CN102992407B - Ammonium rhenate solution crystallization method - Google Patents
Ammonium rhenate solution crystallization method Download PDFInfo
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- CN102992407B CN102992407B CN201110267640.5A CN201110267640A CN102992407B CN 102992407 B CN102992407 B CN 102992407B CN 201110267640 A CN201110267640 A CN 201110267640A CN 102992407 B CN102992407 B CN 102992407B
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- acid ammonium
- rehenic acid
- ammonium rhenate
- ammonium solution
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Abstract
The invention provides an ammonium rhenate solution crystallization method. The technical scheme of the invention is characterized in that the method comprises the following steps: 1, placing an ammonium rhenate solution having a temperature of 30-90DEG C and a concentration of not less than 15g/L in an open container, wherein the ammonium rhenate solution is obtained after evaporating concentration; 2, adding a substance which can hydrolyze to generate NH4<+> into the ammonium rhenate solution in order to adjust the pH value of the ammonium rhenate solution to 8-11, wherein the substance is ammonia water; 3, blowing the ammonium rhenate solution by a wind source commonly used in the industry in order to cool the ammonium rhenate solution to room temperature, and preliminarily crystallizing the ammonium rhenate solution in the cooling process; 4, cooling the ammonium rhenate solution in an environment having a temperature of -10-0DEG C for above 6h; and 5, taking the ammonium rhenate solution out of the environment, and carrying out solid-liquid separation to obtain crude ammonium rhenate. The ammonium rhenate solution crystallization method has the advantages of crystallization efficiency improvement and ammonium rhenate product output improvement.
Description
Technical field
The present invention relates to a kind of technique of wet production rehenic acid ammonium, relate in particular to a kind of rehenic acid ammonium solution crystallization method, belong to technical field of wet metallurgy.
Background technology
In wet production rehenic acid ammonium technique, the crystallization method of traditional rehenic acid ammonium solution is, adopt water quench or by the mode of gas blower blast-cold, evaporation concentration to the rehenic acid ammonium solution after finite concentration is carried out to crystallisation by cooling, thereby carry out afterwards solid-liquid separation, obtain rehenic acid ammonium product.The shortcoming of this crystallization method is that the rehenic acid ammonium product production obtaining is low.
Summary of the invention
The invention provides a kind of rehenic acid ammonium solution crystallization method, solve the problem of above-mentioned existence.
Technical scheme of the present invention is: a kind of rehenic acid ammonium solution crystallization method, comprises following methods step: by the temperature after evaporation concentration, be a) that 30 ℃～90 ℃, the rehenic acid ammonium solution of concentration>=15g/L are placed in open container; B) to adding in rehenic acid ammonium solution to be hydrolyzed, produce NH
4 +material, the pH value of rehenic acid ammonium solution is adjusted to 8～11; C) the conventional wind regime of use industry is by the blast-cold of rehenic acid ammonium solution to room temperature, and rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) it is cooling under the environment of-10 ℃～0 ℃ rehenic acid ammonium solution being put into temperature, and be more than 6 hours cooling time; E) take out rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.Above-mentioned can hydrolysis produces NH
4 +material be ammoniacal liquor.
The invention has the beneficial effects as follows: due in crystallisation process, NH
4 +can produce common-ion effcet with rehenic acid ammonium solution, and in described crystalline environment, promote the degree of depth of crystallization to carry out, thereby improve crystalline rate, improve rehenic acid ammonium product production.
Embodiment
The embodiment of the present invention is below described in detail in detail.
