CN107827139A - The preparation method of anhydrous praseodymium chloride - Google Patents
The preparation method of anhydrous praseodymium chloride Download PDFInfo
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- CN107827139A CN107827139A CN201710818303.8A CN201710818303A CN107827139A CN 107827139 A CN107827139 A CN 107827139A CN 201710818303 A CN201710818303 A CN 201710818303A CN 107827139 A CN107827139 A CN 107827139A
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2006/82—Compositional purity water content
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Abstract
The invention discloses a kind of preparation method of anhydrous praseodymium chloride, including step：S1, seven water praseodymium chlorides are carried out to one section of fluidisation dehydration at 60 DEG C~100 DEG C, obtain three water praseodymium chloride crude products；S2, three water praseodymium chloride crude products are carried out to two sections of fluidisation dehydrations at 120 DEG C~130 DEG C, obtain a water praseodymium chloride crude product；S3, a water praseodymium chloride crude product is carried out to three sections of fluidisation dehydrations at 140 DEG C~160 DEG C, obtain anhydrous praseodymium chloride；Wherein, three sections of fluidisation dehydrations are carried out in hydrogen chloride gas atmosphere.According to the preparation method of the anhydrous praseodymium chloride of the present invention; by the way that seven water praseodymium chlorides are carried out into segmentation fluidisation dehydration; and hydrogen chloride protective gas atmosphere is provided, so as to effectively inhibit the water praseodymium chloride of intermediate product one, to the hydrolysis during anhydrous praseodymium chloride, to substantially increase product purity in dehydration；And the preparation method dehydration temperaturre of the anhydrous praseodymium chloride is low, preparation cost is low, and dehydrating effect is good.
Description
Technical field
The invention belongs to technical field of rare earth material preparation, it relates in particular to which one kind is using seven water praseodymium chlorides as raw material
The method for preparing anhydrous praseodymium chloride.
Background technology
Rare earth element is the element for having 21 century strategic position, special by physical chemistry such as its unique light, electricity, magnetic
Property, and it is widely used in national economy and the every field of national defense industry, therefore, rare earth element is referred to as " 21 century new material
Treasure-house ".In recent years, rare earth element be even more due to its important bioactivity and pharmacotoxicological effect, and increasingly by
The concern of people.
Preparing the method for anhydrous rare earth chloride at present has following 4 kinds：(1) tetrahydrofuran complex method, i.e. Deacon in
The method for preparing anhydrous rare earth chloride by metal exchange reaction in THF solution of development in 1979, this method is from rare earth
Metal sets out, through being reacted with mercury chloride, the method for preparing the THF complexs of anhydrous rare-earth chlorination；(2) crystallization water and rare earth
The decompression dehydration method of chloride, i.e., after hydrometallurgy be made re chloride, then be concentrated under reduced pressure, crystallisation by cooling, people
Aqueous crystallization rare earth chloride, obtains anhydrous rare earth chloride after vacuum dehydration made from the processes such as work is broken；(3) ammonium chloride
Sublimed method, it is to convert at 300 DEG C~450 DEG C rare earth oxide with ammonium chloride, rare earth oxide is converted into rare earth chloride；With
And (4) rare earth oxide chloridising.But the drawbacks of larger is but individually present in above-mentioned preparation method, wherein, tetrahydrofuran is matched somebody with somebody
Compound method introduces tetrahydrofuran, by-product noxious material such as HgCl in process of production2Deng seriously polluting environment, subsequent treatment
Process is difficult, and this method initiation material needs the rare earth metal of high-purity, is not suitable for preparing on a large scale；The crystallization water
Bad with the decompression dehydration method dehydrating effect of rare earth-iron-boron, product purity is not high；Ammonium chloride sublimed method prepares rare earth chloride mistake
Cheng Zhong, if in rare earth in the presence of+4 valency rare earth elements in the presence of, such as CeO2If it is dilute to prepare anhydrous chlorination with ammonium chloride sublimed method
Soil, the generation of redox reaction is had in course of reaction, it is difficult to which the higher anhydrous rare earth chloride of purity is made；And rare earth oxygen
3%~58% Re is typically contained in anhydrous rare earth chloride prepared by compound chloridising2O, 5%~10% water and 5%~
10% contains water-insoluble, and this method product is unstable, and chlorination temperature is up to 1050 DEG C~1100 DEG C, chlorination process chlorine
Gas is serious to equipment corrosion at high temperature.
