CN110002503A - A kind of method of purification removing organic matter in rehenic acid ammonium - Google Patents
A kind of method of purification removing organic matter in rehenic acid ammonium Download PDFInfo
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- CN110002503A CN110002503A CN201910175799.0A CN201910175799A CN110002503A CN 110002503 A CN110002503 A CN 110002503A CN 201910175799 A CN201910175799 A CN 201910175799A CN 110002503 A CN110002503 A CN 110002503A
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- Prior art keywords
- rehenic acid
- acid ammonium
- ammonium
- purification
- purification according
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of methods of purification of organic matter in removal rehenic acid ammonium, belong to the rehenic acid ammonium purification technique field in hydrometallurgy.A kind of method of purification removing organic matter in rehenic acid ammonium comprising the steps of: (1) the rehenic acid ammonium containing organic impurities is put into container, deionized water is added and simultaneously is heated to being completely dissolved；(2) it is passed through gas strong oxidizer into Ammonium rhenate solution, stirs simultaneously, until organic matter is fully oxidized in solution；(3) it is filtered after removing solution surface foam, filtered filtrate is placed in cooling device cooling until rehenic acid ammonium is fully crystallized, filters again, take out rehenic acid crystalline ammonium substance and simultaneously carried out centrifugal dehydration treatment, dewatered rehenic acid ammonium is dry, obtain high-purity rehenic acid ammonium product.The rehenic acid ammonium product purity of this method preparation has the advantages that simple process, high-efficient, at low cost 99.995% or more.
Description
Technical field
The invention belongs to the rehenic acid ammonium purification technique field in hydrometallurgy, it is related to organic matter in a kind of removal rehenic acid ammonium
Method of purification.
Background technique
Industrialization purification rehenic acid ammonium is to obtain high-purity by selecting proper method to purify Ammonium rhenate solution, then by crystallization
Rehenic acid ammonium, main method have crystallisation, ion exchange-crystallisation and extraction, and industrial most widely used for extraction
Method.
Extraction, also known as solvent extraction or liquid-liquid extraction are that have different solubility in a solvent using component in system
Carry out the unit operation of separating mixture.It is to utilize substance solubility or distribution in the solvent of two kinds immiscible (or slightly soluble)
The difference of coefficient makes solute substance from a kind of method being transferred in another solvent in solvent.It is most of at present to use extraction
Follow the example of technique production rehenic acid ammonium product.In purification process, a small amount of organic matter sandwiches in crude product crude product, when purification, has
The impurity such as machine are difficult to remove completely, cause unstable product quality.Existing method be added the liquid oxidizers such as hydrogen peroxide into
Row oxidation organic impurities, to remove organic matter, but the liquid oxidizers such as hydrogen peroxide can be impure to bring because of oxidant itself
Other metal impurities such as sodium, potassium and magnesium, thus the purity of polluted product.
Summary of the invention
The purification side for being introduced into organic matter in the removal rehenic acid ammonium of other impurities can be prevented the object of the present invention is to provide one kind
Method.The purpose of the present invention is achieved through the following technical solutions.
A kind of method of purification removing organic matter in rehenic acid ammonium, which is characterized in that comprise the steps of:
(1) the rehenic acid ammonium containing organic impurities is put into container, deionized water is added and is heated to being completely dissolved；
(2) it is passed through gas strong oxidizer into Ammonium rhenate solution, stirs simultaneously, until organic matter is by complete oxygen in solution
Change；
(3) it filters, filtered filtrate is placed in cooling device cooling until rehenic acid after removing solution surface foam
Ammonium is fully crystallized, and is filtered again, is taken out rehenic acid crystalline ammonium substance and is carried out centrifugal dehydration treatment, by dewatered rehenic acid ammonium
It is dry, obtain high-purity rehenic acid ammonium product.
Further, deionized water additional amount is that 500~800 milliliters of deionizations are added in every kilogram of rehenic acid ammonium in step (1)
Water.
Further, solution temperature is 60-90 DEG C, preferably 80-85 DEG C in step (1).
Further, gas strong oxidizer is selected from one of ozone, chlorine, fluorine gas, preferably ozone in step (2).
Further, gas strong oxidizer flow is 0.1-0.3m in step (2)3/ h is passed through gas time as 5-20 points
Clock.