Embodiment 1:a) by the temperature after evaporation concentration, be that the rehenic acid ammonium solution that 30 ℃, concentration are 15g/L is placed in open container; B) in rehenic acid ammonium solution, add ammoniacal liquor, the pH value of rehenic acid ammonium solution is adjusted to 8; C) with gas blower by the blast-cold of rehenic acid ammonium solution to room temperature, rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) rehenic acid ammonium solution is put into temperature for cooling under the environment of-10 ℃, be 6 hours cooling time; E) take out rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
Embodiment 2:a) by the temperature after evaporation concentration, be that the rehenic acid ammonium solution that 50 ℃, concentration are 20g/L is placed in open container; B) in rehenic acid ammonium solution, add ammoniacal liquor, the pH value of rehenic acid ammonium solution is adjusted to 9; C) with gas blower by the blast-cold of rehenic acid ammonium solution to room temperature, rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) rehenic acid ammonium solution is put into temperature for cooling under the environment of-8 ℃, be 8 hours cooling time; E) take out rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
Embodiment 3:a) by the temperature after evaporation concentration, be that the rehenic acid ammonium solution that 90 ℃, concentration are 30g/L is placed in open container; B) in rehenic acid ammonium solution, add ammoniacal liquor, the pH value of rehenic acid ammonium solution is adjusted to 11; C) with gas blower by the blast-cold of rehenic acid ammonium solution to room temperature, rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) it is cooling under the environment of 0 ℃ rehenic acid ammonium solution being put into temperature, and be 12 hours cooling time; E) take out rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
Claims (1)
1. a rehenic acid ammonium solution crystallization method, is characterized in that comprising following methods step: by the temperature after evaporation concentration, be a) that 30 ℃～90 ℃, the rehenic acid ammonium solution of concentration>=15g/L are placed in open container; B) to adding in rehenic acid ammonium solution to be hydrolyzed, produce NH
4 +material, the pH value of rehenic acid ammonium solution is adjusted to 8～11; C) the conventional wind regime of use industry is by the blast-cold of rehenic acid ammonium solution to room temperature, and rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) it is cooling under the environment of-10 ℃～0 ℃ rehenic acid ammonium solution being put into temperature, and be more than 6 hours cooling time; E) take out rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium; Above-mentioned can hydrolysis produces NH
4 +material be ammoniacal liquor.
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| CN201110267640.5A CN102992407B (en) | 2011-09-11 | 2011-09-11 | Ammonium rhenate solution crystallization method |
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| CN201110267640.5A CN102992407B (en) | 2011-09-11 | 2011-09-11 | Ammonium rhenate solution crystallization method |
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| CN102992407A CN102992407A (en) | 2013-03-27 |
| CN102992407B true CN102992407B (en) | 2014-11-26 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630509B (en) * | 2015-02-03 | 2016-11-23 | 嵩县开拓者钼业有限公司 | A kind of method preparing ammonium perrhenate |
| CN106498194B (en) * | 2016-10-27 | 2019-02-01 | 洛阳佰尼尔新材料科技有限公司 | A method of preparing rhenium metal |
| CN106745293B (en) * | 2016-12-08 | 2018-01-16 | 江苏鼎杰合金科技有限公司 | A kind of preparation method of high-purity rehenic acid ammonium |
| CN107419101B (en) * | 2017-07-14 | 2019-01-01 | 周华元 | A kind of method that efficiently concentrating rhenium prepares ammonium perrhenate |
| CN110606511A (en) * | 2019-08-01 | 2019-12-24 | 中国科学院金属研究所 | Ammonium rhenate with uniform particle size and preparation method thereof |
| CN110527854B (en) * | 2019-09-11 | 2021-06-11 | 广东先导稀材股份有限公司 | Method for preparing particle size controllable ultra-pure ammonium rhenate crystal |
| CN115611325B (en) * | 2022-10-09 | 2023-11-24 | 中国科学院金属研究所 | High-purity ammonium rhenate and preparation method thereof |
Citations (2)
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|---|---|---|---|---|
| US5891407A (en) * | 1996-05-30 | 1999-04-06 | H.C. Starck Gmbh & Co. Kg | Process for producing pure ammonium metallates |
| CN101240378A (en) * | 2007-02-07 | 2008-08-13 | 江西铜业集团公司 | Technique for reclaiming rhenium from multiple mixed acid system |
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2011
- 2011-09-11 CN CN201110267640.5A patent/CN102992407B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5891407A (en) * | 1996-05-30 | 1999-04-06 | H.C. Starck Gmbh & Co. Kg | Process for producing pure ammonium metallates |
| CN101240378A (en) * | 2007-02-07 | 2008-08-13 | 江西铜业集团公司 | Technique for reclaiming rhenium from multiple mixed acid system |
Non-Patent Citations (4)
| Title |
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| 《化学化工大辞典》编委会 等."高铼酸铵".《化学化工大辞典（上、下册）》.化学工业出版社,2003,(第1版),780. * |
| 《化学化工大辞典》编委会 等."高铼酸铵".《化学化工大辞典(上、下册)》.化学工业出版社,2003,(第1版),780. * |
| 从净化洗涤污酸中提取金属铼的试验研究;高志正;《中国有色冶金》;20081231(第6期);68-70 * |
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