CN114100529A - Dry-type fluorination device and terbium fluoride preparation method - Google Patents
Dry-type fluorination device and terbium fluoride preparation method Download PDFInfo
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- CN114100529A CN114100529A CN202210076562.9A CN202210076562A CN114100529A CN 114100529 A CN114100529 A CN 114100529A CN 202210076562 A CN202210076562 A CN 202210076562A CN 114100529 A CN114100529 A CN 114100529A
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
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- 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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- 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
- C01F17/265—Fluorides
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Abstract
The invention relates to a dry fluorination device and a method for preparing terbium fluoride, wherein the dry fluorination device comprises a hydrogen fluoride gas storage tank, a horizontal dry fluorination furnace and a tail gas purification device which are sequentially connected, the horizontal dry fluorination furnace comprises a resistance wire heating sleeve, a stainless steel furnace body and a rotary high-temperature corrosion-resistant inner container which are sequentially arranged from outside to inside, and the rotary high-temperature corrosion-resistant inner container is connected with a rotation driving device; the method for preparing terbium fluoride comprises the following steps: heating the dry type fluorination device, putting a raw material terbium oxide into a rotary high-temperature corrosion-resistant inner container after the temperature is stable, then introducing anhydrous hydrogen fluoride gas at a constant speed, calculating the whole excess by 40% according to the process, stopping gas after 10 hours, not cooling, discharging at a high temperature, and then putting the high-temperature terbium fluoride into a vacuum box for cooling. On the premise of ensuring the product quality, the invention reduces the consumption of hydrogen fluoride, shortens the reaction time of a single furnace, reduces the energy consumption, improves the production efficiency, does not need to be cooled when the equipment discharges materials, and has small equipment loss and high reliability.
Description
Technical Field
The invention relates to the technical field of terbium fluoride preparation, in particular to a dry type fluorination device and a method for preparing terbium fluoride.
Background
There are two common dry processes for terbium fluoride preparation. One method is to mix ammonium bifluoride and terbium oxide uniformly and then react, and the method is a solid-solid reaction and has the problem of incomplete reaction, and has the deaminizing and dehydrating process treatment and more complex steps. The other one is obtained by reacting anhydrous hydrogen fluoride with terbium oxide, but the hydrogen fluoride is usually excessive by 2-3 times, the hydrogen fluoride loss is large, and the tail gas emission is large; moreover, the single furnace has long reaction time which needs 48 to 60 hours, and has large energy consumption and low production efficiency.
The traditional equipment used in the dry preparation process is in a frequent cold and hot state, so that the corrosion of the inner container is aggravated, the service life of the equipment is shortened, the equipment needs to be frequently replaced, the equipment loss is high, and the reliability is low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a dry fluorination device and a method for preparing terbium fluoride.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a dry-type fluorination device, includes hydrogen fluoride gas holder, horizontal dry process fluorination stove and tail gas cleanup unit that connect gradually, and horizontal dry process fluorination stove is including resistance wire heating jacket, stainless steel furnace body and the rotatory high temperature corrosion-resistant inner bag that sets gradually from the extroversion inwards, and wherein, rotatory high temperature corrosion-resistant inner bag even has rotation drive arrangement, and rotatory high temperature corrosion-resistant inner bag can 360 rotatory.
The bottom of the hydrogen fluoride gas storage tank is provided with an electronic scale.
The rotation driving device is a motor.
