CN104498722A - Method for comprehensively recovering mercury and selenium from metallurgical slag - Google Patents
Method for comprehensively recovering mercury and selenium from metallurgical slag Download PDFInfo
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- CN104498722A CN104498722A CN201410774379.1A CN201410774379A CN104498722A CN 104498722 A CN104498722 A CN 104498722A CN 201410774379 A CN201410774379 A CN 201410774379A CN 104498722 A CN104498722 A CN 104498722A
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Abstract
The invention discloses a method for comprehensively recovering mercury and selenium from metallurgical slag and belongs to the field of metallurgy. The method comprises following steps: grinding the metallurgical slag to the range of 130-150 microns, blending the metallurgical slag with quick lime accounting for 10-30% of the metallurgical slag and roasting at a temperature ranging from 750 to 900 DEG C for 6-8 hours; collecting dust from mercury-containing vapor firstly by use of a cloth bag and then by virtue of cyclone, condensing the mercury vapor by use of a two-stage condensation apparatus to recovery the mercury, and returning mercurial soot and a tail gas adsorption filler to the metallurgical slag for reutilization, wherein no pollutant is emitted in the process; next, leaching selenium-containing slag by use of an oxidation solution prepared from hydrochloric acid and sodium chlorate in the ratio of 2:1, analyzing the contents of Hg<2+>, Fe<2+>, Ca<2+> and Mg<2+> in the leachate in the liquid-solid ratio of 2:1, respectively, precipitating the ions by use of sodium sulfide in the ratio of 1:1 to the total content of the ions and then filtering to remove the irons, and reducing for 2 hours by use of hydroxylamine hydrochloride, thereby obtaining the elemental selenium after washing the precipitate. The method for comprehensively recovering mercury and selenium from the metallurgical slag is high in extraction rate and prone to industrial production.
Description
Technical field
The invention belongs to field of metallurgy, be specifically related to a kind of method of synthetical recovery mercury selenium from metallurgical slag.
Background technology
In recent years, along with the continuous expansion with production capacity that develops rapidly of science and technology, mercury and selenium are all widely used in different industries with the characteristic of its excellence.Mercury produces the catalyzer raw material of PVC as calcium carbide route, and current PVC industry production capacity continuous expansion, mercury resource is day by day exhausted in addition, extracts mercury resource particularly important from metallurgical slag.And elemental selenium and selenium compound are widely used in semiconductor material with the physics-chem characteristic of its excellence, market outlook are comparatively wide; With regard in current technology, only have the method for single recovery selenium, have no the method for synthetical recovery selenium mercury, not only cause the wasting of resources, and contaminate environment.
Summary of the invention
It is high that goal of the invention of the present invention is to provide a kind of extraction yield, is easy to realize the method for synthetical recovery mercury selenium from metallurgical slag of suitability for industrialized production.
The scheme that the present invention solves the problems of the technologies described above is as follows:
A kind of method from metallurgical slag synthetical recovery mercury selenium of the present invention, comprises the steps:
(1) metallurgical slag is crushed to 130 ~ 150 μm, allocates the 10-30% that unslaked lime amount is metallurgical slag into, roasting 6-8 hour at 750 DEG C ~ 900 DEG C;
(2) carry out cyclone dust collection containing after the first bag collection of mercury vapour, mercury vapour adopts two sections of condensing equipment condensations to reclaim mercury, and mercurial soot ash and tail gas adsorption filler return metallurgical slag and re-use, non-pollutant discharge in this step;
(3) oxidation solution being 2:1 containing selenium slag employing hydrochloric acid and sodium chlorate amount of substance leaches, and liquid-solid ratio is 2:1, Hg in leach liquor
2+, Fe
2+, Ca
2+, Mg
2+analyze its content respectively, the sodium sulphite adopting each ion content summation 1:1 to measure carries out sedimentation and filtration removing,
(4) adopt oxammonium hydrochloride reductase 12 hour, obtain elemental selenium by after washing of precipitate.
