CN115924979A - Method for purifying ammonium rhenate - Google Patents
Method for purifying ammonium rhenate Download PDFInfo
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- CN115924979A CN115924979A CN202211421884.9A CN202211421884A CN115924979A CN 115924979 A CN115924979 A CN 115924979A CN 202211421884 A CN202211421884 A CN 202211421884A CN 115924979 A CN115924979 A CN 115924979A
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- HRLYFPKUYKFYJE-UHFFFAOYSA-N tetraoxorhenate(2-) Chemical compound [O-][Re]([O-])(=O)=O HRLYFPKUYKFYJE-UHFFFAOYSA-N 0.000 title claims abstract description 122
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 50
- 238000001816 cooling Methods 0.000 claims abstract description 42
- 239000013078 crystal Substances 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 39
- 238000002425 crystallisation Methods 0.000 claims abstract description 31
- 230000008025 crystallization Effects 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000000967 suction filtration Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000007605 air drying Methods 0.000 claims abstract description 8
- 238000009775 high-speed stirring Methods 0.000 claims description 6
- 238000009826 distribution Methods 0.000 abstract description 18
- 239000000243 solution Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 11
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052702 rhenium Inorganic materials 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000691 Re alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229940098458 powder spray Drugs 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- DECCZIUVGMLHKQ-UHFFFAOYSA-N rhenium tungsten Chemical compound [W].[Re] DECCZIUVGMLHKQ-UHFFFAOYSA-N 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for purifying ammonium rhenate, which comprises the following steps: adding distilled water into low-purity crude ammonium rhenate serving as a raw material, stirring, heating, dissolving, and performing suction filtration to obtain an ammonium rhenate supersaturated solution; introducing the supersaturated solution of ammonium rhenate into a cooling crystallization reactor, mechanically stirring at a high speed by adopting a disc turbine type stirrer, controlling the stirring intensity and the cooling rate, cooling to-10-0 ℃, keeping the temperature in the temperature range, and continuously performing high-speed mechanical stirring to obtain a solid-liquid mixture; and carrying out suction filtration and natural air drying on the obtained solid-liquid mixture to obtain the high-purity ammonium rhenate crystal with micronized particles. The method can effectively realize the controllability of the particle size of the ammonium rhenate crystal, optimize the morphology of the ammonium rhenate crystal, improve the purity of the ammonium rhenate, the uniformity of particle size distribution and the specific surface area, and has good engineering application prospect.
Description
Technical Field
The invention relates to the technical field of rare metal element recovery, in particular to a method for purifying ammonium rhenate.
Background
The ammonium rhenate is an important raw material for preparing rhenium metal powder, and the prepared rhenium powder can be processed into rhenium ingots and rhenium strips and is also an important raw material for alloy series such as tungsten-rhenium alloys, aerospace materials, high-temperature-resistant mechanical equipment parts and the like. In addition, the high-purity rhenium powder prepared by hydrogen reduction of ammonium rhenate has excellent powder performance, is also applied to preparation of rhenium materials in the aerospace field, and is a key high-quality rhenium resource.
In view of the rapid development of metallurgical technology, the traditional crystallization purification method cannot meet the requirement of modern metallurgical technology on the performance of ammonium rhenate powder, and is particularly used as a raw material for preparing high-purity rhenate powder and in the modern metallurgical fields of powder injection molding and powder spray molding. Therefore, improving the purity of ammonium rhenate and realizing the controllability of the particle size and morphology of the ammonium rhenate have important influence on the application effect of the ammonium rhenate in the field of modern metallurgy. At present, the ammonium rhenate crystallization and purification technology cannot realize the controllability of the particle size and the morphology, the macroscopic morphology and the particle size distribution of the purified ammonium rhenate are not uniform, the purity is not high, and the high powder performance requirement of the ammonium rhenate in the field of modern metallurgy cannot be met.