Anhydrous praseodymium chloride is the basic agent for preparing rear earth containing organic compound, can play and urge in petroleum refining
Change acts on, meanwhile, it can be used to smelt the important source material of rare earth metal, rare earth alloy, and produce the primary raw material of polishing powder.
As one kind in rare earth element, the preparation of high-purity anhydrous praseodymium chloride has certain difficulty.Therefore, it is necessary to explore one kind
The preparation method for the anhydrous praseodymium chloride that technique is simple and dewatering efficiency is high, product purity is high.
The content of the invention
, should the invention provides a kind of preparation method of anhydrous praseodymium chloride to solve the above-mentioned problems of the prior art
Preparation method is simple for process, dewatering efficiency is high, preparation temperature is low, the problem of alleviating equipment corrosion, while environmental pollution
It is small, and the anhydrous praseodymium chloride purity prepared is high.
In order to reach foregoing invention purpose, present invention employs following technical scheme：
A kind of preparation method of anhydrous praseodymium chloride, including step：
S1, seven water praseodymium chlorides are carried out to one section of fluidisation dehydration at 60 DEG C~100 DEG C, obtain three water praseodymium chloride crude products；
S2, the three water praseodymium chloride crude product is carried out to two sections of fluidisation dehydrations at 120 DEG C~130 DEG C, obtain a water chlorination
Praseodymium crude product；
S3, the water praseodymium chloride crude product is carried out to three sections of fluidisation dehydrations at 140 DEG C~160 DEG C, obtain anhydrous chlorination
Praseodymium；
Wherein, three sections of fluidisations dehydration is carried out in hydrogen chloride gas atmosphere.
Further, two sections of fluidisations dehydration is carried out in hydrogen chloride gas atmosphere.
Further, one section of fluidisation dehydration is carried out in hydrogen chloride gas atmosphere.
Further, by controlling air blast speed to make one section of fluidisation dehydration, two in the step S1~S3
Duan Liuhua, which is dehydrated, and three sections of fluidisation dehydrations are steady is carried out.
Further, it is described one section fluidisation dehydration, two sections fluidisation dehydration and three sections fluidisation dehydration air blast speed according to
Secondary reduction.
Further, in the step S1, the seven water praseodymium chloride leading powder before one section of fluidisation dehydration is carried out
It is broken.
Further, after the step S3, by tail gas recycle and for providing hydrogen chloride gas atmosphere.
The present invention provides hydrogen chloride protective gas atmosphere by the way that seven water praseodymium chlorides are carried out into segmentation fluidisation dehydration, so as to
The water praseodymium chloride of intermediate product one is effectively inhibited, to the hydrolysis during anhydrous praseodymium chloride, to substantially increase production in dehydration
Product purity；And the preparation method dehydration temperaturre of the anhydrous praseodymium chloride is low, preparation cost is low, and dehydrating effect is good.Compared to existing skill
Anhydrous praseodymium chloride is typically prepared method in art, and preparation in accordance with the present invention is not related to high-temperature oxidation process, operation letter
Single, relatively low to equipment requirement, the problem of alleviating equipment corrosion, simultaneously reduces environmental pollution.
Brief description of the drawings
The following description carried out in conjunction with the accompanying drawings, above and other aspect, feature and the advantage of embodiments of the invention
It will become clearer, in accompanying drawing：
Fig. 1 is the structural representation according to the fluidisation dehydration device of the present invention；
Fig. 2 is the step flow chart according to the preparation method of the anhydrous praseodymium chloride of the present invention.
Embodiment
Hereinafter, with reference to the accompanying drawings to embodiments of the invention are described in detail.However, it is possible to come in many different forms
Implement the present invention, and the specific embodiment of the invention that should not be construed as limited to illustrate here.Conversely, there is provided these
Embodiment be in order to explain the present invention principle and its practical application so that others skilled in the art it will be appreciated that
Various embodiments of the present invention and the various modifications for being suitable for specific intended application.In the accompanying drawings, for the sake of clarity, can be with
Exaggerate the shape and size of element, and identical label will be used to indicate same or analogous element all the time.
The invention provides a kind of preparation method of anhydrous praseodymium chloride, the preparation method is using seven water praseodymium chlorides as raw material, tool
Body carries out segmentation fluidisation dehydration under hydrogen chloride protective atmosphere, you can simply and efficiently obtains the nothing that purity is high, dehydrating effect is good
Water praseodymium chloride.
What deserves to be explained is it is based on a kind of stream with three Room according to the preparation method of the anhydrous praseodymium chloride of the present invention
Change what dehydration device was carried out.