A kind of above-mentioned method from metallurgical slag synthetical recovery mercury selenium, wherein: mercury content 7 ~ 30% in mercurous selenic acid mud, selenium content 25 ~ 40%.
The present invention compared with prior art, has obvious beneficial effect, as can be known from the above technical solutions: adopt hydrochloric acid and sodium chlorate Oxidation Leaching containing selenium slag, compared with other conventional oxidation agent, raw materials cost is lower, Hg in leach liquor
2+, Fe
2+, Ca
2+, Mg
2+remove after adopting sodium sulphite to carry out sedimentation and filtration, because the solubility product constant of corresponding sulfide is less than the solubility product constant of oxyhydroxide, adopt sodium sulphite generation to precipitate comparatively sodium hydroxide pellets more thorough.Metallurgical slag allocates unslaked lime roasting into, adopt bag collection and cyclone dust collection respectively containing mercuryvapour, mercury vapour adopts two sections of condensing equipment condensations to reclaim mercury, and mercurial soot ash and tail gas adsorption filler return metallurgical slag and re-use, not only mercury but also non-pollutant discharge were reclaimed, safety and environmental protection.Therefore, present method reclaim mercury obtain purity higher while, non-pollutant discharge, safety and environmental protection.
The beneficial effect of the inventive method is further illustrated below by way of specific experiment example.
Embodiment
embodiment 1
From a method for metallurgical slag synthetical recovery mercury selenium, comprise the steps:
By mercurous for copper smelting plant selenic acid mud, mercury content 30%, selenium content 40%, is crushed to about 140 μm, allocate that unslaked lime amount is metallurgical slag into about 30%, at 900 DEG C roasting 8 hours must containing mercuryvapour with containing selenium slag; Cyclone dust collection will be carried out containing after the first bag collection of mercury vapour.Mercury vapour adopts two sections of condensing equipment condensations to obtain mercury, mercurial soot ash and tail gas adsorption filler return metallurgical slag and re-use, and the rate of recovery of mercury reaches 98%, are leached the oxidation solution being 2:1 containing selenium slag employing hydrochloric acid and sodium chlorate amount of substance, liquid-solid ratio is 2:1, Hg in leach liquor
2+, Fe
2+, Ca
2+, Mg
2+analyze its content respectively, after the sodium sulphite adopting each ion content summation 1:1 to measure carries out sedimentation and filtration removing, adopt oxammonium hydrochloride reductase 12 hour containing selenium liquid, obtain elemental selenium by after washing of precipitate, the rate of recovery of selenium reaches 97%.
embodiment 2
From a method for metallurgical slag synthetical recovery mercury selenium, comprise the steps:
By mercurous for molybdenum smeltery selenic acid mud, mercury content 7%, selenium content 30%, is crushed to 130 μm, allocate that unslaked lime amount is metallurgical slag into 10%, at 800 DEG C roasting 6 hours must containing mercuryvapour with containing selenium slag; To carry out cyclone dust collection containing after the first bag collection of mercury vapour, mercury vapour adopts two sections of condensing equipment condensations to obtain mercury.The rate of recovery of mercury reaches 98%,
Leached by the oxidation solution being 2:1 containing selenium slag employing hydrochloric acid and sodium chlorate amount of substance, liquid-solid ratio is 2:1, Hg in leach liquor
2+, Fe
2+, Ca
2+, Mg
2+, analyze its content respectively, after the sodium sulphite adopting each ion content summation 1:1 to measure carries out sedimentation and filtration removing, adopt oxammonium hydrochloride reductase 12 hour containing selenium liquid, obtain elemental selenium by after washing of precipitate, the rate of recovery of selenium reaches 97%.
embodiment 3
From a method for metallurgical slag synthetical recovery mercury selenium, comprise the steps:
By mercurous for nickel smelter selenic acid mud, mercury content 20%, selenium content 25%, is crushed to about 150 μm, allocate that unslaked lime amount is metallurgical slag into about 20%, at 750 DEG C roasting 8 hours must containing mercuryvapour with containing selenium slag; To carry out cyclone dust collection containing after the first bag collection of mercury vapour, mercury vapour adopts two sections of condensing equipment condensations to obtain mercury, and the rate of recovery of mercury reaches 99%.
