CN107052357A - A kind of preparation method of high-purity rhenium powder - Google Patents
A kind of preparation method of high-purity rhenium powder Download PDFInfo
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- CN107052357A CN107052357A CN201710234499.6A CN201710234499A CN107052357A CN 107052357 A CN107052357 A CN 107052357A CN 201710234499 A CN201710234499 A CN 201710234499A CN 107052357 A CN107052357 A CN 107052357A
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Classifications
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- 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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Abstract
The invention discloses a kind of preparation method of high-purity rhenium powder, comprise the following steps：Purification, once centrifugal atomizing, the step such as reduction, secondary reduction.A kind of preparation method of high-purity rhenium powder is provided, from raw material ammonium rhenate powder end preparation start with the big technique of rehenic acid ammonium calcining reduction two, improve ammonium rhenate powder end reducibility, reduce powder grow up motive power, accomplish that each stage material purity is controllable；Using two benches hydrogen reducing, increase the contact with hydrogen, be conducive to the exclusion of vapor, favourable conditions are provided to obtain fine particle size, powder evenly.
Description
Technical field
The present invention relates to Rare Metals Materials field, in particular to a kind of system of the efficient, high-purity rhenium powder of soilless sticking
Preparation Method.
Background technology
Rhenium fusing point is up to 3180 DEG C, is only second to tungsten, and its antiacid caustic corrosion is strong, not oxidized in atmosphere.Rhenium is used as one
Kind rare refractory material, shakes performance and splendid creep-resistant property with superior thermal, under larger thermal expansion, does not occur machine
Tool is damaged, and is widely used in heating element heater, high temperature alloy and high temperature corrosion-resisting coating etc..Because the fusing point of rhenium is very high, prepare
Pure rhenium material typically uses powder metallurgy process, i.e., do raw material using rhenium powder, is obtained by compacting, sintering, calendering processing.It is special
It is not when preparing rhenium alloys, to be mixed with using rhenium powder with other powder, tiny, the few composition of obtained rhenium alloys grain size is inclined
Analysis, is that other method of smelting can not compare.
In recent years, due to breakthrough of China's aero-engine with the technology of preparing of rhenium-containing nickel base superalloy, also have and partly lead
Body material, high-end thermodynamic material, the market demand increase of petroleum refining, greatly expand the market application of high-purity rhenium.Traditional height
Pure rhenium powder is typically obtained using high-purity rehenic acid ammonium calcining reduction, and specific practice is：The grinding of rehenic acid ammonium is broken, in hydrogen atmosphere
Calcining reduction obtains rhenium powder, then grinds the broken rhenium powder for obtaining suitable particle size and being distributed so that the duration in later stage is than making reaction
Time will be grown a lot.Such a method, also in the presence of some drawbacks.First, rehenic acid ammonium ball milling takes time and effort and introduces impurity；Second,
There is also the possibility of easy impurity in rhenium sphere of powder mill, the rhenium powder after ball milling is made in offset flat shape and in the presence of obvious processing hardening
Shaped and processing into follow-up pressed compact the problems such as apparent density of powder is low, suppression performance is poor, is had a strong impact on.
The rhenium Powder Particle Size prepared to top method is general relatively thick, and the primary particle existed is very more, between particle with
Metallurgical binding form is present, the application performance of extreme influence powder.In general, rhenium powder mainly has three kinds long in reduction process
Big mechanism：Volatilization-deposition grows up, sinters collective recrystallization and grow up and grown up with redox.Wherein, first two mechanism of growing up accounts for master
Lead mechanism.Volatilization-deposition mechanism of growing up is：During reduction, rhenium oxide volatilization combines to form vaporous water with vapor
Oxide is closed, and is reduced with gas phase in hydrogen atmosphere, the rhenium after reduction deposits to unreduced oxygen with atomic form
Compound or as-reduced rhenium powder particles surface, so that rhenium powder particles are grown up.Sintering collective recrystallization mechanism of growing up is：With also
The rise of former temperature, the extension of recovery time, the rhenium powder particles contacted with each other gradually spread under high temperature action, are formed between particle
Neck is sintered, the contact of rhenium powder is ultimately resulted in and is changed into crystal grain boundary, form second particle.In production, when typically being reduced by adjusting
Agglomeration of the hydrogen flowing quantity with reduction temperature to adjust rhenium Powder Particle Size and solve presence, but in actual effect less, because
State for rhenium Powder Particle Size also with ammonium rhenate powder end is closely bound up.
