxide more particularly to one kind
The method of water rare earth-iron-boron.
Technical background
Rare earth element accounts for about 1/7th of element periodic table, includes scandium, yttrium and 15 kinds of lanthanide series.To rare earth
The further investigation of element will not only facilitate discovery new property, explore new material, and the development that will push inorganic chemistry.Rare earth
The characteristics such as the excellent light of element, electricity, magnetic are known as the treasure-house of new material, and have become important strategic element, are world technologies
The commanding elevation of competition.Anhydrous rare-earth chlorination is similarly subjected to more and more extensive as the precursor for preparing organolanthanide complexes
Concern.
At present it has been reported that anhydrous rare-earth chlorination preparation method mainly include (1) chemical vapor transport method: using dilute
Native oxide reacts at high temperature with aluminium chloride generates anhydrous rare-earth chlorination, the severe reaction conditions, generates in reaction process
High pressure is unfavorable for scale safety in production；(2) ammonium chloride sublimed method: rare earth oxide turns at high temperature in the presence of ammonium chloride
Anhydrous rare-earth chlorination is turned to, if rare earth is changeable valence rare earth, during the reaction often with redox reaction, the production of generation
Object is impure；(3) three sections of fluidization process: fluidisation dehydration is carried out by three sections of aqueous rare earth-iron-boron point, is dehydrated in hydrogen chloride gas atmosphere
Lower progress, this method need strict temperature control and wind speed, it is desirable that condition it is more stringent, and hydrogen chloride is needed in preparation process
Gas shield；(4) preparation method that CN108455650A discloses a kind of anhydrous samarium trichloride uses chlorination using samarium oxide as raw material
Ammonium solid is reacted, then is passed through dry hydrogen chloride gas, is heated to fully reacting, and product is dry, obtains anhydrous chlorination
Shirt needs to be passed through inert gas in preparation process, increases cost, and this method also needs hydrogen chloride gas and protected.
The use of hydrogen chloride gas increases the risk of release of toxic gas, is unfavorable for keeping the safety in production.
Anhydrous rare-earth chlorination has important application in rare earth coordination chemical field, therefore, further development operation
Easy, safety, the high method for preparing anhydrous rare-earth chlorination of product purity have important value.
Summary of the invention
The purpose of the present invention is provide a kind of prepare aiming at the problem that synthesis anhydrous rare-earth chlorination technical deficiency at present
The method of anhydrous rare-earth chlorination, this method have many advantages, such as that easy to operate, product purity is high, yield is high.
The purpose of the present invention is what is be achieved through the following technical solutions:
The raw material for preparing of the synthesis anhydrous rare-earth chlorination includes: rare earth oxide, hydrochloric acid, ammonium chloride.
In order to achieve the purpose that foregoing invention, the invention adopts the following technical scheme:
S1, rare earth oxide is dissolved using hydrochloric acid, obtains the aqueous solution of rare earth-iron-boron；
S2, ammonium chloride is added into dissolved rare-earth chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
S3, in a heated condition evaporation and fried dry obtain the solid mixing of rare earth-iron-boron and ammonium chloride containing the crystallization water
Object；
S4, the solid mixture after above-mentioned fried dry is transferred in sublimation apparatus, from 80 DEG C by the way of gradient increased temperature
390 DEG C are risen to, while carrying out decompression operation, during heating under reduced pressure, the crystallization water of ammonium chloride and rare earth-iron-boron is successive
It is removed, to obtain the anhydrous rare-earth chlorination of high-purity.
Preferably, in the step S1, rare earth oxide can be completely dissolved by added water and hydrochloric acid just, be conducive to accelerate
Progress is evaporated in S3 and reduces energy consumption.
In the step S2, the purpose that ammonium chloride is added is to inhibit rare earth-iron-boron during subsequent evaporation and fried dry
Decomposition, the ratio between amount of substance of rare earth oxide and ammonium chloride is 1:(1-50), preferably 1:12.
Preferably, it in the step S3, after each fried dry, will be fried again after obtained solid mixture grind into powder state
It is dry, until no longer there is caking phenomenon in the solid of fried dry.
Preferably, heating described in step S4 is by the way of gradient increased temperature.
It preferably, is 0.5-15 DEG C/min from the heating rate, such as 5 DEG C/min.