It will be appreciated that although can be used term " first ", " second " etc. to describe various elements herein, but this
A little elements should not be limited by these terms.These terms are only used for making a distinction an element with another element.
Referring in particular to Fig. 1, the fluidisation dehydration device includes being sequentially connected logical first class room 11, the second fluidising chamber 12
And the 3rd fluidising chamber 13；The wherein top of first class room 11 is communicated with raw material feed bin 21, to store dehydrated raw material (this Shen
Please in refer specifically to seven water praseodymium chlorides) and feed into first class room 11；Meanwhile the bottom of the 3rd fluidising chamber 13 is communicated with product
Feed bin 22, to store dehydration product (anhydrous praseodymium chloride is referred specifically in the application).First class room 11, the second fluidising chamber 12
And the 3rd the bottom of fluidising chamber 13 be connected to primary heater 31, the heater 33 of secondary heater 32 and the 3rd, to
Three fluidising chamber are heated respectively；Meanwhile first class room 11, the second fluidising chamber 12 and the 3rd fluidising chamber 13 also divide
Air blower 44 is not connected to by the first breather valve 41, the second breather valve 42 and three-way air valve 43, to be flowed to three
Change room and be passed through air blast, to realize the fluidisation dehydration in three fluidising chamber with reference to heating operation.
In order to better control over charging rate, be typically additionally provided between raw material feed bin 21 and first class room 11 into
Glassware 51；Need to carry out crushing operation before fluidisation is dehydrated based on some dehydrated raw materials, therefore, feeder 51 is preferably spiral shell
Precession glassware, in this way, the pulverization process of dehydrated raw material is completed while charging, to prevent the dehydrated raw material of agglomerate body
The problem of fluidisation dehydration is insufficient in fluidising chamber.
Meanwhile generally, due to fluidizing needs progress air blast that material to be drained off " blowing afloat " is made into its suspension in dehydration
In fluidising chamber, therefore the unavoidable dust that produces can influence to fluidize dewater treatment, it is therefore preferable that also connecting in the 3rd fluidising chamber 13
It is connected to cyclone dust collectors 52；Two connected rotations are preferably employed in fluidisation dehydration device used in embodiments of the invention
Wind deduster 52.
In the above-mentioned fluidisation dehydration device of the present invention, it is interconnected between each part by pipeline, not shown in figure,
Only represented with overstriking lines.
The preparation method of the anhydrous praseodymium chloride of the present invention is described in detail below in conjunction with Fig. 2, according to the present invention's
The preparation method of anhydrous praseodymium chloride comprises the steps：
Step S1, seven water praseodymium chlorides are carried out to one section of fluidisation dehydration at 60 DEG C~100 DEG C, it is thick to obtain three water praseodymium chlorides
Product.
Specifically, seven water praseodymium chlorides are initially stored in raw material feed bin 21, then feed seven water praseodymium chlorides to first
In fluidising chamber 11, and first class room 11 is heated using primary heater 31, meanwhile, the first breather valve 41 control drum
The air blast speed that blower fan 44 leads in first class room 11, so that seven water praseodymium chlorides are put down in first class room 11
One section of steady fluidisation dehydration, and generate three water praseodymium chloride crude products；As shown in Equation 1：
PrCl3·7H2O→PrCl3·3H2O+4H2O (g) formulas 1.
Significantly, since seven water praseodymium chlorides are easily tied admittedly blocking, therefore, then fed to first class room
, it is necessary to be crushed in advance before 11；Preferably, you can fed by the feeding screw being connected with raw material feed bin 21, such as
This, that is, effectively prevent the caking phenomenon of seven water praseodymium chlorides；Meanwhile the working frequency of feeding screw have impact on charging speed
Degree.
Step S2, three water praseodymium chloride crude products are carried out to two sections of fluidisation dehydrations at 120 DEG C~130 DEG C, obtain a water chlorination
Praseodymium crude product.
Specifically, the three water praseodymium chloride crude products obtained in first class room 11 mainly move in the presence of air blast
Moving into the second fluidising chamber 12, secondary heater 32 heats to the second fluidising chamber 12, meanwhile, the second breather valve 42 controls
The air blast speed that air blower 44 leads in the second fluidising chamber 12, so that three water praseodymium chlorides are carried out in the second fluidising chamber 12
Stable two sections of fluidisations dehydration, and generate a water praseodymium chloride crude product；As shown in Equation 2：
PrCl3·3H2O→PrCl3·H2O+2H2O (g) formulas 2.