How solving poly- rhenium powder ball, reduction process flow, improving powder purity is the problem to be solved in the present invention.This case will
Start with from the preparation at raw material ammonium rhenate powder end with the big technique of rehenic acid An calcining reductions two, improve the reducible of ammonium rhenate powder end
Property, reduction powder grow up motive power, accomplish that each stage material purity is controllable.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of high-purity rhenium powder, from the preparation at raw material ammonium rhenate powder end with
The big technique of rehenic acid ammonium calcining reduction two is started with, improve the reducibility at ammonium rhenate powder end, reduction powder grow up motive power, accomplish each
Stage material purity is controllable.
To realize object above, the technical solution adopted by the present invention is：A kind of preparation method of high-purity rhenium powder, including it is as follows
Step：
（A）Purification, Ammonium rhenate solution is purified, its purity is more than 99.99%；
（B）Centrifugal atomizing, is pumped Ammonium rhenate solution to spray drying top of tower with quantitative terms with the chemical pump of acid and alkali-resistance
Centrifugal atomizer, centrifugal atomizer rotating speed collects the ammonium rhenate powder end of bottom between 12000-20000rad/min；
（C）Ammonium rhenate powder end is loaded in high-purity corundum boat, inversely logical hydrogen reduction obtains dark brown rhenium dioxide powder；
（D）Rhenium dioxide is suitably fiddled with to loose, is reloaded into boat, reverse logical hydrogen reduction obtains the rhenium powder of Dark grey.
It is preferred that, the concentration of Ammonium rhenate solution is 70-150g/L.
It is preferred that, the centrifugal atomizing in the step B, rotating speed is between 12000-18000rad/min, centrifugal atomizing mist formation
It is 250-320 DEG C, preferably 250-270 to change thermal current operating temperature in liquid, atomized liquid and high-temperature hot air counter current contact in tower, tower
DEG C, evaporative crystallization obtains ammonium rhenate powder end.
It is preferred that, the step（B）In, the particle mean size at ammonium rhenate powder end is 2-12um.
It is preferred that, the step（C）In, boat charge 0.8-1.2kg pushes away boat speed 20-35min/ times, goes back protohydrogen temperature control
System is in 350-420 DEG C, hydrogen flowing quantity 3-5m3/h.
It is preferred that, the step（D）In, boat charge 1-1.5kg pushes away boat speed 30-40min/ times, hydrogen flowing quantity, 5-7m
3/h, 720-790 DEG C of reduction temperature.
Beneficial effects of the present invention：
1st, ammonium rhenate powder end is prepared using centrifugal atomizing drying, reduces equipment investment, raise labour productivity, powder is actual to be received
Collection rate is up to more than 99%.
2nd, ammonium rhenate powder end can once be obtained by being dried with above method, and ammonium rhenate powder end is not present agglomeration and dredged
Pine, by adjust solution concentration, atomizing disk rotating speed, atomized soln flow to reach the purpose of the last granularity of regulation ammonium rhenate powder；
In reduction, under oxygen free condition, using two benches hydrogen reducing, increase the contact with hydrogen, be conducive to the exclusion of vapor, be
Obtain fine particle size, powder evenly and favourable conditions are provided.
3rd, in whole technical process, container, pump, the centrifugal atomizing disk contacted with the persursor material of rhenium is corrosion-resistant
The material that material, wherein container and pump are used for polytetrafluoroethylene (PTFE), centrifugal atomizing disk material be titanium alloy, boat be it is high-purity just
Jade, largely ensures the purity of gained rhenium powder, and powder purity can reach more than 99.995%.