Preferably, every 20-60 DEG C of heating keeps constant temperature 10-80min immediately, and such as every 30 DEG C of heating keeps constant temperature immediately
20min。
It is a discovery of the invention that gradient increased temperature is to 100 DEG C, ammonium chloride starts to decompose and re-forms ammonium chloride in temperature lower
Solid, it is preferred that longer heating time is kept between 100-250 DEG C, until ammonium chloride divides completely with rare earth-iron-boron
From.
Preferably, longer constant temperature time is kept, between 320-390 DEG C to guarantee that the rare earth-iron-boron crystallization water is removed completely
Go, for example, 390 DEG C holding constant temperature 1 hour.
Compared with prior art, the present invention has the advantage that
(1) with use rare earth-iron-boron as the invention of precursor compared with, rare earth oxide is cheap, advantageously reduces into
This；
(2) present invention first reacts rare earth oxide with hydrochloric acid solution, effectively prevents hydrogen chloride in subsequent operation
The introducing of gas simplifies operating process and improves safety；
(3) present invention is after rare earth oxide carries out reacting generation rare earth-iron-boron with hydrochloric acid solution, immediately to solution
Middle addition ammonium chloride, enable rare earth-iron-boron with ammonium chloride is more full and uniform mixes；
(4) the gradient increased temperature mode that the present invention uses, so that rare earth-iron-boron crude product is not needing repeatedly to shift sample
In the case of purified, avoid the adverse effect generated in sample transfer process；
(5) present invention, using the operation vacuumized, eliminates the interference of air, in ammonium chloride during gradient increased temperature
In the presence of inhibit the decomposition of rare earth-iron-boron, product purity is up to 99.9%.
Specific embodiment
Implementation of the invention is described in detail below, so that advantages and features of the invention are easier to by this field
Technical staff understands, but the present invention is not limited in scope of embodiments.
The rare earth element that this method is related to includes scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium
(Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu).This
The involved raw material of invention includes: rare earth oxide (Ln2O3), ammonium chloride (NH4Cl), hydrochloric acid.
Embodiment 1:
(1) 10g scandium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of scandium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved scandium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation, heating rate are 5 DEG C/min, temperature control method are as follows: 80 DEG C rise to 130 DEG C, keep 20min, then be warming up to 180 DEG C, protect
20min is held, then is warming up to 210 DEG C, keeps 50min, then be warming up to 240 DEG C, keeps 20min, then be warming up to 270 DEG C, is kept
20min, then 300 DEG C are warming up to, 20min is kept, then be warming up to 330 DEG C, keep 20min, then be warming up to 360 DEG C, kept
20min, then 390 DEG C are warming up to, 60min is kept, to obtain the anhydrous rare-earth chlorination of high-purity.
Embodiment 2:
(1) 10g yttrium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of yttrium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved yttrium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 3:
(1) 10g lanthana is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of lanthanum chloride is obtained；
(2) 70g ammonium chloride is added into dissolved lanthanum chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 4:
(1) 10g cerium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of cerium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved solution of cerium chloride by oxidation, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 5:
(1) 10g praseodymium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of praseodymium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved praseodymium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 6:
(1) 10g neodymia is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of neodymium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved neodymium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 7:
(1) 10g samarium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of samarium trichloride is obtained；
(2) 70g ammonium chloride is added into dissolved samarium trichloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 8:
(1) 10g europium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of Europium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved Europium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 9:
(1) 10g gadolinium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of scandium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved gadolinium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 10:
(1) 10g terbium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of terbium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved terbium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 11:
(1) 10g dysprosia is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of dysprosium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved dysprosium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 12:
(1) 10g holimium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of holmium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved holmium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 13:
(1) 10g erbium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of erbium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved erbium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 14:
(1) 10g thulium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of thulium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved thulium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 15:
(1) 10g ytterbium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of ytterbium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved ytterbium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Embodiment 16:
(1) 10g luteium oxide is put into crucible, adds 60mL water, hydrochloric acid is slowly added into crucible under agitation, directly
To being completely dissolved, the aqueous solution of lutecium chloride is obtained；
(2) 70g ammonium chloride is added into dissolved lutecium chloride solution, obtains the mixing of rare earth-iron-boron and ammonium chloride
Liquid；
(3) evaporation and fried dry, the solid for obtaining rare earth-iron-boron and ammonium chloride containing the crystallization water mix in a heated condition
Solid is transferred to grind into powder in mortar, is again transferred in crucible and carries out heating fried dry, so repeats to solid to exist by object
Until there is no caking phenomenon after heating in crucible；
(4) above-mentioned solid powder is transferred in sublimation apparatus, is heated by the way of gradient increased temperature and is persistently subtracted
Press operation.