Step S3, one water praseodymium chloride crude product is carried out to three sections of fluidisation dehydrations at 140 DEG C~160 DEG C, obtain anhydrous chlorination
Praseodymium.
Specifically, the water praseodymium chloride crude product obtained in the second fluidising chamber 12 mainly moves in the presence of air blast
Moving into the 3rd fluidising chamber 13, the 3rd heater 33 heats to the 3rd fluidising chamber 13, meanwhile, three-way air valve 43 controls
The air blast speed that air blower 44 leads in the 3rd fluidising chamber 13, so that a water praseodymium chloride is carried out in the 3rd fluidising chamber 13
Stable three sections of fluidisations dehydration, and control three sections of fluidisation dehydrations to be carried out in hydrogen chloride gas atmosphere, obtain anhydrous chlorination
Praseodymium；As shown in Equation 3：
PrCl3·H2O→PrCl3+H2O (g) formulas 3.
The anhydrous praseodymium chloride product obtained is finally transferred in the product feed bin being connected with the 3rd fluidising chamber.
Simultaneously as during above-mentioned formula 3 is carried out, employ hydrogen chloride atmosphere and protected, so as to effectively suppress
The hydrolysis of formula 4：
PrCl3·H2O → PrOCl+2HCl (g) formulas 4.
Preferably, hydrogen chloride gas atmosphere is provided for convenience, in the lump can be passed through hydrogen chloride gas by air blower 44
Into the 3rd fluidising chamber 13, it is therefore preferable that two sections of fluidisation dehydrations and one section of fluidisation dehydration are also entered in hydrogen chloride gas atmosphere
OK, so that the gas passage that air blower 44 connects is the air of rich hydrogen chloride gas.
Further, after the completion of preparation, the tail gas recycle in each fluidising chamber will be full of and recycled, for carrying
For hydrogen chloride gas atmosphere.
What deserves to be explained is because the raw material in first class room 11 has the more crystallization water, therefore its proportion is more
Greatly, in order to obtain stable fluidisation dehydration, it is therefore desirable to bigger air blast speed is provided, by seven water praseodymium chlorides
" blowing afloat "；It is therefore, corresponding to need and the crystallization water of the second fluidising chamber 12 and the reactant in the 3rd fluidising chamber 13 gradually reduces
The air blast speed wanted is also corresponding gradually to be reduced；That is, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three sections of fluidisations
The air blast speed of dehydration is sequentially reduced.
In addition, fluidisation dewatering time is influenceed by air blast speed, and air blast speed is by the shadow of charging rate
Ring；Charging rate is not provided specifically in the preparation method of the application, it is only necessary to according to the specific of fluidisation dehydration device
Scale is specifically chosen, and adjusts air blast speed and fluidisation dewatering time, makes smoothly to be flowed in different fluidising chamber
Change dehydration, and mainly obtain target product.
In this way, realize seven water by being segmented fluidisation evaporation and combining the effect of hydrogen chloride protective gas atmosphere
The complete dehydration of praseodymium chloride, obtains anhydrous praseodymium chloride；Wherein, hydrogen chloride protective gas atmosphere effectively inhibits intermediate product
One water praseodymium chloride, to the hydrolysis during anhydrous praseodymium chloride, substantially increases product purity in dehydration；And the anhydrous chlorine
It is low to change the preparation method dehydration temperaturre of praseodymium, preparation cost is low, and dehydrating effect is good.
Detailed retouch will be carried out to the preparation method of the above-mentioned anhydrous praseodymium chloride of the present invention by specific embodiment below
State.
Embodiment 1
In embodiment 1, it is 100kg/h to control charging rate, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three sections
The temperature of fluidisation dehydration is respectively 70 DEG C, 120 DEG C and 140 DEG C, meanwhile, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three
The time of Duan Liuhua dehydrations is 20min, is finally obtained anhydrous praseodymium chloride product.
The anhydrous praseodymium chloride product obtained to the present embodiment is analyzed, and wherein water insoluble matter content is 7.0%
(wt%)；It is 7.0% (wt%) to detect wherein moisture by karl Fischer moisture teller；Meanwhile can through XRD analysis
Know, product principal component is anhydrous praseodymium chloride.
Embodiment 2
In example 2, it is 100kg/h to control charging rate, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three sections
The temperature of fluidisation dehydration is respectively 80 DEG C, 130 DEG C and 140 DEG C, meanwhile, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three
The time of Duan Liuhua dehydrations is 20min, is finally obtained anhydrous praseodymium chloride product.
