CN113310312B - Dehydration device for preparing anhydrous rare earth halide - Google Patents
Dehydration device for preparing anhydrous rare earth halide Download PDFInfo
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- CN113310312B CN113310312B CN202110630849.7A CN202110630849A CN113310312B CN 113310312 B CN113310312 B CN 113310312B CN 202110630849 A CN202110630849 A CN 202110630849A CN 113310312 B CN113310312 B CN 113310312B
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/14—Rotary-drum furnaces, i.e. horizontal or slightly inclined with means for agitating or moving the charge
- F27B7/16—Rotary-drum furnaces, i.e. horizontal or slightly inclined with means for agitating or moving the charge the means being fixed relatively to the drum, e.g. composite means
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/10—Rotary-drum furnaces, i.e. horizontal or slightly inclined internally heated, e.g. by means of passages in the wall
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/20—Details, accessories, or equipment peculiar to rotary-drum furnaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/20—Details, accessories, or equipment peculiar to rotary-drum furnaces
- F27B7/32—Arrangement of devices for charging
- F27B7/3205—Charging
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/20—Details, accessories, or equipment peculiar to rotary-drum furnaces
- F27B7/34—Arrangements of heating devices
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B7/00—Rotary-drum furnaces, i.e. horizontal or slightly inclined
- F27B7/20—Details, accessories, or equipment peculiar to rotary-drum furnaces
- F27B7/42—Arrangement of controlling, monitoring, alarm or like devices
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Engineering & Computer Science (AREA)
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- General Engineering & Computer Science (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a dehydration device for preparing anhydrous rare earth halide, which comprises a rotary furnace, wherein a furnace tube is arranged in the rotary furnace, a plurality of material stirring plates are arranged in the furnace tube, a microwave generator and a resistance wire are arranged in the rotary furnace, the microwave generator and the resistance wire are both positioned at the outer side of the furnace tube, one side of the rotary furnace is provided with a rotary transmission mechanism, and the rotary transmission mechanism is connected with the furnace tube. The dehydration device for preparing the anhydrous rare earth halide provided by the invention utilizes the microwave generated by the microwave generator to dehydrate the hydrated rare earth halide, then closes the microwave generator, opens the lower resistance wire to carry out high-temperature treatment, separates the dehydrating agent, and condenses the removed moisture and the dehydrating agent in the condenser after passing through the buffer tank.
Description
Technical Field
The invention belongs to the field of rare earth halides, and particularly relates to a dehydration device for preparing anhydrous rare earth halides.
Background
The anhydrous rare earth halide is an important chemical reagent in chemical industry and manufacturing industry, and has important and wide application prospect in the fields of luminescent materials, heat insulation materials, hydrogen storage materials, ceramic materials, catalysis, military industry and the like. However, the preparation of anhydrous rare earth halides requires removal of impurities such as oxyhalides and oxides of rare earth halides, which are formed due to their extreme deliquescence, which makes the preparation of anhydrous rare earth halides extremely difficult.
At present, the equipment for preparing anhydrous rare earth halide by dehydrating hydrated rare earth halide mainly comprises 1. A vacuum shaft furnace, 2. A horizontal tube furnace, 3. A microwave drying box matched with a rotary furnace and the like. The vacuum pit furnace and the horizontal tube furnace adopt a heat radiation heating mode, and the equipment can realize the preparation of the anhydrous rare earth halide by one step, but the production cycle is longer, and one production cycle can reach 24 to 36 hours; the microwave drying box is matched with the rotary furnace, because the microwave rapid dehydration principle is utilized, the production cycle is shortened to a certain extent, the operation can be completed within 20 hours, and the operation is more complicated because the material is required to be discharged and filled secondarily. At present, equipment with short production period, recyclable auxiliary materials and simple and convenient operation is urgently needed to complete the production task.
Disclosure of Invention
In view of the above, the present invention provides a dehydration apparatus for preparing anhydrous rare earth halide, which aims to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the dehydration device for preparing the anhydrous rare earth halide comprises a rotary furnace, wherein a furnace tube is arranged in the rotary furnace, a plurality of material turning plates are arranged in the furnace tube, a microwave generator and a resistance wire are arranged in the rotary furnace, the microwave generator and the resistance wire are both positioned on the outer side of the furnace tube, a rotary transmission mechanism is arranged on one side of the rotary furnace, and the rotary transmission mechanism is connected with the furnace tube.
Further, the rotary furnace comprises an upper hearth and a lower hearth, the upper hearth is positioned above the lower hearth, the furnace tube is positioned between the upper hearth and the lower hearth, the microwave generator is fixed on the inner side of the upper hearth, and the resistance wire is positioned on the inner side of the lower hearth; the microwave generator is positioned above the furnace tube, and the resistance wire is positioned below the furnace tube.
