CN112499661A - Preparation method of flaky chlorinated rare earth - Google Patents
Preparation method of flaky chlorinated rare earth Download PDFInfo
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- CN112499661A CN112499661A CN202011516055.XA CN202011516055A CN112499661A CN 112499661 A CN112499661 A CN 112499661A CN 202011516055 A CN202011516055 A CN 202011516055A CN 112499661 A CN112499661 A CN 112499661A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 195
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- -1 rare earth chloride Chemical class 0.000 claims abstract description 148
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 34
- 239000010959 steel Substances 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 21
- 238000005303 weighing Methods 0.000 claims description 18
- 238000002425 crystallisation Methods 0.000 claims description 17
- 230000008025 crystallization Effects 0.000 claims description 17
- 239000012809 cooling fluid Substances 0.000 claims description 14
- 238000004806 packaging method and process Methods 0.000 claims description 11
- 239000000428 dust Substances 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000005507 spraying Methods 0.000 description 13
- 230000008020 evaporation Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 6
- 238000007738 vacuum evaporation Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000001788 irregular Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a preparation method of flaky chlorinated rare earth, which is realized by a preparation system of flaky chlorinated rare earth, wherein the preparation system comprises a melting unit, a continuous discharging unit, a conveying unit and a crushing unit which are sequentially connected, and the preparation method comprises the following steps: 1) putting the rare earth chloride solution into a melting unit, evaporating and concentrating to form molten rare earth chloride, and sending the molten rare earth chloride to an analysis unit to detect that the content of rare earth oxide in the rare earth chloride is 42-48%; 2) the molten rare earth chloride is conveyed to the conveying unit through the continuous discharging unit, and is cooled to below 40 ℃ on the conveying unit, so that the rare earth chloride is cooled and crystallized; 3) and conveying the cooled and crystallized rare earth chloride into the crushing unit for crushing to obtain flaky rare earth chloride. According to the method, through the preparation system of the flaky rare earth chloride, the labor intensity of workers can be reduced, and the production efficiency can be improved.
Description
Technical Field
The invention relates to the technical field of preparation of rare earth chloride, in particular to a preparation method of flaky rare earth chloride.
Background
The rare earth chloride is prepared by taking rare earth ore as a raw material through a chemical method or an extraction method, can be used as a raw material for preparing rare earth compounds, petroleum cracking catalysts, polishing powder, rare earth concentrates and the like, and is widely applied to the fields of chemical industry, light textile, agriculture and the like. In the application process of the rare earth chloride, large blocks of solid rare earth chloride are generally required to be prepared into rare earth chloride with smaller volume.
In the prior art, rare earth chloride is generally heated and concentrated to be molten, the molten rare earth chloride flows into a crystallization tank to be naturally cooled and crystallized by cooling, and the area of a crystal is approximately equal to that of the crystallization tank (30-500 m)2) However, the cooling crystallization time is long (about 8-24h), the thickness of the crystallized rare earth chloride is usually 100-200mm, the crushed rare earth chloride needs to be crushed manually, the size of the crushed rare earth chloride is large, the shape of the crushed rare earth chloride is irregular, and the labor intensity of subsequent manual weighing and packaging is high, thereby causing low production efficiency.
Disclosure of Invention
The invention aims to provide a preparation method of flaky rare earth chloride, which aims to solve the problems of high labor intensity of workers and low production efficiency caused by large volume and irregular shape of crystallized rare earth chloride due to natural crystallization in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of flaky chlorinated rare earth, which is realized by a preparation system of flaky chlorinated rare earth, wherein the preparation system comprises a melting unit, a continuous discharging unit, a conveying unit and a crushing unit which are sequentially connected, and the preparation method comprises the following steps:
1) putting the rare earth chloride solution into a melting unit, evaporating and concentrating to form molten rare earth chloride, wherein the content of rare earth oxide in the rare earth chloride is 42-48%;
2) the molten rare earth chloride is conveyed to the conveying unit through the continuous discharging unit, and is cooled to below 40 ℃ on the conveying unit, so that the rare earth chloride is cooled and crystallized;
3) and conveying the cooled and crystallized rare earth chloride into the crushing unit for crushing to obtain flaky rare earth chloride.
In some embodiments of the invention, the flaky rare earth chloride has a thickness of 2 to 15mm and a length and width of less than 50 mm.