The anhydrous praseodymium chloride product obtained to the present embodiment is analyzed, and wherein water insoluble matter content is 4.0%
(wt%)；It is 4.0% (wt%) to detect wherein moisture by karl Fischer moisture teller；Meanwhile can through XRD analysis
Know, product principal component is anhydrous praseodymium chloride.
Embodiment 3
In embodiment 3, it is 100kg/h to control charging rate, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three sections
The temperature of fluidisation dehydration is respectively 90 DEG C, 120 DEG C and 150 DEG C, meanwhile, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three
The time of Duan Liuhua dehydrations is 20min, is finally obtained anhydrous praseodymium chloride product.
The anhydrous praseodymium chloride product obtained to the present embodiment is analyzed, and wherein water insoluble matter content is 5.0%
(wt%)；It is 10.0% (wt%) to detect wherein moisture by karl Fischer moisture teller；Meanwhile can through XRD analysis
Know, product principal component is anhydrous praseodymium chloride.
Embodiment 4
In example 4, it is 100kg/h to control charging rate, one section of fluidisation dehydration, two sections of fluidisation dehydrations and three sections
Fluidisation dehydration temperature be respectively 100 DEG C, 120 DEG C and 145 DEG C, meanwhile, one section fluidisation dehydration, two sections fluidisation dehydration and
The time of three sections of fluidisation dehydrations is 20min, is finally obtained anhydrous praseodymium chloride product.
The anhydrous praseodymium chloride product obtained to the present embodiment is analyzed, and wherein water insoluble matter content is 3.0%
(wt%)；It is 5.0% (wt%) to detect wherein moisture by karl Fischer moisture teller；Meanwhile can through XRD analysis
Know, product principal component is anhydrous praseodymium chloride.
It can be seen from above-described embodiment that according to the preparation method of the anhydrous praseodymium chloride of the present invention, the nothing finally obtained
Moisture is typically not over 10% in water praseodymium chloride product, or even can reach 5% or so so low level；This
The anhydrous neodymium chloride major impurity that one product performance is typically prepared acquisition more in the prior art is water, and content is relatively low, existing skill
Rare earth oxide, impurity calcium, barium, iron etc. are typically contained in the product that rare earth oxide chloridising obtains in art, impurity content is higher,
Chlorination temperature is high generally 950 DEG C~1050 DEG C, and this also illustrates the dehydration of the preparation method of the anhydrous praseodymium chloride according to the present invention
Effect is good.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, form can be carried out herein
With the various change in details.
Claims (7)
1. a kind of preparation method of anhydrous praseodymium chloride, it is characterised in that including step：
S1, seven water praseodymium chlorides are carried out to one section of fluidisation dehydration at 60 DEG C~100 DEG C, obtain three water praseodymium chloride crude products；
S2, the three water praseodymium chloride crude product is carried out to two sections of fluidisation dehydrations at 120 DEG C~130 DEG C, it is thick to obtain a water praseodymium chloride
Product；
S3, the water praseodymium chloride crude product is carried out to three sections of fluidisation dehydrations at 140 DEG C~160 DEG C, obtain anhydrous praseodymium chloride；
Wherein, three sections of fluidisations dehydration is carried out in hydrogen chloride gas atmosphere.
2. preparation method according to claim 1, it is characterised in that two sections of fluidisations dehydration is in hydrogen chloride gas atmosphere
Interior progress.
3. preparation method according to claim 2, it is characterised in that one section of fluidisation dehydration is in hydrogen chloride gas atmosphere
Interior progress.
4. according to any described preparation methods of claim 1-3, it is characterised in that pass through control in the step S1~S3
Air blast speed is dehydrated one section of fluidisation, two sections of fluidisation dehydrations and three sections of fluidisation dehydrations are steadily carried out.
5. preparation method according to claim 4, it is characterised in that it is described one section fluidisation dehydration, two sections fluidisation dehydration and
The air blast speed of three sections of fluidisation dehydrations is sequentially reduced.
6. preparation method according to claim 1, it is characterised in that in the step S1, the seven water praseodymium chloride exists
Crushed in advance before one section of fluidisation dehydration.
7. according to any described preparation methods of claim 1-3, it is characterised in that after the step S3, by tail gas recycle simultaneously
For providing hydrogen chloride gas atmosphere.
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Cited By (1)
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| CN108298573A (en) * | 2018-04-13 | 2018-07-20 | 上海泰坦科技股份有限公司 | A kind of preparation method of anhydrous yttrium chloride |
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Application publication date: 20180323 |