Furthermore, the rotary transmission mechanism adopts a gear transmission mechanism or a belt transmission mechanism.
Furthermore, the rotary transmission mechanism comprises a driven gear, a driving gear and a first motor, wherein the driven gear is fixed at one end of the furnace tube and is meshed with the driving gear, and the driving gear is connected with the first motor.
Furthermore, the dehydration device also comprises a water injection vacuum pump, a jacket condenser and a buffer tank, wherein the water injection vacuum pump is connected with the jacket condenser through a pipeline, and the jacket condenser and the rotary furnace are respectively connected with the buffer tank through pipelines.
Furthermore, the material turning plate is of a trapezoid structure, one end of the material turning plate is fixed on the inner side of the furnace tube, and the other end of the material turning plate faces the central line of the furnace tube.
Furthermore, the furnace tube is made of quartz or ceramic.
Furthermore, the buffer tank is made of polypropylene or polyethylene.
Furthermore, the jacket condenser is made of glass or quartz; the material of the water jet vacuum pump is PP material; the pipeline is made of polytetrafluoroethylene, quartz or glass.
Furthermore, a water inlet and a water outlet are arranged on the jacket condenser, the water outlet is positioned at the upper part of the jacket condenser, the water inlet is positioned at the lower part of the jacket condenser, a rotating shaft is arranged inside the jacket condenser, the top of the rotating shaft is connected with a second motor, a scraping plate is arranged on the rotating shaft, and a collecting tank is arranged below the rotating shaft; the scraping plate is made of one of polytetrafluoroethylene, PP (polypropylene), quartz or glass; the collecting tank is made of one of polytetrafluoroethylene, PP (polypropylene), quartz or glass.
The frequency of the microwave generator is 2450MHz or 915MHz.
Hydrated rare earth halide is LnX 3 ·nH 2 O, wherein Ln is one of La, ce, pr, nd, eu, sm, yb or Y, X is one of F, cl, br or I, and n is less than or equal to 7.
The method comprises the steps of filling materials into a furnace tube, arranging a trapezoidal material turning plate inside the furnace tube, starting a first motor, starting a water injection vacuum pump, enabling the water injection vacuum pump to be made of plastic, starting a microwave generator on the upper portion of a hearth after the vacuum degree reaches a certain requirement, performing dehydration treatment, closing the microwave generator after the dehydration treatment is finished, opening a heating resistance wire on the lower portion to heat, separating a dehydrating agent, closing heating after the operation is finished, cooling, discharging after the temperature is reduced to 40 ℃, uniformly collecting the dehydrating agent condensed by a jacket condenser, and then recycling the dehydrating agent, wherein the jacket condenser is made of glass. The equipment is greatly shortened in production period, high in production efficiency, simple and convenient to operate, capable of avoiding the trouble of secondary material filling, capable of being repeatedly used by collecting the dehydrating agent separated out simultaneously, and stable in quality of produced products, and meets the national environment-friendly production requirements.
Compared with the prior art, the invention has the following advantages:
the dehydration device for preparing the anhydrous rare earth halide provided by the invention utilizes the microwave generated by the microwave generator to dehydrate the hydrated rare earth halide, then the microwave generator is closed, the lower resistance wire is opened to carry out high-temperature treatment, the dehydrating agent is separated, the removed moisture and the dehydrating agent are condensed in the condenser after passing through the buffer tank, meanwhile, the condenser is internally provided with the rotary scraping plate, and the rotary scraping plate is hung and falls into the collecting tank after the materials are condensed, so that the condensed materials are conveniently recovered, and the condensing efficiency can be ensured. The collected dehydrating agent can be recycled because the material is not contacted with any metal in the treatment process, thereby saving the preparation cost; meanwhile, the anhydrous rare earth halide can be prepared in one step with high efficiency, energy conservation and high quality through the equipment.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of a dehydration apparatus for preparing anhydrous rare earth halide according to an embodiment of the present invention;
FIG. 2 is a schematic view of a rotary kiln according to an embodiment of the present invention;
fig. 3 is a cross-sectional view of a furnace tube according to an embodiment of the invention.
Description of reference numerals:
1. a water jet vacuum pump; 2. a jacket condenser; 3. a buffer tank; 4. a rotary kiln; 5. a furnace tube; 6. a material turning plate; 7. a microwave generator; 8. a resistance wire; 21. a water inlet; 22. a water outlet; 23. a second motor; 24. a rotating shaft; 25. a scraping plate; 26. a collection tank; 9. a rotation transmission mechanism; 41. an upper hearth; 42. a lower hearth; 91. a driven gear; 92. a driving gear; 93. a first motor.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings, which are based on the orientations and positional relationships indicated in the drawings, and are used for convenience in describing the present invention and for simplicity in description, but do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
As shown in fig. 1-3, a dehydration device for preparing anhydrous rare earth halide comprises a rotary furnace 4, a furnace tube 5 is arranged in the rotary furnace 4, 4 material stirring plates 6 are arranged in the furnace tube 5, a microwave generator 7 and a resistance wire 8 are arranged in the rotary furnace 4, the microwave generator 7 and the resistance wire 8 are both positioned at the outer side of the furnace tube 5, a rotary transmission mechanism 9 is arranged at one side of the rotary furnace 4, and the rotary transmission mechanism 9 is connected with the furnace tube 5.