Leached by the oxidation solution being 2:1 containing selenium slag employing hydrochloric acid and sodium chlorate amount of substance, liquid-solid ratio is 2:1, Hg in leach liquor
2+, Fe
2+, Ca
2+, Mg
2+analyze its content respectively, after the sodium sulphite adopting each ion content summation 1:1 to measure carries out sedimentation and filtration removing, adopt oxammonium hydrochloride reductase 12 hour containing selenium liquid, obtain elemental selenium by after washing of precipitate, the rate of recovery of selenium reaches 98%.
The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, anyly do not depart from technical solution of the present invention content, the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (2)
1., from a method for metallurgical slag synthetical recovery mercury selenium, comprise the steps:
(1) metallurgical slag is crushed to 130 ~ 150 μm, allocates the 10-30% that unslaked lime amount is metallurgical slag into, roasting 6-8 hour at 750 DEG C ~ 900 DEG C;
(2) carry out cyclone dust collection containing after the first bag collection of mercury vapour, mercury vapour adopts two sections of condensing equipment condensations to reclaim mercury, and mercurial soot ash and tail gas adsorption filler return metallurgical slag and re-use, non-pollutant discharge in this step;
(3) oxidation solution being 2:1 containing selenium slag employing hydrochloric acid and sodium chlorate amount of substance leaches, and liquid-solid ratio is 2:1, Hg in leach liquor
2+, Fe
2+, Ca
2+, Mg
2+analyze its content respectively, the sodium sulphite adopting each ion content summation 1:1 to measure carries out sedimentation and filtration removing,
(4) adopt oxammonium hydrochloride reductase 12 hour, obtain elemental selenium by after washing of precipitate.
2. a kind of method from metallurgical slag synthetical recovery mercury selenium as claimed in claim 1, wherein: mercury content 7 ~ 30% in mercurous selenic acid mud, selenium content 25 ~ 40%.
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| CN201410774379.1A CN104498722A (en) | 2014-12-16 | 2014-12-16 | Method for comprehensively recovering mercury and selenium from metallurgical slag |
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| CN201410774379.1A CN104498722A (en) | 2014-12-16 | 2014-12-16 | Method for comprehensively recovering mercury and selenium from metallurgical slag |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104894381A (en) * | 2015-05-22 | 2015-09-09 | 铜陵有色设计研究院 | Method for recycling mercury from copper smelting lead filter cake |
| CN104988339A (en) * | 2015-08-17 | 2015-10-21 | 湖南久泰冶金科技有限公司 | Zero-emission mercury metal preparing method |
| CN105039747A (en) * | 2015-07-27 | 2015-11-11 | 湖南有色金属研究院 | Method for enrichment and separation of selenium and mercury from lead filter cake |
| CN105060258A (en) * | 2015-08-11 | 2015-11-18 | 湖南有色金属研究院 | Method for recycling alkaline leached residues through selenium fixation and mercury removal |
| CN105385850A (en) * | 2015-11-02 | 2016-03-09 | 上海交通大学 | Method for separating and recycling heavy metal in mercury, selenium and arsenic containing dirt acid sludge |
| CN104828788B (en) * | 2015-04-24 | 2016-08-17 | 湘潭大学 | A kind of method extracting selenium from hydrargyrum selenic acid mud waste material |
| CN106853959A (en) * | 2016-09-19 | 2017-06-16 | 三门峡市有色金属质量科学研究所 | A kind of method that use impure selenium wet method prepares high purity selenium |