Patent CN201910939501.9 discloses a method for purifying copper smelting crude ammonium rhenate, and pure water-nitric acid-ammonia water is adopted to purify ammonium rhenate. In the prior patent, a large amount of inorganic acid and ammonia water are used in the process of purifying ammonium rhenate, and waste liquid generated in the technical process is difficult to treat.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for purifying ammonium rhenate.
The invention is realized by the following technical scheme.
A method for purifying ammonium rhenate comprises the following steps:
(1) Taking low-purity crude ammonium rhenate as a raw material, gradually adding distilled water under the normal pressure condition, stirring and heating until the crude ammonium rhenate is dissolved, and performing suction filtration to obtain an ammonium rhenate supersaturated solution at the temperature of 120-130 ℃;
(2) Cooling and crystallizing the ammonium rhenate supersaturated solution: introducing the supersaturated solution of ammonium rhenate into a cooling crystallization reactor, mechanically stirring at a high speed by adopting a disc turbine type stirrer, controlling the stirring intensity to be 500-900 rpm, the cooling rate to be 2-4 ℃/min, cooling to-10-0 ℃, keeping the temperature, and continuously performing high-speed mechanical stirring by adopting the disc turbine type stirrer, wherein the stirring intensity is 500-900 rpm, and the stirring time is 8-10 hours, so as to obtain a solid-liquid mixture;
(3) And (3) carrying out suction filtration and natural air drying on the solid-liquid mixture obtained in the step (2) to obtain the high-purity ammonium rhenate crystal with micronized particles.
Further, in the step (1), the purity of the ammonium rhenate is 93-95 wt%.
Further, in the step (1), heating is carried out at a heating rate of 2-3 ℃/min until the crude ammonium rhenate is dissolved.
Further, in the step (2), the temperature is reduced at the speed of 2-4 ℃/min, when the temperature of the system is reduced to 0 ℃, the temperature is kept for crystallization for 1-2 hours, then the temperature of the cooling crystallization reactor is adjusted to-10-0 ℃, and high-speed stirring is continued.
The ammonium rhenate crystal prepared by the method has the advantages of regular morphology, controllable particle size, uniform particle size distribution, large specific surface area and purity higher than 99.99%.
The design mechanism of the invention is as follows:
the method utilizes the characteristic that ammonium rhenate is slightly soluble in cold water, controls the dissolving rate of the ammonium rhenate in water by adjusting the heating rate, and removes insoluble solid impurities by suction filtration to obtain a heat supersaturated solution of the ammonium rhenate; in the crystallization purification process, utilize the powerful shearing force of disc turbine formula agitator, make large granule agglomerate broken under high-speed stirring, the tiny particle after the breakage grows for the ammonium rhenate crystal through the secondary crystallization, control mechanical stirring intensity, cooling rate obtains the even high-purity ammonium rhenate crystal of particle size distribution after the condensation crystallization. The method has the advantages that large-particle crystals can be crushed by the disc turbine type stirrer, the cooling rate is changed to regulate the precipitation rate of the crystals so as to realize purification, the stirring strength is changed to regulate the particle size of ammonium rhenate, and the ammonium rhenate powder with uniform particle size distribution, regular crystal morphology and large specific surface area is obtained.
The invention has the following beneficial effects:
1. the invention adopts a disc turbine type stirrer to crush large-particle agglomerates under high-speed stirring, and the crushed small particles grow into ammonium rhenate crystals through secondary crystallization; mechanical stirring intensity and cooling rate are regulated and controlled, the precipitation rate and particle size of ammonium rhenate crystals are controllable, and the purity, particle uniformity and specific surface area of the ammonium rhenate are improved.
2. According to the method, the low-purity ammonium rhenate is crystallized and purified in the aqueous solution by regulating and controlling the cooling rate, the mechanical stirring strength and the crystallization time within different temperature ranges, so that the high-purity ammonium rhenate crystal with regular macro morphology, uniform particle size distribution, large specific surface area and adjustable particle size is obtained. In the stirring speed range with the stirring intensity of 500-900 rpm, the meso-position diameter of the ammonium rhenate and the stirring intensity are in an inverse proportion rule, and the crystal morphology is changed from irregular agglomerated particles into tetragonal crystals with similar sizes.
