CN102992407A - Ammonium rhenate solution crystallization method - Google Patents
Ammonium rhenate solution crystallization method Download PDFInfo
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- CN102992407A CN102992407A CN2011102676405A CN201110267640A CN102992407A CN 102992407 A CN102992407 A CN 102992407A CN 2011102676405 A CN2011102676405 A CN 2011102676405A CN 201110267640 A CN201110267640 A CN 201110267640A CN 102992407 A CN102992407 A CN 102992407A
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- acid ammonium
- rehenic acid
- ammonium solution
- ammonium rhenate
- 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 the wet production rehenic acid ammonium technique, the crystallization method of traditional rehenic acid ammonium solution is, adopt water quench or with the mode of gas blower blast-cold, the rehenic acid ammonium solution of evaporation concentration to the finite concentration carried out crystallisation by cooling, obtain rehenic acid ammonium product thereby carry out afterwards solid-liquid separation.The shortcoming of this crystallization method is that the rehenic acid ammonium product production that obtains 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 the following methods step: a) be that 30 ℃～90 ℃, the rehenic acid ammonium solution of concentration 〉=15g/L place open container with the temperature after the evaporation concentration; B) add in the rehenic acid ammonium solution and can be hydrolyzed generation NH4
+Material, the pH value of rehenic acid ammonium solution is adjusted to 8～11; C) to room temperature, the rehenic acid ammonium solution is preliminary crystallization in temperature-fall period with the blast-cold of rehenic acid ammonium solution for usefulness industry wind regime commonly used; D) the rehenic acid ammonium solution being put into temperature is to cool off under-10 ℃～0 ℃ the environment, and be more than 6 hours cooling time; E) take out the rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
Above-mentioned can the hydrolysis produces NH4
+Material be ammoniacal liquor.
The invention has the beneficial effects as follows: because in crystallisation process, NH4
+Can produce common-ion effcet with the 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 invention below is described in detail in detail.
Embodiment 1:a) be that 30 ℃, concentration are that the rehenic acid ammonium solution of 15g/L places open container with the temperature after the evaporation concentration; B) in the rehenic acid ammonium solution, add ammoniacal liquor, the pH value of rehenic acid ammonium solution is adjusted to 8; C) with gas blower with the blast-cold of rehenic acid ammonium solution to room temperature, the rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) the rehenic acid ammonium solution is put into temperature and cools off under-10 ℃ the environment, be 6 hours cooling time; E) take out the rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
Embodiment 2:a) be that 50 ℃, concentration are that the rehenic acid ammonium solution of 20g/L places open container with the temperature after the evaporation concentration; B) in the rehenic acid ammonium solution, add ammoniacal liquor, the pH value of rehenic acid ammonium solution is adjusted to 9; C) with gas blower with the blast-cold of rehenic acid ammonium solution to room temperature, the rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) the rehenic acid ammonium solution is put into temperature and cools off under-8 ℃ the environment, be 8 hours cooling time; E) take out the rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
Embodiment 3:a) be that 90 ℃, concentration are that the rehenic acid ammonium solution of 30g/L places open container with the temperature after the evaporation concentration; B) in the rehenic acid ammonium solution, add ammoniacal liquor, the pH value of rehenic acid ammonium solution is adjusted to 11; C) with gas blower with the blast-cold of rehenic acid ammonium solution to room temperature, the rehenic acid ammonium solution is preliminary crystallization in temperature-fall period; D) the rehenic acid ammonium solution being put into temperature is to cool off under 0 ℃ the environment, and be 12 hours cooling time; E) take out the rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
Claims (2)
1. rehenic acid ammonium solution crystallization method is characterized in that comprising the following methods step: a) be that 30 ℃～90 ℃, the rehenic acid ammonium solution of concentration 〉=15g/L place open container with the temperature after the evaporation concentration; B) add in the rehenic acid ammonium solution and can be hydrolyzed generation NH4
+Material, the pH value of rehenic acid ammonium solution is adjusted to 8～11; C) to room temperature, the rehenic acid ammonium solution is preliminary crystallization in temperature-fall period with the blast-cold of rehenic acid ammonium solution for usefulness industry wind regime commonly used; D) the rehenic acid ammonium solution being put into temperature is to cool off under-10 ℃～0 ℃ the environment, and be more than 6 hours cooling time; E) take out the rehenic acid ammonium solution and carry out solid-liquid separation, obtain the thick product of rehenic acid ammonium.
2. a kind of rehenic acid ammonium solution crystallization method according to claim 1 is characterized in that: above-mentioned energy hydrolysis generation NH4
+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 true CN102992407A (en) | 2013-03-27 |
| CN102992407B CN102992407B (en) | 2014-11-26 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630509A (en) * | 2015-02-03 | 2015-05-20 | 嵩县开拓者钼业有限公司 | Method for preparing ammonium perrhenate |
| CN106498194A (en) * | 2016-10-27 | 2017-03-15 | 嵩县开拓者钼业有限公司 | A kind of method for preparing rhenium metal |
| CN106745293A (en) * | 2016-12-08 | 2017-05-31 | 江苏鼎杰合金科技有限公司 | A kind of preparation method of high-purity rehenic acid ammonium |
| CN107419101A (en) * | 2017-07-14 | 2017-12-01 | 周华元 | A kind of method that efficiently concentrating rhenium prepares ammonium perrhenate |
| CN110527854A (en) * | 2019-09-11 | 2019-12-03 | 广东先导稀材股份有限公司 | Method for preparing particle size controllable ultra-pure ammonium rhenate crystal |
| 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 |
| CN115611325A (en) * | 2022-10-09 | 2023-01-17 | 中国科学院金属研究所 | High-purity ammonium rhenate and preparation method thereof |
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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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| 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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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104630509A (en) * | 2015-02-03 | 2015-05-20 | 嵩县开拓者钼业有限公司 | Method for preparing ammonium perrhenate |
| CN106498194A (en) * | 2016-10-27 | 2017-03-15 | 嵩县开拓者钼业有限公司 | A kind of method for preparing rhenium metal |
| 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 |
| CN106745293A (en) * | 2016-12-08 | 2017-05-31 | 江苏鼎杰合金科技有限公司 | A kind of preparation method of high-purity rehenic acid ammonium |
| CN107419101A (en) * | 2017-07-14 | 2017-12-01 | 周华元 | A kind of method that efficiently concentrating rhenium prepares ammonium perrhenate |
| 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 |
| CN110527854A (en) * | 2019-09-11 | 2019-12-03 | 广东先导稀材股份有限公司 | Method for preparing particle size controllable ultra-pure ammonium rhenate crystal |
| 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 |
| CN115611325A (en) * | 2022-10-09 | 2023-01-17 | 中国科学院金属研究所 | High-purity ammonium rhenate and preparation method thereof |
| 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 |
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| CN102992407B (en) | 2014-11-26 |
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