In some embodiments of the present invention, the conveying unit comprises a steel belt and a driving member for driving the steel belt to run, wherein the running speed of the steel belt is 2-10 m/min.
In some embodiments of the present invention, the steel strip has a first surface and a second surface opposite to the first surface, wherein the first surface is used for supporting the molten rare earth chloride, and the second surface is used for contacting with a cooling fluid to reduce the temperature of the molten rare earth chloride to below 40 ℃.
In some embodiments of the invention, the flow rate of the cooling fluid is 20 to 60m3/h。
In some embodiments of the invention, the molten rare earth chloride is spread on the first surface of the steel strip, and the thickness of the layer of rare earth chloride spread on the first surface is 2-15 mm.
In some embodiments of the invention, the preparation system further comprises a heat dissipation unit and a dust collection unit disposed above the conveying unit.
In some embodiments of the invention, the cooling crystallization time is from 10 to 30 min.
In some embodiments of the invention, the preparation system further comprises a weighing unit in communication with the crushing unit and a packaging unit connected to the weighing unit.
In some embodiments of the invention, in step 1), the molten rare earth chloride can be stored in an environment above 125 ℃ and maintained in a molten state.
The embodiment provided by the invention has at least the following beneficial effects:
according to the preparation method of the flaky chlorinated rare earth, provided by the invention, through a preparation system of the flaky chlorinated rare earth, a chlorinated rare earth solution is put into a melting unit to be evaporated and concentrated to form molten chlorinated rare earth, and the content of Rare Earth Oxide (REO) in the chlorinated rare earth is 42-48%, so that the REO content in the subsequently obtained flaky chlorinated rare earth is ensured to be more than 45%, namely the preparation method meets the standard requirement of mixed chlorinated rare earth products (GB/T4148-2015). In addition, the molten rare earth chloride is conveyed to the conveying unit through the continuous discharging unit and cooled to the temperature below 40 ℃ for crystallization, so that the crystallized rare earth chloride is easy to break to form flaky rare earth chloride, the operation can be completed without the participation of workers, the labor intensity of the workers can be reduced, and the production efficiency can be improved.
In addition to the technical problems solved by the present invention, the technical features constituting the technical solutions, and the advantageous effects brought by the technical features of the technical solutions, other technical problems solved by the method for preparing a flaky rare earth chloride according to the present invention, other technical features included in the technical solutions, and advantageous effects brought by the technical features will be described in further detail in the detailed description of the embodiments.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart showing a method for producing a flaky rare earth chloride of the present invention;
FIG. 2 is a flow chart showing a production system used in the production method of a flaky rare earth chloride of the present invention.
Detailed Description
The technical solutions in the examples of the present disclosure will be clearly and completely described below in connection with the specific embodiments of the present disclosure, and it is obvious that the described embodiments and/or examples are only a part of the embodiments and/or examples of the present disclosure, and not all embodiments and/or examples. All other embodiments and/or all other examples that can be obtained by one of ordinary skill in the art without making any inventive step based on the embodiments and/or examples in the present disclosure are within the scope of the present disclosure.
In the description of the present specification, the term "comprising", "including" or "containing" means that it may have, in addition to the components, other components which impart different properties to the heavy metal stabilizing chelating agent. In addition, the terms "comprising," including, "or" containing "as used in this disclosure may also include" consisting essentially of, and may instead be "or" consisting of.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
In the description of the present specification, amounts, ratios, and the like are by weight unless otherwise specified.
In the description of the present specification, reference to the description of the terms "one embodiment", "some embodiments", "an illustrative embodiment", "an example", "a specific example", or "some examples", etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The invention provides a preparation method of flaky chlorinated rare earth, which is realized by a preparation system of flaky chlorinated rare earth, wherein the preparation system comprises a melting unit, a continuous discharging unit, a conveying unit and a crushing unit which are sequentially connected, and the preparation method of flaky chlorinated rare earth comprises the following steps:
1) putting the rare earth chloride solution into a melting unit, evaporating and concentrating to form molten rare earth chloride, wherein the content of rare earth oxide in the rare earth chloride is 42-48%;
2) the molten rare earth chloride is conveyed to the conveying unit through the continuous discharging unit, and the temperature of the molten rare earth chloride is reduced to be below 40 ℃ on the conveying unit, so that the rare earth chloride is cooled and crystallized;
3) and conveying the cooled and crystallized rare earth chloride into a crushing unit for crushing to obtain flaky rare earth chloride.