3. The method can effectively realize the controllability of the particle size of the ammonium rhenate crystal, optimize the morphology of the ammonium rhenate crystal, improve the purity of the ammonium rhenate, the uniformity of particle size distribution and the specific surface area, and has good engineering application prospect.
Drawings
Fig. 1 is a scanning electron micrograph of ammonium rhenate of example 1.
Fig. 2 is a particle size distribution diagram of ammonium rhenate from example 1.
FIG. 3 is a scanning electron micrograph of ammonium rhenate from example 2.
Fig. 4 is a particle size distribution plot of ammonium rhenate from example 2.
FIG. 5 is a scanning electron micrograph of ammonium rhenate from example 2.
Fig. 6 is a particle size distribution diagram of ammonium rhenate from example 2.
Fig. 7 is a scanning electron micrograph of ammonium rhenate of comparative example 1.
Fig. 8 is a particle size distribution diagram of ammonium rhenate of comparative example 1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
A method for purifying ammonium rhenate comprises the following steps:
(1) Taking crude ammonium rhenate with the purity of 93-95 wt% as a raw material, gradually adding distilled water under the normal pressure condition, stirring and heating at the heating rate of 2-3 ℃/min until the crude ammonium rhenate is dissolved, and performing suction filtration to obtain an ammonium rhenate supersaturated solution with the temperature of 120-130 ℃;
(2) And (3) cooling and crystallizing the ammonium rhenate supersaturated solution: introducing the supersaturated solution of ammonium rhenate into a cooling crystallization reactor for crystallization and purification, performing high-speed mechanical stirring by adopting a disc turbine type stirrer, controlling the stirring intensity to be 500-900 rpm, cooling at the cooling rate of 2-4 ℃/min, keeping the temperature for crystallization for 1-2 hours when the temperature of the system is reduced to 0 ℃, then adjusting the temperature of the cooling crystallization reactor to be-10-0 ℃, keeping the temperature in the temperature range, and continuing performing high-speed mechanical stirring by adopting the disc turbine type stirrer, wherein the stirring intensity is 500-900 rpm, and the stirring time is 8-10 hours, so as to obtain a solid-liquid mixture;
(3) And (3) carrying out suction filtration and natural air drying on the solid-liquid mixture obtained in the step (2) to obtain the high-purity ammonium rhenate crystal with micronized particles.
In above-mentioned step (2), adopt broken large granule agglomerate of disc turbine formula agitator, make large granule agglomerate broken, broken tiny particle passes through secondary crystallization growth to rhenate crystal, can regulate and control the particle size of rhenate through regulation and control mechanical stirring intensity and cooling rate, the speed is appeared out to the rhenate, the impurity compound that the water-solubility is strong stays in the mother liquor, optimize the appearance of rhenate crystal, improve the purity of rhenate, particle size distribution's homogeneity and specific surface area, mechanical stirring intensity is 500 ~ 900rpm within range, rhenate particle size diminishes along with the reinforcing of stirring intensity, the crystal appearance becomes the square crystal that the appearance is close by random glomerate granule.
The ammonium rhenate crystal prepared by the method has the advantages of regular morphology, controllable particle size, uniform particle size distribution and specific surface area of more than 20m 2 The grain median diameter is less than 80um, and the purity is higher than 99.99%.