A method for preparing terbium fluoride comprises the following specific steps:
s1 preparation of raw materials
Calculating the mass of the raw material terbium oxide according to the mass of the terbium fluoride to be prepared, and weighing to obtain the raw material terbium oxide;
s2, preheating
Firstly, heating the temperature inside a stainless steel furnace body of the dry-type fluorination device to 500 ℃ and 550 ℃ by using a resistance wire heating sleeve, and carrying out heat preservation treatment for a period of time;
s3, Synthesis reaction
After the temperature is stable, putting the raw material terbium oxide obtained in the step S1 into a rotary high-temperature corrosion-resistant inner container of a dry type fluorination device, then opening a control valve of a hydrogen fluoride storage tank, introducing anhydrous hydrogen fluoride gas into the rotary high-temperature corrosion-resistant inner container at a constant speed, wherein the introduced hydrogen fluoride gas is 40% more than a theoretical value, the rotary high-temperature corrosion-resistant inner container is driven by a rotation driving device to rotate, the rotating speed of the rotary high-temperature corrosion-resistant inner container is 40 revolutions per minute, the rotary high-temperature corrosion-resistant inner container is stopped for 15-20 minutes after rotating every 180 degrees, and the synthetic reaction is carried out for 10 hours;
s4, high-temperature discharging
And after the synthesis reaction is finished, discharging at high temperature, and cooling the prepared high-temperature terbium fluoride in a vacuum box.
In step S4, the prepared high-temperature terbium fluoride is put into a tray, and then put into a vacuum box for cooling.
The invention has the beneficial effects that: on the premise of ensuring the product quality, the invention reduces the consumption of hydrogen fluoride, shortens the reaction time of a single furnace, reduces the energy consumption, improves the production efficiency, does not need to be cooled when the equipment discharges materials, prolongs the service life of the equipment, and has small equipment loss and high reliability.
Drawings
FIG. 1 is a schematic structural view of a dry fluorination apparatus of the present invention;
FIG. 2 is a schematic cross-sectional view of a horizontal dry fluorination furnace;
in the figure: 1-a hydrogen fluoride gas storage tank; 2-horizontal dry fluorination furnace; 3-a tail gas purification device; 4-electronic scale;
2.1-resistance wire heating jacket; 2.2-stainless steel furnace body; 2.3-rotating the high-temperature corrosion-resistant inner container;
the following detailed description will be made in conjunction with embodiments of the present invention with reference to the accompanying drawings.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
as shown in fig. 1 to 2, the dry fluorination device comprises a hydrogen fluoride gas storage tank 1, a horizontal dry fluorination furnace 2 and a tail gas purification device 3 which are sequentially connected, wherein the horizontal dry fluorination furnace 2 comprises a resistance wire heating sleeve 2.1, a stainless steel furnace body 2.2 and a rotary high-temperature corrosion-resistant liner 2.3 which are sequentially arranged from outside to inside, wherein the rotary high-temperature corrosion-resistant liner 2.3 is connected with a rotation driving device, and the rotary high-temperature corrosion-resistant liner 2.3 can rotate by 360 degrees.
An electronic scale 4 is arranged at the bottom of the hydrogen fluoride storage tank 1.
The rotation driving device is a motor.
A method for preparing terbium fluoride comprises the following specific steps:
s1 preparation of raw materials
Calculating the mass of the raw material terbium oxide according to the mass of the terbium fluoride to be prepared, and weighing to obtain the raw material terbium oxide;
s2, preheating
Firstly, the temperature in a stainless steel furnace body 2.2 of the dry type fluorination device is raised to 500-550 ℃ by using a resistance wire heating sleeve 2.1, and heat preservation treatment is carried out for a period of time;
s3, Synthesis reaction
After the temperature is stable, putting the raw material terbium oxide obtained in the step S1 into a rotary high-temperature corrosion-resistant inner container 2.3 of a dry type fluorination device, then opening a control valve of a hydrogen fluoride gas storage tank 1, introducing anhydrous hydrogen fluoride gas into the rotary high-temperature corrosion-resistant inner container 2.3 at a constant speed, wherein the introduced hydrogen fluoride gas is excessive by 40% compared with the theoretical value, the rotary high-temperature corrosion-resistant inner container 2.3 is driven by a rotary driving device to rotate, the rotating speed of the rotary high-temperature corrosion-resistant inner container 2.3 is 40 revolutions per minute, the rotary high-temperature corrosion-resistant inner container 2.3 is stopped for 15-20 minutes after rotating by 180 degrees every time, and the synthetic reaction is carried out for 10 hours;
s4, high-temperature discharging
And after the synthesis reaction is finished, discharging at high temperature, and cooling the prepared high-temperature terbium fluoride in a vacuum box.
