CN115026297B - High-purity rhenium powder and preparation process thereof - Google Patents
High-purity rhenium powder and preparation process thereof Download PDFInfo
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- CN115026297B CN115026297B CN202210492495.9A CN202210492495A CN115026297B CN 115026297 B CN115026297 B CN 115026297B CN 202210492495 A CN202210492495 A CN 202210492495A CN 115026297 B CN115026297 B CN 115026297B
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- purity
- rhenium
- rhenium powder
- perrhenic acid
- powder
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- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- QSHYGLAZPRJAEZ-UHFFFAOYSA-N 4-(chloromethyl)-2-(2-methylphenyl)-1,3-thiazole Chemical compound CC1=CC=CC=C1C1=NC(CCl)=CS1 QSHYGLAZPRJAEZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052702 rhenium Inorganic materials 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 7
- HRLYFPKUYKFYJE-UHFFFAOYSA-N tetraoxorhenate(2-) Chemical compound [O-][Re]([O-])(=O)=O HRLYFPKUYKFYJE-UHFFFAOYSA-N 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000005342 ion exchange Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 238000010926 purge Methods 0.000 claims description 3
- 239000012492 regenerant Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000000227 grinding Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000004886 process control Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of powder metallurgy, and provides a preparation process of high-purity rhenium powder, which comprises the following steps: s1, preparing high-purity perrhenic acid; s2, feeding the high-purity perrhenic acid obtained in the step S1 into a jet reaction furnace to obtain high-purity rhenium powder; the preparation process provided by the invention is characterized in that the primary rhenium-containing product is purified and converted into perrhenic acid, and then the perrhenic acid is used as an intermediate to prepare high-purity rhenium powder through direct hydrogen reduction, and the process is short, does not need grinding, and has high process control degree, high product purity and stable quality; the recovery rate of rhenium metal is high; has the advantages of obvious environmental protection advantage, low cost and the like.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to high-purity rhenium powder and a preparation process thereof.
Background
The traditional method for preparing the rhenium powder mainly comprises the steps of dissolving, purifying, crystallizing, filtering and drying the primary ammonium rhenate with low purity to prepare ammonium rhenate with higher purity, grinding and sieving the ammonium rhenate, and reducing the ammonium rhenate with hydrogen. The traditional method for preparing the rhenium powder needs to purify and crystallize primary ammonium rhenate or potassium rhenate to form ammonium rhenate solid, then the ammonium rhenate solid is dried and ground into powder with small granularity, and then the powder is reduced, filtered, dried, ground, screened and the like, so that the metal recovery rate is low due to long flow and the cost is high; the probability of introducing impurities in the process of the same-time long flow is high, and the purity of the obtained rhenium powder is often influenced by process control. In addition, auxiliary materials such as ammonia and the like are required to be used for purifying ammonium rhenate, and the process has high environmental protection risk.
Content of the application
The invention provides high-purity rhenium powder and a preparation process thereof, which can effectively solve the problems.
The embodiment of the invention is realized by the following technical scheme:
a preparation process of high-purity rhenium powder comprises the following steps:
s1, preparing high-purity perrhenic acid;
s2, feeding the high-purity perrhenic acid obtained in the step S1 into a jet reaction furnace to obtain high-purity rhenium powder.
The preparation process of the high-purity rhenium powder provided by the invention has the following beneficial effects:
the preparation process provided by the invention is characterized in that the primary rhenium-containing product is purified and converted into perrhenic acid, and then the perrhenic acid is used as an intermediate to prepare high-purity rhenium powder through direct hydrogen reduction, and the process is short, does not need grinding, and has high process control degree, high product purity and stable quality; the recovery rate of rhenium metal is high; has the advantages of obvious environmental protection advantage, low cost and the like. The process for preparing the high-purity rhenium powder has the advantages that:
(1) The purity requirement of the raw materials for preparing perrhenic acid is low, and the impurity removal effect is good;
(2) The process flow is short, the working procedures of filtering, drying, grinding, sieving and the like are not needed, the process control degree is high, and the product quality is stable; the recovery rate of rhenium metal is high;
(3) The method has few varieties of auxiliary materials; ammonia water is not introduced, ammonia gas or nitrogen gas is not generated to pollute hydrogen gas, the hydrogen gas can be recycled, the process has no three wastes, and the environmental protection advantage is obvious;
(4) The equipment is automatically controlled, the operation is continuous, the cost is greatly reduced, and the method has good engineering application value and economic value.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an electron microscope scan of the high purity rhenium powder provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The specific embodiment provides a preparation process of high-purity rhenium powder, which comprises the following steps:
s1, preparing high-purity perrhenic acid;
s2, feeding the high-purity perrhenic acid obtained in the step S1 into a jet reaction furnace to obtain high-purity rhenium powder.
In step S1, the method specifically includes:
s11, dissolving a rhenium primary product in water to obtain rhenium dissolution liquid;
s12, pumping the rhenium solution obtained in the step S11 into an ion exchange column for adsorption to obtain column outlet liquid with the pH value less than or equal to 1.5;
and S13, concentrating the column liquid obtained in the step S12 until the rhenium concentration is not less than 280g/l, and stopping concentrating to obtain the concentrated liquid which is the high-purity perrhenic acid.
Wherein, in step S11, the primary rhenium product is ammonium rhenate, potassium rhenate or sodium rhenate.