4th, powder mean particle sizes are between 0.3-10 μm, and this method may not only be applied to prepare ultrafine particle powder, can also prepare
Regular particle size powder.Reunion is not present in powder and primary particle is seldom, it is not necessary to grind, and directly screening is with regard to that can obtain being adapted to work
The powder of skill granularity, and oversize is minimum.
Embodiment
In order that those skilled in the art more fully understand technical scheme, the present invention is retouched in detail below
State, the description of this part is only exemplary and explanatory, there should not be any restriction effect to protection scope of the present invention.
Embodiment 1：
After 100L Ammonium rhenate solutions are purified, purity is more than 99.995%, then suitably adjusts high-purity Ammonium rhenate solution pH value,
Wherein rehenic acid ammonium concentration is 70g/L；
Ammonium rhenate solution is pumped to spray drying tower by evaporative crystallization, feeding speed 7kg/h, rotating disk speed by pump
Thermal current operating temperature is 250 DEG C or so in 18000r/min, tower.The particle mean size of obtained rehenic acid ammonium is 2.6um, rehenic acid ammonium
Purity reaches 99.998%, and powder collection rate reaches 99%.This method is made using atomizing disk of corrosion-resistant material, rather than is adopted
With stainless steel, there is certain corrosivity to stainless steel because Ammonium rhenate solution has under alkalescent, thermosol liquid status, be easily introduced
The metal impurities such as Fe, Cr, Ni.In addition, the inwall that spray drying chamber, collecting tank and each cyclone ducts are contacted with rehenic acid ammonium
Using polytetrafluorethylecoatings coatings, the coating high temperature resistant is good, small with powder adherent, it is possible to decrease powder contaminative, improves powder and receives
Collection rate etc..Above measure, it is ensured that the purity of rehenic acid ammonium in whole drying process, the appearance of pollution sources is just controlled in source.
Dried ammonium rhenate powder end is directly loadable into high-purity corundum boat without sieving, boat charge 0.8kg, pushes away boat speed
Degree 30min/ times, hydrogen flowing quantity 5m3/h, 350 DEG C of reduction temperature, logical hydrogen reduction obtains rhenium dioxide powder.Due to seven oxidations two
Rhenium high volatility, it is necessary to shorten the period under the conditions of the temperature and atmosphere of its presence.Reduction process is as follows：
NH4ReO4(s)=HReO4(s)+NH3(g)
2HReO4(s)=Re2O7(s)+H2O(g)
Re2O7(s)+3H2(g)=2ReO2(s)+3H2O(g) （Note：ReO3 will not be formed when hydrogen flowing quantity is increased）
Rhenium dioxide is reloaded into boat, boat charge 1kg pushes away boat speed 30min/ times, hydrogen flowing quantity 7m3/h, reduction temperature
790 DEG C, lead to hydrogen reduction and obtain rhenium powder.Reduction process is as follows：ReO2(s)+2H2(g)=Re(s)+2H2O(g).
Obtained rhenium powder particle mean size is 0.5 μm, and purity is up to 99.995%.
Embodiment 2
A certain amount of rehenic acid crystalline ammonium particle is added in high-purity Ammonium rhenate solution after by purification and is heated, PH is to 9 for regulation,
Wherein rehenic acid ammonium concentration is 150g/L, and purity is more than 99.999%.
Ammonium rhenate solution is pumped to spray drying tower by evaporative crystallization, feeding speed 13kg/h, rotating disk speed by pump
It is 270 DEG C or so to spend thermal current operating temperature in 12000r/min, tower.The particle mean size of obtained rehenic acid ammonium is 12um.Will be dry
Ammonium rhenate powder end after dry is directly loadable into high-purity corundum boat without sieving, and boat charge 1.2kg pushes away boat speed 35min/ times,
Hydrogen flowing quantity 3.5m3/h, 420 DEG C of reduction temperature, logical hydrogen reduction obtains rhenium dioxide powder.