In step S4, the prepared high-temperature terbium fluoride is put into a tray, and then put into a vacuum box for cooling.
Specific example 1:
the temperature of the horizontal dry-method fluorination furnace 2 is 500 ℃, 10 kg of terbium oxide is put into the rotary high-temperature corrosion-resistant inner container 2.3, the rotating speed of the rotary high-temperature corrosion-resistant inner container 2.3 is 40 r/min, the waiting time of 180 degrees is 15 min, the aeration speed of anhydrous hydrogen fluoride is 0.45 kg/h, the integral aeration time is controlled for 10 h, and the total aeration amount is 4.5 kg.
And (3) discharging at high temperature after gas is stopped, putting the prepared high-temperature terbium fluoride into a material tray by using a tool, and then putting the material tray into a vacuum box for cooling.
After cooling, 11.46 kg of terbium fluoride is obtained, and REO 85.46% is detected.
Specific example 2:
the temperature of the horizontal dry-method fluorination furnace 2 is 550 ℃, 10 kg of terbium oxide is put into the rotary high-temperature corrosion-resistant inner container 2.3, the rotating speed of the rotary high-temperature corrosion-resistant inner container 2.3 is 40 revolutions per minute, the waiting time of 180 degrees is 15 minutes, the aeration speed of anhydrous hydrogen fluoride is 0.45 kg/hour, the integral aeration time is controlled for 10 hours, and the total aeration quantity is 4.5 kg.
And (3) discharging at high temperature after gas is stopped, putting the prepared high-temperature terbium fluoride into a material tray by using a tool, and then putting the material tray into a vacuum box for cooling.
After cooling, 11.46 kg of terbium fluoride is obtained, and REO 85.72% is detected.
Specific example 3:
the temperature of the horizontal dry-method fluorination furnace 2 is 550 ℃, 15 kg of terbium oxide is put into the rotary high-temperature corrosion-resistant inner container 2.3, the rotating speed of the rotary high-temperature corrosion-resistant inner container 2.3 is 40 revolutions per minute, the waiting time of 180 degrees is 15 minutes, the aeration speed of anhydrous hydrogen fluoride is 0.68 kg/hour, the integral aeration time is controlled to be 10 hours, and the total aeration quantity is 6.8 kg.
And (3) discharging at high temperature after gas is stopped, putting the prepared high-temperature terbium fluoride into a material tray by using a tool, and then putting the material tray into a vacuum box for cooling.
After cooling, 17.21 kg of terbium fluoride is obtained, and REO 86.11% is detected.
Specific example 4:
the temperature of the horizontal dry-method fluorination furnace 2 is 550 ℃, 15 kg of terbium oxide is put into the rotary high-temperature corrosion-resistant inner container 2.3, the rotating speed of the rotary high-temperature corrosion-resistant inner container 2.3 is 40 revolutions per minute, the waiting time of 180 degrees is 20 minutes, the aeration speed of anhydrous hydrogen fluoride is 0.68 kg/hour, the integral aeration time is controlled to be 10 hours, and the total aeration quantity is 6.8 kg.
And (3) discharging at high temperature after gas is stopped, putting the prepared high-temperature terbium fluoride into a material tray by using a tool, and then putting the material tray into a vacuum box for cooling.
After cooling, 17.22 kg of terbium fluoride is obtained, and REO 85.13% is detected.
On the premise of ensuring the product quality, the invention reduces the consumption of hydrogen fluoride from the original excess of 200% to the excess of 40%, shortens the reaction time of a single furnace from the original 60 hours to 10 hours, reduces the energy consumption, improves the production efficiency, and ensures that the redundant hydrogen fluoride and water vapor directly enter the tail gas purification device 3 from the exhaust port without polluting the outside. The whole equipment and the process are simple to operate, the controllable point is high, unmanned operation can be basically realized except for material entering and exiting of the equipment, the material entering and exiting does not need to be cooled, the service life of the equipment is prolonged, equipment loss is small, and reliability is high.