As mentioned above, in the embodiment of the present invention, the content of REO in the chlorinated rare earth solution is 100g/L-400g/L, and the content of REO in the chlorinated rare earth solution can be, but is not limited to, 100g/L, 101g/L, 102g/L, 103g/L, 104g/L, 105g/L, 106g/L, 107g/L, 108g/L, 109g/L, 110g/L, 111g/L, 112g/L, 113g/L, 114g/L, 115g/L, 116g/L, 117g/L, 118g/L, 119g/L or 120g/L-180g/L, 181g/L, 182g/L, 183g/L, 184g/L, 185g/L, 186g/L, 187g/L, 188g/L, 189g/L, 190g/L, 191g/L, 192g/L, 193g/L, 194g/L, 195g/L, 196g/L, 197g/L, 198g/L, 199g/L, 200g/L, 201g/L, 202g/L, 203g/L, 204g/L, 205g/L, 206g/L, 207g/L, 208g/L, 209g/L, 210g/L, 211g/L, 212g/L, 213g/L, 214g/L, 215g/L, 216g/L, 217g/L, 218g/L, 219g/L, 220g/L, 221g/L, 222g/L, 223g/L, 224g/L, 225g/L, 226g/L, 227g/L, 228g/L, 229g/L or 230g/L-260g/L, 261g/L, 262g/L, 263g/L, 264g/L, 265g/L, 267g/L, 268g/L, 269g/L, 270g/L, 271g/L, 272g/L, 273g/L, 274g/L, 275g/L, 276g/L, 277g/L, 278g/L, 279g/L, 280g/L, 281g/L282g/L, 283g/L, 284g/L, 285g/L or 285g/L-400 g/L. The rare earth chloride solution is put into a smelting unit to form molten rare earth chloride through evaporation and concentration, the REO content in the rare earth chloride is 42-48%, and the REO content in the subsequently obtained flaky rare earth chloride is more than 45%, namely the rare earth chloride meets the standard requirement of the product of mixed rare earth chloride (GB/T4148-2015).
In some embodiments of the invention, the smelting unit comprises an evaporation concentration tank, and the rare earth chloride solution is transferred into the evaporation concentration tank and then evaporated and concentrated by reduced pressure and vacuum to form molten rare earth chloride.
Further, in some embodiments of the present invention, the smelting unit further includes a storage tank, the storage tank is communicated with the bottom of the evaporation concentration tank, so that the molten rare earth chloride can be stored in the storage tank, and the temperature in the storage tank needs to be greater than 125 ℃ to maintain the molten rare earth chloride, so that the processing amount of the rare earth chloride can be increased through the storage tank, and the production efficiency can be further increased.
In addition, in the process of carrying out vacuum concentration and storage on the rare earth chloride solution under reduced pressure, the generated steam can be used for recovering condensed water through a gas-liquid separator, and the condensed water can be used as cooling fluid for subsequent cooling crystallization of the rare earth chloride, so that the use amount of the cooling fluid can be reduced, and the purpose of reducing the preparation cost of the flaky rare earth chloride is achieved.
In some embodiments of the present invention, the continuous discharging unit in the preparation system is a belt distributor, the belt distributor can continuously convey the molten rare earth chloride to the conveying unit, and the conveyed molten rare earth chloride is uniformly distributed on the conveying unit, so that the temperature reduction of the molten rare earth chloride can be accelerated, and the time for cooling and crystallizing can be shortened. In addition, the belt distributor can treat rare earth chloride products with the amount of 50t per day, which is far higher than that treated by the prior art.
In some embodiments of the present invention, the conveying unit comprises a steel belt and a driving member for driving the steel belt to run, wherein the steel belt is a conveying steel belt known to those skilled in the art, and the driving member is any driving device known to those skilled in the art, such as a motor and the like. The length of the above-mentioned steel strip can be generally 10-80m, and the specific length can be determined according to the weight of the rare earth chloride actually treated.
Further, a conventional steel strip generally has a first surface and a second surface opposite to the first surface, wherein the first surface is used for bearing the molten rare earth chloride, and the second surface is used for contacting with a cooling fluid to reduce the temperature of the molten rare earth chloride to below 40 ℃.
