CN102851502B - Method for extracting and separating beryllium - Google Patents
Method for extracting and separating beryllium Download PDFInfo
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- CN102851502B CN102851502B CN2012101281855A CN201210128185A CN102851502B CN 102851502 B CN102851502 B CN 102851502B CN 2012101281855 A CN2012101281855 A CN 2012101281855A CN 201210128185 A CN201210128185 A CN 201210128185A CN 102851502 B CN102851502 B CN 102851502B
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Abstract
The invention relates to a method for extracting and separating beryllium. Beryllium-containing dosage liquor is a sulfuric acid solution containing beryllium ions, wherein the concentration of the beryllium ions is 0.2-30g/L. The method is characterized in that the method comprises the steps of: (1) a naphthenic acid-alcohol or isooctanol-kerosene organic phase is uniformly mixed with the beryllium-containing dosage liquor; an alkaline solution is added to the mixed liquid, such that the pH value of the liquid is 5-8; (2) an acidic solution is added to the organic phase obtained in the step (1) for stripping impurities, such that an organic phase which is an impurity-removed beryllium-containing organic-phase solution is obtained; and (3) an alkaline solution is added to the organic phase obtained in the step (2) for stripping beryllium, such that a water phase which is an impurity-removed beryllium-containing solution is obtained; and the organic phase is delivered back to the step (1) and is reused. With the method provided by the invention, beryllium can be selectively separated from impurities such as iron and aluminum. The extraction stages are few, the process is simple, a separation effect is good, and a beryllium recovery rate is high.
Description
Technical field
The present invention relates to a kind of method of extracting and separating beryllium.
Background technology
Beryllium is the alkali earth metal of density minimum, is widely used in nuclear power, aerospace and the fields such as aviation, metallurgy.
At present, the main production method of extracting in the world beryllium oxide from ore is fluorination method and sulfuric acid process.Fluorination method be with levigate beryllium with after Sodium Silicofluoride, iron ice crystal and yellow soda ash mix briquetting in mass ratio in the resistive heating kiln sintering, water leaches behind the agglomerate mix grinding.The flow process of fluorination method is fairly simple, and the protection against corrosion condition is good, and is fit to process fluorine-containing high raw material, but quality product is slightly poorer than sulfuric acid process.When this method is processed low grade ore, except the auxiliary consumption increases, the increase of calcium and phosphorus will reduce the content of water-soluble beryllium in the sintered material, affect the rate of recovery, and also bring the problem of fluorine processing during three wastes processing.Sulfuric acid process is with the beryllium melting, destroys the crystalline texture of its aluminizing Si oxide, makes solvent with sulfuric acid, and what make that oxide dissolution becomes vitriol contains the beryllium feed liquid.Then use the method for a series of wet separation separating-purifying, beryllium is extracted and makes beryllium hydroxide, be calcination at last industrial beryllium oxide.This method long flow path, but quality product is purer.So far, sulfuric acid process has been passed through and has been updated and perfect, is one of method of widespread use during modern beryllium hydroxide and beryllium oxide are produced.
At present, contain beryllium sulfuric acid liquid removal of impurities process and mainly contain: exsiccated ammonium alum crystallization process, hydrolytic precipitation method and P204 extraction process etc.Because the exsiccated ammonium alum crystallization process is except aluminium weak effect, troublesome poeration; The hydrolytic precipitation method can only deironing, can not remove aluminium; The P204 extraction process can separate beryllium and other alkaline-earth metal, but the method extraction progression is many, to iron, aluminium inferior separating effect, needs anti-stripping agent stepwise deironing, aluminium, troublesome poeration.Therefore, also need to seek more suitable, the better extracting process of selectivity.
Summary of the invention
The object of the present invention is to provide the method for the good extracting and separating beryllium of a kind of selectivity.
The method of extracting and separating beryllium of the present invention is as follows: (1) with volume ratio be 15 ~ 25% naphthenic acid-15 ~ 25% octanol or isooctyl alcohol-50 ~ 70% kerosene organic phase with contain the beryllium feed liquid and mix at 0.5 ~ 5: 1 by volume, adding basic solution in the mixed solution, to make material liquid pH value be 5 ~ 8; (2) by organic phase and acidic solution volume ratio 0.1 ~ 5: 1 adding acidic solution back extraction impurity in the organic phase of step (1) gained, organic phase is and contains the beryllium organic phase solution after the removal of impurities; (3) by organic phase and basic solution volume ratio 0.1 ~ 5: 1, adding basic solution reextraction beryllium in the organic phase of step (2) gained, water are and contain beryllium solution after the removal of impurities, and organic phase is returned step (1) and reused.