The invention has been described in connection with the accompanying drawings, it is to be understood that the invention is not limited to the specific embodiments disclosed, but is intended to cover various modifications, adaptations or uses of the invention, and all such modifications and variations are within the scope of the invention.
Claims (5)
1. The utility model provides a dry-type fluorination device, includes hydrogen fluoride gas holder (1), horizontal dry process fluorination stove (2) and tail gas cleanup unit (3) that connect gradually, its characterized in that, horizontal dry process fluorination stove (2) are including resistance wire heating jacket (2.1), stainless steel furnace body (2.2) and rotatory high temperature corrosion-resistant inner bag (2.3) that set gradually from the extroversion, wherein, rotatory high temperature corrosion-resistant inner bag (2.3) even have rotation drive arrangement, rotatory high temperature corrosion-resistant inner bag (2.3) can 360 rotatory.
2. The dry fluorination apparatus as claimed in claim 1, wherein an electronic scale (4) is installed at the bottom of the hydrogen fluoride storage tank (1).
3. A dry fluorination device as claimed in claim 2 wherein the rotary drive means is an electric motor.
4. A method for preparing terbium fluoride by using the dry fluorination device of any one of claims 1 to 3, which comprises the following steps:
s1 preparation of raw materials
Calculating the mass of the raw material terbium oxide according to the mass of the terbium fluoride to be prepared, and weighing to obtain the raw material terbium oxide;
s2, preheating
Firstly, the temperature in a stainless steel furnace body (2.2) of the dry type fluorination device is raised to 500-550 ℃ by using a resistance wire heating sleeve (2.1), and heat preservation treatment is carried out for a period of time;
s3, Synthesis reaction
After the temperature is stable, putting the raw material terbium oxide obtained in the step S1 into a rotary high-temperature corrosion-resistant inner container (2.3) of a dry type fluorination device, then opening a control valve of a hydrogen fluoride gas storage tank (1), introducing anhydrous hydrogen fluoride gas into the rotary high-temperature corrosion-resistant inner container (2.3) at a constant speed, wherein the introduced hydrogen fluoride gas is excessive by 40 percent compared with the theoretical value, the rotary high-temperature corrosion-resistant inner container (2.3) is driven by a rotary driving device to rotate, the rotating speed of the rotary high-temperature corrosion-resistant inner container (2.3) is 40 revolutions per minute, the rotary high-temperature corrosion-resistant inner container (2.3) is stopped for 15-20 minutes after rotating by 180 degrees every time, and a synthetic reaction is carried out for 10 hours;
s4, high-temperature discharging
And after the synthesis reaction is finished, discharging at high temperature, and cooling the prepared high-temperature terbium fluoride in a vacuum box.
5. The method for preparing terbium fluoride according to claim 4, wherein in step S4, the prepared high-temperature terbium fluoride is placed in a tray and then placed in a vacuum chamber for cooling.
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| CN202210076562.9A CN114100529A (en) | 2022-01-24 | 2022-01-24 | Dry-type fluorination device and terbium fluoride preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115159556A (en) * | 2022-07-26 | 2022-10-11 | 中天捷晟(天津)新材料科技有限公司 | Horizontal dry-process fluorination device and fluorination method for terbium fluoride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201962084U (en) * | 2011-03-18 | 2011-09-07 | 赣州科力稀土新材料有限公司 | Device for preparing rare-earth fluoride |
| WO2017008092A1 (en) * | 2015-07-10 | 2017-01-19 | Plansee Se | Metal filter |
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2022
- 2022-01-24 CN CN202210076562.9A patent/CN114100529A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201962084U (en) * | 2011-03-18 | 2011-09-07 | 赣州科力稀土新材料有限公司 | Device for preparing rare-earth fluoride |
| WO2017008092A1 (en) * | 2015-07-10 | 2017-01-19 | Plansee Se | Metal filter |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115159556A (en) * | 2022-07-26 | 2022-10-11 | 中天捷晟(天津)新材料科技有限公司 | Horizontal dry-process fluorination device and fluorination method for terbium fluoride |
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