Further, the temperature of filtering is 60-90 DEG C for the first time in step (3).
Further, cooling temperature is 0-5 DEG C in step (3), 90-120 minutes cooling time.
Further, drying temperature is 100-120 DEG C in step (3), drying time 60-90 minute.
The beneficial effects of the present invention are:
1. the extractant carried secretly in Ammonium rhenate solution forms foam by the oxidation of ozone and is removed, to reduce
Carbon content in Ammonium rhenate solution；
The metal ions such as lower valency Fe, Cu for being not easy to remove are made to switch to high-valence state Fe, Cu easily removed etc. 2. being passed through ozone
Metal ion and remove the metal impurities such as Fe, Cu, while lower valency rhenium salt being made to switch to the rhenium salt of high-valence state, ensure that rehenic acid ammonium produces
The purity of product improves rhenium comprehensive recovery,
3. being passed through ozone can avoid as the liquid oxidizers such as hydrogen peroxide bring sodium, potassium and magnesium and other impurities.
4. the rehenic acid ammonium product purity prepared by this method is 99.995% or more.
Specific embodiment
Below by way of the implementation of specific embodiment the present invention will be described in detail technical solution, but cannot can be real to of the invention
It applies range and forms any restriction.Those of ordinary skill in the art technical solution of the present invention is made according to above content one
A little nonessential modifications and adaptations, still fall within protection scope of the present invention.
Embodiment 1
A kind of method of purification of rehenic acid ammonium removal organic matter comprising the steps of:
1) rehenic acid ammonium product is put into container, 500 milliliters of water are added with every kilogram of rehenic acid ammonium product and are heated to 82 DEG C
It is dissolved, until being completely dissolved；
2) ozone, flow 0.3m are passed through into Ammonium rhenate solution3/ h is stirred 20 minutes；
3) it filters, filtered filtrate is placed in cooling device, at 3 DEG C at 80 DEG C after removing solution surface foam
Under the conditions of cooling 120 minutes, filter again, take out crystalline material and crystalline material is simultaneously subjected to centrifuge dehydration, crystal
Matter is placed in baking oven, is produced to get the rehenic acid ammonium to purity greater than 99.995% within evenly drying 80 minutes under the conditions of 100 DEG C
Product.
Embodiment 2
A kind of method of purification of rehenic acid ammonium removal organic matter comprising the steps of:
1) rehenic acid ammonium product is put into container, 600 milliliters of water are added with every kilogram of rehenic acid ammonium product and are heated to 83 DEG C
It is dissolved, until being completely dissolved；
2) ozone, flow 0.3m are passed through into Ammonium rhenate solution3/ h is stirred 20 minutes；
3) it filters, filtered filtrate is placed in cooling device, at 5 DEG C at 83 DEG C after removing solution surface foam
Under the conditions of cooling 120 minutes, filter again, take out crystalline material and crystalline material is simultaneously subjected to centrifuge dehydration, crystal
Matter is placed in baking oven, is produced to get the rehenic acid ammonium to purity greater than 99.995% within evenly drying 70 minutes under the conditions of 120 DEG C
Product.
Embodiment 3
A kind of method of purification of rehenic acid ammonium removal organic matter, comprising the following steps:
1) rehenic acid ammonium product is put into container, 800 milliliters of water are added with every kilogram of rehenic acid ammonium product and are heated to 85 DEG C
It is dissolved, until being completely dissolved；
2) ozone, flow 0.3m are passed through into Ammonium rhenate solution3/ h is stirred 15 minutes；
3) it filters, filtered filtrate is placed in cooling device, at 1 DEG C at 85 DEG C after removing solution surface foam
Under the conditions of cooling 90 minutes, filter again, take out crystalline material and crystalline material is simultaneously subjected to centrifuge dehydration, crystalline material
It is placed in baking oven, evenly drying 75 minutes is under the conditions of 110 DEG C to get the rehenic acid ammonium product for being greater than 99.995% to purity.
Claims (10)
1. the method for purification of organic matter in a kind of removal rehenic acid ammonium, which is characterized in that comprise the steps of:
(1) the rehenic acid ammonium containing organic impurities is put into container, deionized water is added and is heated to being completely dissolved；
(2) it is passed through gas strong oxidizer into Ammonium rhenate solution, stirs simultaneously, until organic matter is fully oxidized in solution；
(3) it is filtered after removing solution surface foam, filtered filtrate is placed in cooling device cooling until rehenic acid ammonium is complete
Holocrystalline filters again, takes out rehenic acid crystalline ammonium substance and is carried out centrifugal dehydration treatment, dewatered rehenic acid ammonium is done
It is dry, obtain high-purity rehenic acid ammonium product.