Specifically, the cooling fluid can be sprayed on the second surface of the steel strip in a spraying manner, and the sprayed cooling fluid can be recycled after being cooled, so that the preparation cost of the flaky rare earth chloride is further reduced.
It will be appreciated that the cooling fluid may be a cooling fluid known to those skilled in the art, such as water.
In addition, the temperature drop of the rare earth chloride at each section on the steel belt is adjusted by controlling the running speed of the steel belt and the flow of the cooling fluid spray. In some embodiments of the invention, the flow rate of the cooling fluid is generally in the range of 20 to 60m3The steel strip running speed is generally 2-10 m/min.
In some embodiments of the present invention, the molten rare earth chloride may be spread on the first surface of the steel strip, and the thickness of the spread layer of rare earth chloride is 2-15mm, so as to increase the contact area with the cooling fluid, help to rapidly reduce the temperature of the rare earth chloride, and further shorten the cooling crystallization time to 10-30 min.
In addition, in some embodiments of the invention, the preparation system further comprises a heat dissipation unit and a dust collection unit which are arranged above the conveying unit, and the heat dissipation unit can be an exhaust fan, so that the heat dissipation effect of the rare earth chloride on the steel strip can be accelerated, and the cooling crystallization time can be further shortened. And the dust collecting unit can collect dust, so that the environment pollution and the damage to the health of workers are avoided.
The larger flaky rare earth chloride formed after cooling crystallization passes through a crushing unit, in some embodiments of the invention, the crushing unit is a horizontal crusher, and the larger flaky rare earth chloride can obtain rare earth chloride with the thickness of 2-15mm and the length and width of less than 50mm after passing through the horizontal crusher, and the rare earth chloride has a flaky structure, is thinner and has light weight, and is convenient for feeding and dissolving during subsequent rare earth separation.
In some embodiments of the invention, the preparation system further comprises a weighing unit in communication with the crushing unit and a packaging unit connected to the weighing unit. The weighing unit can be an automatic weighing unit, and controls the weighing weight, and when the set weight is reached, the weighing is stopped. The weighed flaky rare earth chloride flows into a plastic bag, is placed into a plastic woven bag after being hot-pressed or bound by a rope, and then is stored in a dry place.
In the production processes of crushing, weighing, packaging and the like, the contact time of the rare earth chloride and the air is short, so that the phenomenon that the rare earth chloride is hardened due to moisture absorption after being exposed in the air for a long time, the REO content in the rare earth chloride is low, and the feeding difficulty of subsequent rare earth separation is increased is effectively prevented.
Hereinafter, the method for preparing the flaky rare earth chloride provided by the present invention will be described in detail by specific examples.
Unless otherwise specified, the chemical materials and instruments used in the following examples are all conventional chemical materials and conventional instruments, and are commercially available.
Example 1
The embodiment provides a preparation method of flaky chlorinated rare earth, which comprises the following steps:
1) rare earth chloride solution (REO: 273g/L) is put into an evaporation concentration tank for vacuum evaporation concentration under reduced pressure to form molten rare earth chloride, the rare earth chloride is analyzed and detected to have the content of rare earth oxide of 45.2 percent, then the concentration and heating are stopped, the molten rare earth chloride is transferred into a storage tank, the temperature in the storage tank is controlled to be 128 ℃, and the rare earth chloride is kept in a molten state;
2) uniformly distributing molten rare earth chloride on a steel belt through a distributor, wherein the running speed of the steel belt is 3m/min, and rapidly cooling to 23 ℃ in a non-contact water spraying manner for cooling crystallization, wherein the flow rate of the water spraying is 55m3/h；
3) Crushing by a horizontal crusher, weighing and packaging to obtain a flaky chlorinated rare earth product, wherein the thickness of the flaky chlorinated rare earth in the product is 4-6mm, the length of the flaky chlorinated rare earth is 1-50mm, and the width of the flaky chlorinated rare earth in the product is 1-50 mm; the content of rare earth oxide in the product is 46.8 percent, and the product meets the standard requirement of rare earth chloride mixture product (GB/T4148-2015).