Example 1
Weighing 300g of low-purity crude ammonium rhenate (with the purity of 93.22 wt%) and placing the crude ammonium rhenate into a container, gradually adding distilled water into the container, fully stirring and heating at the heating rate of 2 ℃/min to dissolve the raw materials, stopping adding distilled water and stopping heating and heating when a little ammonium rhenate solid remains at the bottom of the container, and performing constant-temperature suction filtration to obtain a clear ammonium rhenate thermal supersaturated solution at the temperature of 130 ℃; and introducing the obtained hot supersaturated solution into a cooling crystallization reactor, mechanically stirring and condensing for crystallization by adopting a disc turbine type stirrer, controlling the stirring intensity and the cooling rate, cooling to 0 ℃ at the stirring intensity of 900rpm and the cooling rate of 4 ℃/min, crystallizing for 2 hours under the conditions, keeping the temperature of the cooling crystallization reactor at the temperature, continuously mechanically stirring for 10 hours at 900rpm after adjusting the temperature of the cooling crystallization reactor to be minus 10 ℃, carrying out suction filtration on the obtained material, and naturally air-drying to obtain the ammonium rhenate crystal powder with high-purity micronized particles. The detected median diameter of the ammonium rhenate is 71.17 mu m, and the specific surface area is 26.93m 2 Per kg, the purity is about 99.995%.
Example 2
Weighing 300g of low-purity crude ammonium rhenate (with the purity of 94.72 wt%) and placing the low-purity crude ammonium rhenate into a container, gradually adding distilled water into the container, fully stirring and heating at the heating rate of 2 ℃/min to dissolve the raw materials, stopping adding distilled water and stopping heating and heating when a little ammonium rhenate solid remains at the bottom of the container, and performing constant-temperature suction filtration to obtain a clear ammonium rhenate thermal supersaturated solution at the temperature of 125 ℃; heat obtained is transferred toAnd introducing the supersaturated solution into a cooling crystallization reactor, mechanically stirring and condensing for crystallization by adopting a disc turbine type stirrer, controlling the stirring intensity and the cooling rate, cooling to 0 ℃ at the stirring intensity of 800rpm and the cooling rate of 3 ℃/min, crystallizing for 1.5 hours under the conditions, keeping the temperature at the temperature after regulating the temperature of the reaction kettle to be minus 5 ℃, continuously mechanically stirring for 9 hours at the speed of 800rpm, carrying out suction filtration on the obtained material, and naturally air-drying to obtain the ammonium rhenate crystal powder with high-purity micronized particles. The detected median diameter of the ammonium rhenate is 78.37 mu m, and the specific surface area is 24.56m 2 Per kg, purity of about 99.992%.
Example 3
Weighing 300g of low-purity crude ammonium rhenate (the purity is 93.56 wt%) and placing the raw ammonium rhenate into a container, gradually adding distilled water into the container, fully stirring and heating at the heating rate of 3 ℃/min to dissolve the raw materials, stopping adding the distilled water and heating to raise the temperature after a little ammonium rhenate solid remains at the bottom of the container, and performing suction filtration at constant temperature to obtain a clear ammonium rhenate hot supersaturated solution at the temperature of 120 ℃; and introducing the obtained hot supersaturated solution into a cooling crystallization reactor, mechanically stirring, condensing and crystallizing by adopting a disc turbine type stirrer, controlling the stirring intensity and the cooling rate, cooling to 0 ℃ at the stirring intensity of 700rpm and the cooling rate of 4 ℃/min, crystallizing for 1 hour under the conditions, keeping the temperature at the temperature after adjusting the temperature of the reaction kettle to 0 ℃, continuously mechanically stirring at 700rpm for 8 hours, carrying out suction filtration on the obtained material, and naturally air-drying to obtain the ammonium rhenate crystal powder with high-purity micronized particles. The detected median diameter of the ammonium rhenate is 79.32 mu m, the specific surface area is 23.54m2/kg, and the purity is about 99.990%.
Comparative example 1
Weighing 300g of low-purity crude ammonium rhenate (with the purity of 94.79 wt%) and placing the crude ammonium rhenate into a container, gradually adding distilled water into the container, fully stirring and heating at the heating rate of 2 ℃/min to dissolve the raw materials, stopping adding the distilled water and heating when a little ammonium rhenate solid remains at the bottom of the container, and performing suction filtration at constant temperature to obtain a clear ammonium rhenate heat supersaturated solution; introducing the obtained hot supersaturated solution into a cooling crystallization reactor, cooling and crystallizing without mechanical stirring, wherein the cooling rate is 1 ℃/min,and cooling to-10 ℃, crystallizing for 12 hours, carrying out suction filtration on the obtained solid-liquid mixture, and naturally air-drying to obtain ammonium rhenate crystal powder. The detected median diameter of the ammonium rhenate is 218.6 mu m, and the specific surface area is 9.636m 2 Kg, purity about 97.87%.