Above-mentioned basic solution is ammoniacal liquor, sodium hydroxide, yellow soda ash or bicarbonate of ammonia.
Above-mentioned acidic solution is sulphuric acid soln or hydrochloric acid soln.
The present invention utilizes naphthenic acid to extract easily beryllium, iron, aluminium, and is not strong to alkaline-earth metal extracting powers such as calcium, magnesium, at first by extraction beryllium separated with alkaline-earth metal such as calcium, magnesium; Then utilize under acidity reextraction condition the metal ions such as iron, aluminium easily to strip, and the characteristics such as the difficult reextraction of beryllium with separation of metal ions such as iron, aluminium, stay beryllium to be retained in the organic phase under acidity reextraction condition; By basic solution beryllium is stripped at last, reach the purpose of separating-purifying beryllium.
The method of a kind of extracting and separating beryllium of the present invention can be with impurity selective separation such as beryllium and iron, aluminium, and extraction progression is few, and technique is simple, good separating effect, and the beryllium rate of recovery is high.
Embodiment
Embodiment 1
Certain low-grade complex ore contain beryllium feed liquid, Contents of Main Components Be 5g/L, Fe 9g/L, Al 3g/L.With volume ratio be 15% naphthenic acid-15% octanol-70% kerosene organic phase with contain the beryllium feed liquid by O: A=3: 1 mixes, drip concentration in the whipping process and be 0.6mol/L ammoniacal liquor to pH=5.2, stop to stir standing demix, it is 0.05g/L that analysis records aqueous phase Be, and the beryllium percentage extraction reaches 99% as calculated; The discharging water, then by organic phase and sulphuric acid soln O: A=0.15: 1, be the sulphuric acid soln back extraction organic phase of 0.6mol/L with concentration,, after mixing, stop to stir standing demix, discharging water; At last by organic phase and sodium hydroxide solution O: A=0.13: 1, be the sodium hydroxide solution reextraction organic phase of 2.8mol/L with concentration, after mixing, stop to stir standing demix, organic phase is returned and is reused, water is the sodium beryllate after the removal of impurities, becomes beryllium hydroxide through heating hydrolysis, is sintered into beryllium oxide, purity is 98.2% by analysis, and the beryllium yield reaches 99%.
Embodiment 2
With embodiment 1, the organic phase volume ratio is 25% naphthenic acid-25% isooctyl alcohol-50% kerosene, with organic phase with contain beryllium feed liquid O: A=5: 1 mixes, dripping concentration in the whipping process is that the 6mol/L sodium hydroxide solution is to pH=7.5, stop to stir, standing demix, analyzing and recording aqueous phase Be is 0.02g/L, the beryllium percentage extraction is higher than 99% as calculated.The discharging water, then by organic phase and hydrochloric acid soln O: A=5: 1, be the hydrochloric acid soln adding organic phase of 5mol/L with concentration, after mixing, stop to stir standing demix, discharging water; Press O by organic phase and sodium hydroxide solution at last: A=5: 1, be the sodium hydroxide solution reextraction organic phase of 6mol/L with concentration, after mixing, stop to stir standing demix, organic phase is returned and is reused, water is the sodium beryllate after the removal of impurities, becomes beryllium hydroxide through heating hydrolysis, is sintered into beryllium oxide, purity is 99.0% by analysis, and the beryllium yield reaches 98.9%.
Embodiment 3
Certain low-grade complex ore contain beryllium feed liquid, its component content Be 2g/L, Fe 5g/L, Al 6g/L.With volume ratio be 25% naphthenic acid-15% octanol-60% kerosene organic phase with contain the beryllium feed liquid by O: A=0.6: 1 mixes, dripping concentration in the whipping process is that the 3mol/L sodium carbonate solution is to pH=6.0, stop to stir, standing demix, it is 0.01g/L that analysis records aqueous phase Be, the beryllium percentage extraction reaches 99.5% as calculated, the discharging water; Then press O by organic phase and sulphuric acid soln: A=2: 1, be the sulphuric acid soln back extraction organic phase of 3mol/L with concentration, after mixing, stop to stir standing demix, discharging water; At last by organic phase and ammonium carbonate solution O: A=2: 1, be the ammonium carbonate solution reextraction organic phase of 3.5mol/L with concentration, after mixing, stop to stir standing demix, organic phase is returned and is reused, water is to contain beryllium solution after the removal of impurities, becomes beryllium hydroxide through heating hydrolysis, is sintered into beryllium oxide, purity is 98.7% by analysis, and the beryllium yield reaches 98%.