Only several embodiments of the present invention are expressed for example described above, and what is described is more specific and detailed, but simultaneously
It cannot be therefore understands that being all scope limitations of this patent.It should be pointed out that for those of ordinary skill in the art,
Under the premise of not departing from present inventive concept, various modifications and improvements can be made, and these are all within the scope of protection of the present invention.
Therefore, the protection content of the invention patent should be determined by the appended claims.
Claims (6)
1. a kind of preparation method of anhydrous rare-earth chlorination, which is characterized in that comprising steps of
S1, rare earth oxide is dissolved using hydrochloric acid, obtains the aqueous solution of rare earth-iron-boron；
S2, ammonium chloride is added into dissolved rare-earth chloride solution, obtains the mixed liquor of rare earth-iron-boron and ammonium chloride；
S3, in a heated condition evaporation and fried dry, obtain the solid mixture of rare earth-iron-boron and ammonium chloride containing the crystallization water；
S4, the solid mixture after above-mentioned fried dry is transferred in sublimation apparatus, is risen to by the way of gradient increased temperature from 80 DEG C
390 DEG C, while vacuum pumping is carried out, in vacuumizing heating process, the crystallization water of ammonium chloride and rare earth-iron-boron is successive
It is removed, to obtain the anhydrous rare-earth chlorination of high-purity.
2. a kind of preparation method of anhydrous rare-earth chlorination according to claim 1, which is characterized in that first to rare-earth oxidation
A small amount of water is added in object, is slow added into concentrated hydrochloric acid and is dissolved；Or first dilute concentrated hydrochloric acid, it is used further to dissolution rare-earth oxidation
Object；Rare earth oxide can be completely dissolved by added water and hydrochloric acid just.
3. a kind of preparation method of anhydrous rare-earth chlorination according to claim 1, which is characterized in that the rare-earth oxidation
The ratio between amount of substance of object and ammonium chloride is 1:(1-50).
4. a kind of preparation method of anhydrous rare-earth chlorination according to claim 1, which is characterized in that the rare-earth oxidation
The ratio between amount of substance of object and ammonium chloride is 1:12.
5. a kind of preparation method of anhydrous rare-earth chlorination according to claim 1, which is characterized in that heating side described in S4
Formula is gradient increased temperature；It is 0.5-15 DEG C/min from the heating rate；Every 20-60 DEG C of heating keeps constant temperature 10- immediately
80min keeps longer heating time between 100-250 DEG C, until ammonium chloride is kept completely separate with rare earth-iron-boron.
6. a kind of a kind of preparation method of anhydrous rare-earth chlorination as described in claim 1, which is characterized in that products therefrom without
Water rare earth-iron-boron is for catalyst, cosolvent or prepares purposes in the metallo-organic compound of rare earth.
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| CN112010339A (en) * | 2020-09-04 | 2020-12-01 | 内蒙古蒙稀新材料有限责任公司 | Preparation method of high-purity anhydrous rare earth chloride |
| CN113072090A (en) * | 2021-04-23 | 2021-07-06 | 中国恩菲工程技术有限公司 | Preparation method of anhydrous scandium chloride molten salt |
| CN113772714A (en) * | 2021-10-18 | 2021-12-10 | 天津包钢稀土研究院有限责任公司 | Anhydrous samarium chloride and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112010339A (en) * | 2020-09-04 | 2020-12-01 | 内蒙古蒙稀新材料有限责任公司 | Preparation method of high-purity anhydrous rare earth chloride |
| CN112010339B (en) * | 2020-09-04 | 2021-06-18 | 内蒙古蒙稀新材料有限责任公司 | Preparation method of high-purity anhydrous rare earth chloride |
| CN113072090A (en) * | 2021-04-23 | 2021-07-06 | 中国恩菲工程技术有限公司 | Preparation method of anhydrous scandium chloride molten salt |
| CN113772714A (en) * | 2021-10-18 | 2021-12-10 | 天津包钢稀土研究院有限责任公司 | Anhydrous samarium chloride and preparation method thereof |
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