Rhenium dioxide is reloaded into boat, boat charge 1.5kg pushes away boat speed 40min/ times, hydrogen flowing quantity, 7m3/h, also
Former 720 DEG C of temperature, leads to hydrogen reduction and obtains rhenium powder.Obtained rhenium powder particle mean size is 8.3 μm, and purity is up to 99.999%, oxygen content
Less than 600PPM.
It should be noted that herein, term " comprising ", "comprising" or its any other variant are intended to non-row
His property is included, so that process, method, article or equipment including a series of key elements not only include those key elements, and
And also including other key elements being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.
Specific case used herein is set forth to the principle and embodiment of the present invention, the explanation of above example
It is only intended to the method and its core concept for helping to understand the present invention.Described above is only the preferred embodiment of the present invention, should
When pointing out due to the finiteness of literal expression, and objectively there is unlimited concrete structure, for the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, can also make it is some improve, retouching or change, can also be by
Above-mentioned technical characteristic is combined by rights；These improve retouching, change or combined, or the not improved structure by invention
Think and technical scheme directly applies to other occasions, be regarded as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of high-purity rhenium powder, it is characterised in that comprise the following steps：
（A）Purification, Ammonium rhenate solution is purified, its purity is more than 99.99%；
（B）Centrifugal atomizing, is pumped Ammonium rhenate solution to spray drying top of tower with quantitative terms with the chemical pump of acid and alkali-resistance
Centrifugal atomizer, centrifugal atomizer rotating speed collects the ammonium rhenate powder end of bottom between 12000-20000rad/min；
（C）Once reduce, ammonium rhenate powder end is loaded in high-purity corundum boat, inversely logical hydrogen reduction obtains dark brown rhenium dioxide
Powder；
（D）Secondary reduction, rhenium dioxide is suitably fiddled with loose, is reloaded into boat, and reverse logical hydrogen reduction obtains Dark grey
Rhenium powder.
2. a kind of preparation method of high-purity rhenium powder according to claim 1, it is characterised in that the concentration of Ammonium rhenate solution is
70-150g/L。
3. a kind of preparation method of high-purity rhenium powder according to claim 1, it is characterised in that the centrifugation in the step B
Atomization, rotating speed connects between 12000-18000rad/min, centrifugal atomizing into atomized liquid, atomized liquid with high-temperature hot air convection current in tower
Touch, thermal current operating temperature is 250-320 DEG C in tower, and preferably 250-270 DEG C, evaporative crystallization obtains ammonium rhenate powder end.
4. a kind of preparation method for the high-purity rhenium powder stated according to claim 1, it is characterised in that the step（B）In, rehenic acid ammonium
The particle mean size of powder is 2-12um.
5. a kind of preparation method of high-purity rhenium powder according to claim 1, it is characterised in that the step（C）In, fill boat
0.8-1.2kg is measured, boat speed is pushed away 20-35min/ times, goes back protohydrogen temperature control in 350-420 DEG C, hydrogen flowing quantity 3-5m3/h.
