CN104532013B - Method for recycling silver from jarosite residue - Google Patents

Method for recycling silver from jarosite residue Download PDF

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Publication number
CN104532013B
CN104532013B CN201410799623.XA CN201410799623A CN104532013B CN 104532013 B CN104532013 B CN 104532013B CN 201410799623 A CN201410799623 A CN 201410799623A CN 104532013 B CN104532013 B CN 104532013B
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silver
slag
iron vitriol
vacuum
mixing
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CN104532013A (en
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马红周
桂海平
王耀宁
樊鹏斌
唐雯聃
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Xian University of Architecture and Technology
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Xian University of Architecture and Technology
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention relates to a method for recycling silver from jarosite residue. The method for recycling silver from the jarosite residue comprises the following steps: mixing the jarosite residue with pulverized coal and a desulphurizing agent, and briquetting, thus obtaining mixed spheres, then putting the mixed spheres into a vacuum distillation furnace, and heating at the temperature of 1100-1300 DEG C, thus silver in the jarosite residue is separated, wherein the molar weight ratio of the added pulverized coal to the desulphurizing agent to silver in jarosite residue is 1 to (2-10) to (0.1-10). The method for recycling silver from the jarosite residue has the advantages that the ratio of the pulverized coal to the desulphurizing agent to the jarosite residue is reasonably controlled, and the separation of silver from jarosite residue under the vacuum condition of 1100-1300 DEG C is realized; besides, the whole technological process is carried out in a vacuum furnace, influences on personnel and environments are slight, the method and the required equipment are simple, safe and controllable and are easy to operate, and silver can be recycled from the jarosite residue effectively.