| CN106893865A (en) * | 2017-04-01 | 2017-06-27 | 湖南省环境保护科学研究院 | The method that mercury is extracted from weight acid mud is related to |
| CN112093781A (en) * | 2020-08-06 | 2020-12-18 | 江西铜业股份有限公司 | Method and device for efficiently absorbing and reducing selenium by sulfating roasting copper anode slime |
| CN113005306A (en) * | 2021-01-31 | 2021-06-22 | 济源市孝远实业有限公司 | Rotary kiln roasting mercury smelting system using lead-zinc smelting acid mud as raw material |
| CN113088694A (en) * | 2021-03-08 | 2021-07-09 | 云南驰宏锌锗股份有限公司 | Comprehensive recovery method for valuable metals in lead-zinc smelting acid mud |
| CN114214516A (en) * | 2021-10-15 | 2022-03-22 | 贵州锦丰矿业有限公司 | Method for improving carbon leaching recovery rate of high-mercury gold ore |
| CN115094252A (en) * | 2021-03-12 | 2022-09-23 | 昆明理工大学 | Method for recovering mercury from non-ferrous smelting low-mercury acid sludge by adopting hydrometallurgy technology |
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Non-Patent Citations (1)
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828788B (en) * | 2015-04-24 | 2016-08-17 | 湘潭大学 | A kind of method extracting selenium from hydrargyrum selenic acid mud waste material |
| CN104894381A (en) * | 2015-05-22 | 2015-09-09 | 铜陵有色设计研究院 | Method for recycling mercury from copper smelting lead filter cake |
| CN105039747A (en) * | 2015-07-27 | 2015-11-11 | 湖南有色金属研究院 | Method for enrichment and separation of selenium and mercury from lead filter cake |
| CN105060258A (en) * | 2015-08-11 | 2015-11-18 | 湖南有色金属研究院 | Method for recycling alkaline leached residues through selenium fixation and mercury removal |
| CN104988339A (en) * | 2015-08-17 | 2015-10-21 | 湖南久泰冶金科技有限公司 | Zero-emission mercury metal preparing method |
| CN105385850A (en) * | 2015-11-02 | 2016-03-09 | 上海交通大学 | Method for separating and recycling heavy metal in mercury, selenium and arsenic containing dirt acid sludge |
| CN106853959A (en) * | 2016-09-19 | 2017-06-16 | 三门峡市有色金属质量科学研究所 | A kind of method that use impure selenium wet method prepares high purity selenium |
| CN106853959B (en) * | 2016-09-19 | 2019-07-19 | 三门峡市有色金属质量科学研究所 | A method of high purity selenium is prepared using impure selenium wet process |
| CN106893865A (en) * | 2017-04-01 | 2017-06-27 | 湖南省环境保护科学研究院 | The method that mercury is extracted from weight acid mud is related to |
| CN112093781A (en) * | 2020-08-06 | 2020-12-18 | 江西铜业股份有限公司 | Method and device for efficiently absorbing and reducing selenium by sulfating roasting copper anode slime |
| CN113005306A (en) * | 2021-01-31 | 2021-06-22 | 济源市孝远实业有限公司 | Rotary kiln roasting mercury smelting system using lead-zinc smelting acid mud as raw material |
| CN113088694A (en) * | 2021-03-08 | 2021-07-09 | 云南驰宏锌锗股份有限公司 | Comprehensive recovery method for valuable metals in lead-zinc smelting acid mud |
| CN115094252A (en) * | 2021-03-12 | 2022-09-23 | 昆明理工大学 | Method for recovering mercury from non-ferrous smelting low-mercury acid sludge by adopting hydrometallurgy technology |
| CN115094252B (en) * | 2021-03-12 | 2023-10-24 | 昆明理工大学 | Method for recycling mercury from nonferrous smelting low-mercury acid sludge by adopting hydrometallurgy technology |
| CN114214516A (en) * | 2021-10-15 | 2022-03-22 | 贵州锦丰矿业有限公司 | Method for improving carbon leaching recovery rate of high-mercury gold ore |
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Application publication date: 20150408 |