2. method of purification according to claim 1, which is characterized in that deionized water additional amount is every kilogram in step (1)
500~800 ml deionized waters are added in rehenic acid ammonium.
3. method of purification according to claim 1, which is characterized in that solution temperature is 60-90 DEG C in step (1).
4. method of purification according to claim 1, which is characterized in that solution temperature is 80-85 DEG C in step (1).
5. method of purification according to claim 1, which is characterized in that gas strong oxidizer is selected from ozone, chlorine in step (2)
One of gas, fluorine gas.
6. method of purification according to claim 1, which is characterized in that gas strong oxidizer is ozone in step (2).
7. method of purification according to claim 1, which is characterized in that gas strong oxidizer flow is 0.1- in step (2)
0.3m3/ h, being passed through gas time is 5-20 minutes.
8. method of purification according to claim 1, which is characterized in that the temperature of filtering is 60-90 for the first time in step (3)
℃。
9. method of purification according to claim 1, which is characterized in that cooling temperature is 0-5 DEG C in step (3), when cooling
Between 90-120 minutes.
10. method of purification according to claim 1, which is characterized in that drying temperature is 100-120 DEG C in step (3), is done
Dry time 60-90 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910175799.0A CN110002503A (en) | 2019-03-08 | 2019-03-08 | A kind of method of purification removing organic matter in rehenic acid ammonium |
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| CN201910175799.0A CN110002503A (en) | 2019-03-08 | 2019-03-08 | A kind of method of purification removing organic matter in rehenic acid ammonium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111333116A (en) * | 2020-04-01 | 2020-06-26 | 中国科学院金属研究所 | Rehenic acid ammonium purification system |
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|---|---|---|---|---|
| CN101643246A (en) * | 2009-08-28 | 2010-02-10 | 江西铜业股份有限公司 | Impurity-removing and purifying method of ammonium rhenate |
| CN103172121A (en) * | 2013-02-28 | 2013-06-26 | 江西铜业股份有限公司 | Ammonium rhenate purification method |
| CN105384195A (en) * | 2015-12-11 | 2016-03-09 | 中国地质科学院郑州矿产综合利用研究所 | Method for recovering rhenium from molybdenum smelting waste acid |
| CN106315682A (en) * | 2016-08-18 | 2017-01-11 | 阳谷祥光铜业有限公司 | Method for producing ammonium perrhenate from rhenium-enriched residues |
| US20170114428A1 (en) * | 2015-10-26 | 2017-04-27 | Auris Noble Llc | Method for platinum recovery from materials containing rhenium and platinum metals |
-
2019
- 2019-03-08 CN CN201910175799.0A patent/CN110002503A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643246A (en) * | 2009-08-28 | 2010-02-10 | 江西铜业股份有限公司 | Impurity-removing and purifying method of ammonium rhenate |
| CN103172121A (en) * | 2013-02-28 | 2013-06-26 | 江西铜业股份有限公司 | Ammonium rhenate purification method |
| US20170114428A1 (en) * | 2015-10-26 | 2017-04-27 | Auris Noble Llc | Method for platinum recovery from materials containing rhenium and platinum metals |
| CN105384195A (en) * | 2015-12-11 | 2016-03-09 | 中国地质科学院郑州矿产综合利用研究所 | Method for recovering rhenium from molybdenum smelting waste acid |
| CN106315682A (en) * | 2016-08-18 | 2017-01-11 | 阳谷祥光铜业有限公司 | Method for producing ammonium perrhenate from rhenium-enriched residues |
Non-Patent Citations (1)
| Title |
|---|
| 张倩等: "臭氧氧化技术", 《普通高等院校环境科学与工程类系列规划教材 水环境化学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111333116A (en) * | 2020-04-01 | 2020-06-26 | 中国科学院金属研究所 | Rehenic acid ammonium purification system |
| CN111333116B (en) * | 2020-04-01 | 2024-05-24 | 中国科学院金属研究所 | Ammonium Rhenate Purification System |
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