Wherein, in step S12, an H-type ion exchange resin with model number C180 or 001 x 8 is loaded in an ion exchange column.
In step S12, the regenerant used in the ion exchange process is GR grade hydrochloric acid, and the resistivity of the washing water is 18.25mΩ·cm.
In the step S13, the negative pressure is minus 0.03 to minus 0.08MPa, and the temperature is 40-90 ℃.
Wherein, in step S2, the steps of:
s21, heating the jet reaction furnace, and introducing hydrogen after purging with nitrogen;
s22, feeding the high-purity perrhenic acid into a jet reaction furnace.
In step S21, the temperature in the jet reaction furnace is 600-950 ℃, and the flow rate of hydrogen is 2-10L/min.
In step S22, the flow rate of the high-purity perrhenic acid is 0.1-1L/min.
The inside of the furnace body of the jet reaction furnace is made of pure rhenium metal materials, the furnace body consists of a feed end, an air outlet, a liquid-gas reaction section, a gas-solid reaction section, an air inlet, a discharge end and the like, and the outside of the furnace is electrically heated.
Wherein, the main reactions in the jet reaction furnace are as follows:
2HReO 4 =Re 2 O 7 +H 2 O
Re 2 O 7 +3H 2 =2ReO 2 +3H 2 O
ReO 2 +2H 2 =Re+2H 2 O。
example 1
The embodiment is used for preparing high-purity rhenium powder, and comprises the following steps of:
s1, preparing high-purity perrhenic acid;
s11, dissolving ammonium rhenate in water to obtain rhenium dissolution liquid;
s12, pumping rhenium solution obtained in the step S11 into an ion exchange column filled with ion exchange resin with the model of C180 for adsorption, wherein a regenerant adopted in the ion exchange process is GR-grade hydrochloric acid, the resistivity of washing water is 18.25MΩ &.CM, and H-type ion exchange resin is filled in the ion exchange column to obtain column outlet liquid with the pH value less than or equal to 1.5;
s13, concentrating the column liquid obtained in the step S12, wherein the negative pressure is minus 0.06 to minus 0.07MPa, the temperature is 75 ℃, and the concentration is stopped until the concentration of rhenium is 312g/l, so that the concentrated liquid is high-purity perrhenic acid;
s2, feeding the high-purity perrhenic acid obtained in the step S1 into a jet reaction furnace to obtain rhenium powder with purity higher than 99.999%.
S21, heating the jet reaction furnace to 680 ℃, and then introducing hydrogen after purging with nitrogen, wherein the flow rate of the hydrogen is 3L/min;
s22, feeding the high-purity perrhenic acid into a jet reaction furnace, wherein the flow rate of the high-purity perrhenic acid is 0.1L/min.
Experimental example
The component content of the high purity rhenium powder prepared in example 1 was measured by glow discharge apparatus (GDMS), and the results are shown in table 1 below:
TABLE 1 determination of the content of high purity rhenium powder component GDMS (unit ppm wt) in example 1
Wherein, the purity of the rhenium powder is Re= 99.99965%.
The high purity rhenium powder in example 1 was then examined by electron microscopy, if 1 is indicated.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The preparation process of the high-purity rhenium powder is characterized by comprising the following steps of:
s1, preparing high-purity perrhenic acid:
s11, dissolving a rhenium primary product in water to obtain rhenium dissolution liquid;
s12, pumping the rhenium solution obtained in the step S11 into an ion exchange column for adsorption to obtain column outlet liquid with the pH value less than or equal to 1.5;
s13, concentrating the column liquid obtained in the step S12 until the rhenium concentration is not less than 280g/l, and stopping concentrating to obtain a concentrated solution which is high-purity perrhenic acid;
s2, feeding the high-purity perrhenic acid obtained in the step S1 into a jet reaction furnace to obtain high-purity rhenium powder:
s21, heating the jet reaction furnace to 600-950 ℃, and then introducing hydrogen after purging with nitrogen, wherein the flow rate of the hydrogen is 2-10L/min;
s22, feeding the high-purity perrhenic acid into a jet reaction furnace, wherein the flow rate of the high-purity perrhenic acid is 0.1-1L/min, and reacting to obtain the high-purity rhenium powder.
2. The process for preparing high purity rhenium powder according to claim 1, wherein in step S11, the primary rhenium product is ammonium rhenate, potassium rhenate, or sodium rhenate.
3. The process for preparing high purity rhenium powder according to claim 1, wherein in step S12, an H-type ion exchange resin of model C180 or 001 x 8 is loaded in an ion exchange column.
4. The process for preparing high purity rhenium powder according to claim 1, wherein in step S12, the regenerant used in the ion exchange process is GR-grade hydrochloric acid, and the resistivity of the wash water is 18.25mΩ.
5. The process for preparing high purity rhenium powder according to claim 1, wherein in step S13, the negative pressure is-0.03 to-0.08 MPa and the temperature is 40 to 90 ℃.
6. A high purity rhenium powder produced by the process of any one of claims 1-5, wherein the high purity rhenium powder has a purity greater than 99.999% and a D90 of 50 microns or less.
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|---|---|---|---|---|
| US6102979A (en) * | 1998-08-28 | 2000-08-15 | The United States Of America As Represented By The United States Department Of Energy | Oxide strengthened molybdenum-rhenium alloy |
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2022
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