6. a kind of preparation method of high-purity rhenium powder according to claim 1, it is characterised in that the step（D）In, fill boat
1-1.5kg is measured, boat speed is pushed away 30-40min/ times, hydrogen flowing quantity, 5-7m3/h, 720-790 DEG C of reduction temperature.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107838431A (en) * | 2017-11-16 | 2018-03-27 | 重庆材料研究院有限公司 | A kind of spherical rhenium powder, preparation method thereof |
| CN108480621A (en) * | 2018-04-26 | 2018-09-04 | 航天材料及工艺研究所 | A method of shaping rhenium component using spherical rhenium powder |
| CN109351985A (en) * | 2018-10-19 | 2019-02-19 | 浙江工业大学 | A kind of method that Hydrothermal Pressure Hydrogen Reduction prepares rhenium metal powder |
| CN109773206A (en) * | 2019-03-29 | 2019-05-21 | 中国科学院金属研究所 | A kind of ultrapure superfine rhenium powder and preparation method thereof |
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
| CN111517368A (en) * | 2020-07-03 | 2020-08-11 | 北矿新材科技有限公司 | Method for purifying ammonium rhenate, purified ammonium rhenate and method for preparing metal rhenium or rhenium alloy |
| CN111872409A (en) * | 2020-07-29 | 2020-11-03 | 铜陵铜冠优创特种材料有限公司 | Production process of high-purity aviation-grade rhenium particles |
| CN113857488A (en) * | 2021-08-18 | 2021-12-31 | 西北矿冶研究院 | Method for preparing high-purity superfine rhenium powder by using ammonium perrhenate |
| CN114309631A (en) * | 2021-12-31 | 2022-04-12 | 湖南元极新材料有限公司 | Rhenium powder preparation method |
| CN114397153A (en) * | 2021-12-16 | 2022-04-26 | 国合通用测试评价认证股份公司 | Preparation method and application of high-purity rhenium standard sample for GD-MS component analysis |
| CN114619037A (en) * | 2022-01-31 | 2022-06-14 | 北京科技大学 | Preparation method of sintered rhenium plate |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107838431A (en) * | 2017-11-16 | 2018-03-27 | 重庆材料研究院有限公司 | A kind of spherical rhenium powder, preparation method thereof |
| CN108480621A (en) * | 2018-04-26 | 2018-09-04 | 航天材料及工艺研究所 | A method of shaping rhenium component using spherical rhenium powder |
| CN109351985B (en) * | 2018-10-19 | 2021-08-10 | 浙江工业大学 | Method for preparing metal rhenium powder by hydrothermal hydrogen reduction |
| CN109351985A (en) * | 2018-10-19 | 2019-02-19 | 浙江工业大学 | A kind of method that Hydrothermal Pressure Hydrogen Reduction prepares rhenium metal powder |
| CN109773206A (en) * | 2019-03-29 | 2019-05-21 | 中国科学院金属研究所 | A kind of ultrapure superfine rhenium powder and preparation method thereof |
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
| CN111517368B (en) * | 2020-07-03 | 2020-10-02 | 北矿新材科技有限公司 | Method for purifying ammonium rhenate, purified ammonium rhenate and method for preparing metal rhenium or rhenium alloy |
| CN111517368A (en) * | 2020-07-03 | 2020-08-11 | 北矿新材科技有限公司 | Method for purifying ammonium rhenate, purified ammonium rhenate and method for preparing metal rhenium or rhenium alloy |
| CN111872409A (en) * | 2020-07-29 | 2020-11-03 | 铜陵铜冠优创特种材料有限公司 | Production process of high-purity aviation-grade rhenium particles |
| CN111872409B (en) * | 2020-07-29 | 2024-01-16 | 铜陵铜冠优创特种材料有限公司 | Production process of high-purity aviation-grade rhenium particles |
| CN113857488A (en) * | 2021-08-18 | 2021-12-31 | 西北矿冶研究院 | Method for preparing high-purity superfine rhenium powder by using ammonium perrhenate |
| CN113857488B (en) * | 2021-08-18 | 2023-11-14 | 西北矿冶研究院 | Method for preparing high-purity superfine rhenium powder by using ammonium perrhenate |
| CN114397153A (en) * | 2021-12-16 | 2022-04-26 | 国合通用测试评价认证股份公司 | Preparation method and application of high-purity rhenium standard sample for GD-MS component analysis |
| CN114309631A (en) * | 2021-12-31 | 2022-04-12 | 湖南元极新材料有限公司 | Rhenium powder preparation method |
| CN114309631B (en) * | 2021-12-31 | 2024-01-16 | 湖南元极新材料有限公司 | Preparation method of rhenium powder |
| CN114619037A (en) * | 2022-01-31 | 2022-06-14 | 北京科技大学 | Preparation method of sintered rhenium plate |
| CN114619037B (en) * | 2022-01-31 | 2023-09-01 | 北京科技大学 | Preparation method of sintered rhenium plate |
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Application publication date: 20170818 |