Further, the rotary kiln 4 comprises an upper hearth 41 and a lower hearth 42, the upper hearth 41 is located above the lower hearth 42, the furnace tube 5 is located between the upper hearth 41 and the lower hearth 42, the microwave generator 7 is fixed on the inner side of the upper hearth 41, and the resistance wire 8 is located on the inner side of the lower hearth 42; the microwave generator 7 is positioned above the furnace tube 5, and the resistance wire 8 is positioned below the furnace tube 5.
The rotary transmission mechanism 9 adopts a gear transmission mechanism. The rotary transmission mechanism 9 comprises a driven gear 91, a driving gear 92 and a first motor 93, wherein the driven gear 91 is fixed at one end of the furnace tube 5, the driven gear 91 is meshed with the driving gear 92, and the driving gear 92 is connected with the first motor 93.
The dehydration device also comprises a water injection vacuum pump 1, a jacket condenser 2 and a buffer tank 3, wherein the water injection vacuum pump 1 is connected with the jacket condenser 2 through a pipeline, and the jacket condenser 2 and the rotary furnace 4 are respectively connected with the buffer tank 3 through pipelines.
The material turning plate 6 is in a trapezoid structure, one end of the material turning plate 6 is fixed on the inner side of the furnace tube 5, and the other end of the material turning plate faces to the central line of the furnace tube 5.
The furnace tube 5 is made of quartz. The buffer tank 3 is made of polypropylene. The jacket condenser 2 is made of quartz; the material of the water jet vacuum pump 1 is PP material; the pipeline is made of polytetrafluoroethylene.
A water inlet 21 and a water outlet 22 are arranged on the jacket condenser 2, the water outlet 22 is positioned at the upper part of the jacket condenser 2, the water inlet 21 is positioned at the lower part of the jacket condenser 2, a rotating shaft 24 is arranged inside the jacket condenser 2, the top of the rotating shaft 24 is connected with a second motor 23, a scraping plate 25 is arranged on the rotating shaft 24, and a collecting tank 26 is arranged below the rotating shaft 24; the material of the scraper plate 25 is polytetrafluoroethylene; the collection tank 26 is made of a material.
The implementation process comprises the following steps:
firstly, filling a mixture of neodymium chlorohydrate and a dehydrating agent into a furnace tube 5, starting a water jet vacuum pump 1, starting a first motor 93 after the vacuum degree reaches-0.096 MPa, starting a microwave generator 7 at the upper part of a hearth for dehydration treatment, closing the microwave generator 7 after 2 hours, starting a heating resistance wire 8 at the lower part of the hearth, raising the temperature to 300 ℃, separating the dehydrating agent, closing the heating after 8 hours, raising a furnace cover for cooling, and closing the water jet vacuum pump 1 after the temperature is reduced to 40 ℃, thereby carrying out discharging operation. The stripping results are shown in table 1.
TABLE 1 dehydration results for different products
| The theoretical total amount of rare earth% | Detecting the total content of rare earth% | Detecting the water content% | |
| Anhydrous cerium chloride | 56.83％ | 56.78％ | 1％ |
| Anhydrous lanthanum chloride | 56.63％ | 56.56％ | 1.20％ |
| Anhydrous neodymium chloride | 57.56％ | 57.50％ | 0.80％ |
Through detection, the total amount of the rare earth of the anhydrous rare earth halide prepared by the dehydrating device is very close to the theoretical total amount of the rare earth, and the water content is controlled to be below 1.5 percent, which shows that the device can prepare the anhydrous rare earth halide with high quality and thorough dehydrating agent removal.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The utility model provides a dehydration device of preparation anhydrous rare earth halide which characterized in that: the rotary furnace comprises a rotary furnace, wherein a furnace tube is arranged in the rotary furnace, a plurality of material turning plates are arranged in the furnace tube, a microwave generator and a resistance wire are arranged in the rotary furnace, the microwave generator and the resistance wire are both positioned at the outer side of the furnace tube, one side of the rotary furnace is provided with a rotary transmission mechanism, and the rotary transmission mechanism is connected with the furnace tube;
the rotary furnace comprises an upper hearth and a lower hearth, the upper hearth is positioned above the lower hearth, the furnace tube is positioned between the upper hearth and the lower hearth, the microwave generator is fixed on the inner side of the upper hearth, and the resistance wire is positioned on the inner side of the lower hearth; the microwave generator is positioned above the furnace tube, and the resistance wire is positioned below the furnace tube;
the dehydration device also comprises a water injection vacuum pump, a jacket condenser and a buffer tank, wherein the water injection vacuum pump is connected with the jacket condenser through a pipeline, and the jacket condenser and the rotary furnace are respectively connected with the buffer tank through pipelines;
the material turning plate is of a trapezoidal structure, one end of the material turning plate is fixed on the inner side of the furnace tube, and the other end of the material turning plate faces to the central line of the furnace tube.