Embodiment 4
Embodiment 3 simultaneously, the organic phase volume ratio is 15% naphthenic acid-25% isooctyl alcohol-60% kerosene, with organic phase with contain the beryllium feed liquid by O: A=2: 1 mixes, dripping concentration in the whipping process is that the 6mol/L ammonium bicarbonate soln is to pH=7.9, stop to stir, standing demix, analyzing and recording aqueous phase Be is 0.02g/L, the beryllium percentage extraction is higher than 99% as calculated, the discharging water; Then press O by organic phase and hydrochloric acid soln: A=3: 1, be the hydrochloric acid soln back extraction organic phase of 3mol/L with concentration, after mixing, stop to stir standing demix, discharging water; At last by organic phase and sodium hydroxide solution O: A=3: 1, be the sodium hydroxide solution reextraction organic phase of 4mol/L with concentration, after mixing, stop to stir standing demix, organic phase is returned and is reused, water is the sodium beryllate after the removal of impurities, becomes beryllium hydroxide through heating hydrolysis, is sintered into beryllium oxide, purity is 99.1% by analysis, and the beryllium yield reaches 98.5%.
Claims (3)
1. the method for an extracting and separating beryllium, containing the beryllium feed liquid is the sulphuric acid soln that contains beryllium ion, wherein beryllium ion concentration is 0.2 ~ 30g/L, it is characterized in that being formed by following steps: (1) with volume ratio be 15 ~ 25% naphthenic acid-15 ~ 25% octanol-50 ~ 70% kerosene organic phase with contain the beryllium feed liquid and mix at 0.5 ~ 5: 1 by volume, adding basic solution in the mixed solution, to make material liquid pH value be 5 ~ 8; (2) by organic phase and acidic solution volume ratio 0.1 ~ 5: 1 adding acidic solution back extraction impurity in the organic phase of step (1) gained, organic phase is and contains the beryllium organic phase solution after the removal of impurities; (3) by organic phase and basic solution volume ratio 0.1 ~ 5: 1, adding basic solution reextraction beryllium in the organic phase of step (2) gained, water are and contain beryllium solution after the removal of impurities, and organic phase is returned step (1) and reused.
2. the method for extracting and separating beryllium according to claim 1 is characterized in that described basic solution is ammoniacal liquor, sodium hydroxide, yellow soda ash or bicarbonate of ammonia.
3. the method for extracting and separating beryllium according to claim 1 is characterized in that described acidic solution is sulphuric acid soln or hydrochloric acid soln.
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| CN103468975B (en) * | 2013-08-23 | 2015-03-25 | 西北矿冶研究院 | Method for extracting beryllium from aureobasite type beryllium concentrate with low beneficiation enrichment ratio |
| CN103556186B (en) * | 2013-11-05 | 2016-05-18 | 浙江科菲科技股份有限公司 | The selective separation method of copper and beryllium in a kind of sulfuric acid system |
| CN106673028A (en) * | 2015-11-09 | 2017-05-17 | 虔东稀土集团股份有限公司 | Preparation method of alkaline earth metal compound |
| CN105907962B (en) * | 2016-04-26 | 2018-09-07 | 新疆有色金属研究所 | The preparation method of high-purity strip liquor containing beryllium and preparation method thereof, ammonium fluoberyllate, beryllium fluoride and metallic beryllium |
| CN110438351A (en) * | 2019-08-29 | 2019-11-12 | 中稀(常州)稀土新材料有限公司 | A kind of rare earth impurities separation method |
| CN115074539B (en) * | 2022-07-20 | 2022-11-22 | 中南大学 | Method for recycling and detoxifying beryllium in beryllium-containing sludge |
| CN116282090A (en) * | 2023-02-22 | 2023-06-23 | 中国科学院过程工程研究所 | Method for separating beryllium from beryllium hydroxide containing impurities by adopting chlorination system and application of method |
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| JP2983590B2 (en) * | 1990-08-20 | 1999-11-29 | 昭和シェル石油株式会社 | Asphalt replacement composition |
| CN102168184B (en) * | 2011-05-27 | 2012-10-24 | 广州有色金属研究院 | Method for extracting beryllium oxide from low-grade beryllium ore |
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Effective date of registration: 20171227 Address after: 510651 Changxin Road, Guangzhou, Guangdong, No. 363, No. Patentee after: GUANGDONG INSTITUTE OF RARE METALS Address before: 510651 Changxin Road, Guangzhou, Guangdong, No. 363, No. Patentee before: Guangzhou Research Institute of Non-ferrous Metals |
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Address after: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee after: Institute of rare metals, Guangdong Academy of Sciences Address before: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee before: GUANGDONG INSTITUTE OF RARE METALS |
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