As can be seen from the scanning electron microscope images (fig. 1, 3, 5) and the particle size distribution diagrams (fig. 2, 4, 6) of the cooling crystallization ammonium rhenate crystals in examples 1 to 3 and comparative example 1, the present invention can crush large particle agglomerates under high-speed stirring, and the crushed small particles grow into ammonium rhenate crystals through secondary crystallization; by adjusting the stirring intensity and the cooling rate, the crystal granularity is reduced, the uniformity of the granularity distribution is enhanced, the specific surface area is increased, the purity is improved, and the crystal morphology is changed from irregular agglomerated crystals into regular tetragonal crystals.
The particle size of the ammonium rhenate obtained in examples 1-3 is reduced along with the increase of stirring intensity, the ammonium rhenate obtained in comparative example 1 has a relatively uniform particle size distribution rule, the obtained powder has a relatively large specific surface area and relatively high purity, and the ammonium rhenate obtained in comparative example 1 has non-uniform particle size, irregular crystal morphology and relatively low purity compared with examples 1-3.
According to the experimental result, the method is applied to carry out crystallization and purification on the low-purity coarse ammonium rhenate, large-particle agglomerates are crushed under high-speed stirring, and the crushed small particles grow into ammonium rhenate crystals through secondary crystallization; the particle size of the ammonium rhenate crystals can be controlled, the morphology of the ammonium rhenate crystals is optimized, and the purity, the uniformity of particle size distribution and the specific surface area of the ammonium rhenate are improved.
According to the method, the particle size of the ammonium rhenate crystals can be effectively controlled, the morphology of the ammonium rhenate crystals is optimized, the purity of the ammonium rhenate, the uniformity of particle size distribution and the specific surface area are improved, and the method has a good engineering application prospect.
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. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (4)
1. The method for purifying the ammonium rhenate is characterized by comprising the following steps of:
(1) Taking low-purity ammonium rhenate as a raw material, adding distilled water under normal pressure, stirring and heating until the ammonium rhenate is dissolved, and performing suction filtration to obtain an ammonium rhenate supersaturated solution at the temperature of 120-130 ℃;
(2) Cooling and crystallizing the ammonium rhenate supersaturated solution: introducing the supersaturated solution of the ammonium rhenate into a cooling crystallization reactor, carrying out high-speed mechanical stirring by adopting a disc turbine type stirrer, controlling the stirring intensity to be 500-900 rpm, cooling the solution at the rate of 2-4 ℃/min to-10-0 ℃, keeping the temperature, and continuing carrying out high-speed mechanical stirring by adopting the disc turbine type stirrer, wherein the stirring intensity is 500-900 rpm, and the stirring time is 8-10 hours, so as to obtain a solid-liquid mixture;
(3) And (3) carrying out suction filtration and natural air drying on the solid-liquid mixture obtained in the step (2) to obtain the high-purity ammonium rhenate crystal with micronized particles.
2. The method for purifying ammonium rhenate according to claim 1, wherein in the step (1), the purity of the ammonium rhenate is 93-95 wt%.
3. The method for purifying ammonium rhenate, according to claim 1, wherein in the step (1), heating is carried out at a heating rate of 2-3 ℃/min until the crude ammonium rhenate is dissolved.
4. The method for purifying ammonium rhenate according to claim 1, wherein in the step (2), the temperature is reduced at a rate of 2-4 ℃/min, when the temperature of the system is reduced to 0 ℃, the temperature is kept for crystallization for 1-2 hours, then the temperature of a cooling crystallization reactor is adjusted to-10-0 ℃, and high-speed stirring is continued.
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- 2022-11-14 CN CN202211421884.9A patent/CN115924979A/en active Pending
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