Example 2
The embodiment provides a preparation method of flaky chlorinated rare earth, which comprises the following steps:
1) rare earth chloride solution (REO: 189g/L) is put into an evaporation concentration tank for vacuum evaporation concentration under reduced pressure to form molten rare earth chloride, the rare earth chloride is analyzed and detected to have the content of rare earth oxide of 44.3 percent, then the concentration and heating are stopped, the molten rare earth chloride is transferred into a storage tank, the temperature in the storage tank is controlled to be 126 ℃, and the rare earth chloride is kept in a molten state;
2) uniformly distributing molten rare earth chloride on a steel belt through a distributor, wherein the running speed of the steel belt is 2.8m/min, and rapidly cooling to 36 ℃ in a non-contact water spraying manner for cooling crystallization, wherein the flow rate of the water spraying is 39m3/h；
3) Crushing by a horizontal crusher, weighing and packaging to obtain a flaky chlorinated rare earth product, wherein the thickness of the flaky chlorinated rare earth in the product is 5-8mm, the length of the flaky chlorinated rare earth is 1-50mm, and the width of the flaky chlorinated rare earth in the product is 1-50 mm; the content of rare earth oxide in the product is 46.3 percent, and the product meets the standard requirement of rare earth chloride mixture product (GB/T4148-2015).
Example 3
The embodiment provides a preparation method of flaky chlorinated rare earth, which comprises the following steps:
1) rare earth chloride solution (REO: 207g/L) is put into an evaporation concentration tank to be subjected to vacuum evaporation concentration under reduced pressure to form molten rare earth chloride, the rare earth chloride is sent to be analyzed and detected to have the content of rare earth oxide of 43.8 percent, then the concentration and heating are stopped, the molten rare earth chloride is transferred into a storage tank, the temperature in the storage tank is controlled to be 127 ℃, and the rare earth chloride is kept in a molten state;
2) uniformly distributing molten rare earth chloride on a steel belt through a distributor, wherein the running speed of the steel belt is 7.6m/min, and rapidly cooling to 29 ℃ in a non-contact water spraying manner for cooling crystallization, wherein the flow rate of the water spraying is 42m3/h；
3) Crushing by a horizontal crusher, weighing and packaging to obtain a flaky chlorinated rare earth product, wherein the thickness of the flaky chlorinated rare earth in the product is 2-5mm, the length of the flaky chlorinated rare earth is 1-50mm, and the width of the flaky chlorinated rare earth in the product is 1-50 mm; the content of rare earth oxide in the product is 45.6 percent, and the product meets the standard requirement of rare earth chloride mixture product (GB/T4148-2015).
Example 4
The embodiment provides a preparation method of flaky chlorinated rare earth, which comprises the following steps:
1) rare earth chloride solution (REO: 261g/L) is put into an evaporation concentration tank for vacuum evaporation concentration under reduced pressure to form molten rare earth chloride, the rare earth chloride is analyzed and detected to have the content of rare earth oxide of 45.5 percent, then the concentration and heating are stopped, the molten rare earth chloride is transferred into a storage tank, the temperature in the storage tank is controlled to be 129 ℃, and the rare earth chloride is kept in a molten state;
2) uniformly distributing the molten rare earth chloride on a steel belt through a distributor, wherein the running speed of the steel belt is 3.2m/min, and performing non-contact treatmentRapidly cooling to 32 ℃ in a water spraying manner for cooling crystallization, wherein the flow rate of water spraying is 40m3/h；
3) Crushing by a horizontal crusher, weighing and packaging to obtain a flaky chlorinated rare earth product, wherein the thickness of the flaky chlorinated rare earth in the product is 8-12mm, the length of the flaky chlorinated rare earth is 1-50mm, and the width of the flaky chlorinated rare earth in the product is 1-50 mm; the content of rare earth oxide in the product is 47.3 percent, and the product meets the standard requirement of rare earth chloride mixture product (GB/T4148-2015).