2. The dehydration apparatus for producing an anhydrous rare earth halide according to claim 1, wherein: the rotary transmission mechanism adopts a gear transmission mechanism or a belt transmission mechanism.
3. The dehydration apparatus for producing anhydrous rare earth halide according to claim 2, wherein: the rotary transmission mechanism comprises a driven gear, a driving gear and a first motor, wherein the driven gear is fixed at one end of the furnace tube and meshed with the driving gear, and the driving gear is connected with the first motor.
4. The dehydration apparatus for producing anhydrous rare earth halide according to claim 1, wherein: the furnace tube is made of quartz or ceramic.
5. The dehydration apparatus for producing anhydrous rare earth halide according to claim 1, wherein: the buffer tank is made of polypropylene or polyethylene.
6. The dehydration apparatus for producing an anhydrous rare earth halide according to claim 1, wherein: the jacket condenser is made of glass or quartz; the material of the water jet vacuum pump is PP material; the pipeline is made of polytetrafluoroethylene, quartz or glass.
7. The dehydration apparatus for producing an anhydrous rare earth halide according to claim 1, wherein: the jacket condenser is provided with a water inlet and a water outlet, the water outlet is positioned at the upper part of the jacket condenser, the water inlet is positioned at the lower part of the jacket condenser, a rotating shaft is arranged inside the jacket condenser, the top of the rotating shaft is connected with a second motor, a scraping plate is arranged on the rotating shaft, and a collecting tank is arranged below the rotating shaft; the scraping plate is made of one of polytetrafluoroethylene, PP (polypropylene), quartz or glass; the collecting tank is made of one of polytetrafluoroethylene, PP (polypropylene), quartz or glass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110630849.7A CN113310312B (en) | 2021-06-07 | 2021-06-07 | Dehydration device for preparing anhydrous rare earth halide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110630849.7A CN113310312B (en) | 2021-06-07 | 2021-06-07 | Dehydration device for preparing anhydrous rare earth halide |
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| CN113310312B true CN113310312B (en) | 2022-11-08 |
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| CN113636585A (en) * | 2021-09-28 | 2021-11-12 | 安徽吉华新材料有限公司 | Preparation method for preparing high-purity anhydrous neodymium chloride under normal pressure |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2027521A (en) * | 1978-08-07 | 1980-02-20 | Sherwood W L | Discharging rotary furnaces |
| CN103644730A (en) * | 2013-11-07 | 2014-03-19 | 新时代集团浙江新能源材料有限公司 | Powder material calcination rotary furnace with large-diameter furnace tube and calcination method thereof |
| CN105222582A (en) * | 2015-10-23 | 2016-01-06 | 湖南华冶微波科技有限公司 | A kind of microwave, electric Hybrid Heating high-temperature service |
| US20200300465A1 (en) * | 2015-11-27 | 2020-09-24 | Hunan Dingjiu Energy And Environment Technology Ltd. | Rotary furnace |
| CN112629261A (en) * | 2020-12-02 | 2021-04-09 | 湖南华冶微波科技有限公司 | Microwave and electric hybrid heating tube furnace and control method |
-
2021
- 2021-06-07 CN CN202110630849.7A patent/CN113310312B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2027521A (en) * | 1978-08-07 | 1980-02-20 | Sherwood W L | Discharging rotary furnaces |
| CN103644730A (en) * | 2013-11-07 | 2014-03-19 | 新时代集团浙江新能源材料有限公司 | Powder material calcination rotary furnace with large-diameter furnace tube and calcination method thereof |
| CN105222582A (en) * | 2015-10-23 | 2016-01-06 | 湖南华冶微波科技有限公司 | A kind of microwave, electric Hybrid Heating high-temperature service |
| US20200300465A1 (en) * | 2015-11-27 | 2020-09-24 | Hunan Dingjiu Energy And Environment Technology Ltd. | Rotary furnace |
| CN112629261A (en) * | 2020-12-02 | 2021-04-09 | 湖南华冶微波科技有限公司 | Microwave and electric hybrid heating tube furnace and control method |
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