Comparative example 1
The comparative example provides a method for preparing flaky chlorinated rare earth, which comprises the following steps:
1) rare earth chloride solution (REO: 281g/L) of the rare earth chloride is put into an evaporation concentration tank for vacuum evaporation concentration under reduced pressure to form molten rare earth chloride, the rare earth chloride is sent to be analyzed and detected to have the content of rare earth oxide of 41.4 percent, then the concentration and the heating are stopped, the molten rare earth chloride is transferred into a storage tank, the temperature in the storage tank is controlled to be 127 ℃, and the rare earth chloride is kept in a molten state;
2) uniformly distributing molten rare earth chloride on a steel belt through a distributor, wherein the running speed of the steel belt is 6.7m/min, and rapidly cooling to 29 ℃ in a non-contact water spraying manner for cooling crystallization, wherein the flow rate of the water spraying is 31m3/h；
3) And crushing by a horizontal crusher, weighing and packaging to obtain the rare earth chloride product. However, the cooled and crystallized rare earth chlorides have the phenomenon of mutual adhesion and are difficult to break; the content of rare earth oxide in the product is 43.7 percent, which does not meet the standard requirement of rare earth chloride mixture product (GB/T4148-2015).
Comparative example 2
The comparative example provides a method for preparing flaky chlorinated rare earth, which comprises the following steps:
1) rare earth chloride solution (REO: 226g/L) is put into an evaporation concentration tank for vacuum evaporation concentration under reduced pressure to form molten rare earth chloride, the rare earth chloride is sent to be analyzed and detected to have the content of rare earth oxide of 48.2 percent, then the concentration and heating are stopped, the molten rare earth chloride is transferred into a storage tank, the temperature in the storage tank is controlled to be 128 ℃, and the rare earth chloride is kept in a molten state;
2) uniformly distributing molten rare earth chloride on a steel belt through a distributor, wherein the running speed of the steel belt is 5.3m/min, and rapidly cooling to 36 ℃ in a non-contact water spraying manner for cooling crystallization, wherein the flow rate of the water spraying is 55m3/h；
3) And crushing by a horizontal crusher, weighing and packaging to obtain the rare earth chloride product. Although the content of rare earth oxide in the product is 48.5 percent and meets the standard requirement of mixed rare earth chloride products (GB/T4148-2015), the flaky rare earth chloride is difficult to crush in a crusher, and the surface hardening phenomenon appears after the product is placed in a sealed state for a period of time, so that the content of the oxidized rare earth in the surface product in a product bag is low, and the feeding is difficult during the subsequent rare earth separation.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the flaky rare earth chloride is realized by a preparation system of the flaky rare earth chloride, wherein the preparation system comprises a melting unit, a continuous discharging unit, a conveying unit and a crushing unit which are sequentially connected, and the preparation method comprises the following steps:
1) putting the rare earth chloride solution into a melting unit, evaporating and concentrating to form molten rare earth chloride, wherein the content of rare earth oxide in the rare earth chloride is 42-48%;
2) the molten rare earth chloride is conveyed to the conveying unit through the continuous discharging unit, and is cooled to below 40 ℃ on the conveying unit, so that the rare earth chloride is cooled and crystallized;
3) and conveying the cooled and crystallized rare earth chloride into the crushing unit for crushing to obtain flaky rare earth chloride.
2. The method according to claim 1, wherein the flaky rare earth chloride has a thickness of 2 to 15mm and a length and a width of less than 50 mm.
3. The manufacturing method according to claim 1, wherein the conveying unit comprises a steel belt and a driving member for driving the steel belt to run, wherein the running speed of the steel belt is 2-10 m/min.
4. The method according to claim 3, wherein the steel strip has a first surface and a second surface opposite to the first surface, wherein the first surface is used for carrying the molten rare earth chloride, and the second surface is used for contacting with a cooling fluid to reduce the temperature of the molten rare earth chloride to below 40 ℃.
5. The method of claim 4, wherein the cooling fluid has a flow rate of 20-60m3/h。
6. The method according to claim 4, wherein the molten rare earth chloride is spread on the first surface of the steel strip, and the thickness of the chlorinated rare earth layer spread on the first surface is 2-15 mm.
7. The manufacturing method according to claim 4, wherein the manufacturing system further includes a heat radiating unit and a dust collecting unit disposed above the conveying unit.
8. The method according to claim 6, wherein the cooling crystallization time is 10-30 min.
9. The method of claim 6, further comprising a weighing unit in communication with the crushing unit and a packaging unit connected to the weighing unit.
10. The method according to claim 1, wherein in step 1), the molten rare earth chloride can be stored in an environment of 125 ℃ or higher and maintained in a molten state.
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| CN116497240A (en) * | 2023-05-24 | 2023-07-28 | 山东域潇有色新材料有限公司 | Preparation system for preparing yttrium-rich rare earth by xenotime |
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