Description

The recovery method of silver in a kind of iron vitriol slag
Technical field
The invention belongs to metallurgical technology field and in particular in a kind of iron vitriol slag silver recovery method.
Background technology
Jarosite Residues are the iron dross removings producing in Zinc Hydrometallurgy Process, add calcining to adjust molten in iron removal The pH of liquid, between 1.0-3.0, in iron vitriol slag in addition to containing materials such as lead, zinc, indiums, also contains the elements such as silver, in iron vitriol slag Silver mainly presented in class matter in-phase version and Argentous sulfide. in vitriol slag, in iron vitriol slag, argentiferous is typically in 200-400g/t.
Processing method to silver in iron vitriol slag is presently mainly to be carried out using floatation, and floatation mainly adopts flotation agent Argentous sulfide. in iron vitriol slag is flotated, the response rate of silver is relatively low.A kind of patent " the synthetical recovery of secondary resource in iron vitriol slag Method " (20140191005.7) discloses the lead that a kind of method of utilization vacuum carbon reduction volatilization reclaims in iron vitriol slag, zinc, indium. And in method disclosed in these, it is not directed to the extraction of silver in iron vitriol slag.
Content of the invention
It is an object of the invention to provide silver-colored recovery method in a kind of iron vitriol slag, this process simplify technological process, carry The high recovery rate of silver.
In order to achieve the above object, the technical solution used in the present invention is:Iron vitriol slag with coal dust, desulphurizer mixing and is pressed Ball, obtains mixing spheroid, then loads in vacuum distillation furnace in 1100-1300 DEG C of heating mixing spheroid to isolate iron vitriol slag In silver, wherein, in the mole of the coal dust being added, the mole of desulfurizing agent and ferrovanadium slag silver mole ratio be 1:(2 ~10):(0.1~10).
Described ferrovanadium slag adopts Jarosite Residues or yellow ammonium ferrovanadium slag.
The granularity of described desulfurizing agent is less than 50mm.
Described desulfurizing agent adopts the mixture of one or more of Calx, limestone, dolomite arbitrary proportion.
When described desulfurizing agent is mixed with iron vitriol slag, batch mixing is carried out using grinder, extruder or cylindrical mixer.
The diameter of described mixing spheroid is less than 100mm.
The concrete grammar of the described silver isolated in iron vitriol slag is:It is loaded into mixing spheroid in vacuum distillation furnace with little It is incubated 1-8h in the vacuum equal to 20Pa in 1100-1300 DEG C, insulation terminates, vacuum breaker of then lowering the temperature, and collect vacuum steaming The silver isolated in furnace.
Temperature during described vacuum breaker is less than 100 DEG C.
Further, the granularity of described coal dust is 74 μm of -3mm.
Compared with prior art, the beneficial effects of the present invention is:
The present invention passes through the rational ratio controlling coal dust, desulfurizing agent and ferrovanadium slag, just can in vacuum distillation furnace in The 1100-1300 DEG C of separation realizing silver, and so that the silver content in iron vitriol slag is substantially reduced;In addition, the whole technical process of the present invention Carry out in a vacuum, less to personnel and environmental effect, technique and equipment needed thereby are simple, safely controllable, easy to operate, can be effective Realize the recycling of silver in iron vitriol slag.Reclaim silver in vacuum distillation furnace, silver can form lead zinc-silver with the lead zinc volatilizing and close Gold, silver needs further to be separated with lead zinc, could obtain silver-colored simple substance.In addition, the application adds desulfurizing agent, desulfurizing agent Not only act as desulfidation, also improved the fusing point of iron vitriol slag, so that iron vitriol slag will not be sintered in high temperature, also reduce simultaneously In vacuum, the partial pressure of sulfur, is conducive to the decomposition of Argentous sulfide., so that the silver in iron vitriol slag is evaporated.
Further, the present invention is defined also by the temperature in vacuum distillation process, pressure and time, makes separation of Silver Effect improve further.
Specific embodiment
With reference to embodiment, the present invention is described in further details.
Embodiment 1:
By yellow ammonium ferrovanadium slag be 74 μm of -3mm with granularity coal dust, granularity be that the Calx of 74 μm of -3mm is mixed with grinder Material pressure ball, obtain the mixing spheroid that diameter is less than 5mm, then put into mixing spheroid and reinstall vacuum distilling in corundum crucible Stove, is incubated 6h with the vacuum of 20Pa in 1100 DEG C, and insulation is cooled to vacuum breaker when in-furnace temperature is less than 100 DEG C after terminating, take Go out to isolate slag after silver and reduction in vacuum distillation furnace;Wherein, the mole of the coal dust being added, the mole of Calx and Huang In ammonium ferrovanadium slag, the ratio of the mole of silver is 1:2:2.
Component analyses (component content is by percentage to the quality) are carried out to the silver before and after the present embodiment Huang ammonium ferrovanadium Slag treatment, Its result is as shown in table 1:
Component analyses (g/t) before and after the yellow ammonium ferrovanadium Slag treatment of table 1
As can be seen from Table 1, in the yellow ammonium ferrovanadium slag that the inventive method is processed, the content of silver substantially reduces, therefore, The present invention can effectively realize the recovery of silver in ferrovanadium slag.
Embodiment 2:
By Jarosite Residues and granularity be 74 μm of -3mm coal dust, granularity be that the limestone of 3 μm of -50mm is carried out with extruder Batch mixing pressure ball, obtain the mixing spheroid that diameter is less than 100mm, then put into mixing spheroid and reinstall vacuum in corundum crucible Retort, is incubated 1h with the vacuum of 15Pa in 1200 DEG C, broken true when insulation is cooled to in-furnace temperature less than 100 DEG C after terminating Sky, takes out and isolates slag after silver and reduction in vacuum distillation furnace;Wherein, the mole of the coal dust being added, the rubbing of limestone Your amount is 1 with the ratio of the mole of silver in Jarosite Residues:2:0.1.
Embodiment 3:
By yellow ammonium ferrovanadium slag and granularity be the coal dust of 74 μm of -3mm, granularity be the dolomite cylindrical mixer of 1mm-10mm Carry out batch mixing pressure ball, obtain the mixing spheroid that diameter is less than 50mm, then put into mixing spheroid in corundum crucible and reinstall Vacuum distillation furnace, is incubated 4h with the vacuum of 18Pa in 1100 DEG C, broken when insulation is cooled to in-furnace temperature less than 100 DEG C after terminating Vacuum, takes out and isolates slag after silver and reduction in vacuum distillation furnace;Wherein, the mole of the coal dust being added, dolomite Mole is 1 with the ratio of the mole of silver in yellow ammonium ferrovanadium slag:10:10.
Embodiment 4:
By yellow ammonium ferrovanadium slag and granularity be the coal dust of 74 μm of -3mm, granularity be the desulfurizing agent cylindrical mixer of 1mm-50mm Carry out batch mixing pressure ball, obtain the mixing spheroid that diameter is less than 50mm, then put into mixing spheroid in corundum crucible and reinstall Vacuum distillation furnace, is incubated 8h with the vacuum of 10Pa in 1300 DEG C, broken when insulation is cooled to in-furnace temperature less than 100 DEG C after terminating Vacuum, takes out and isolates slag after silver and reduction in vacuum distillation furnace;Wherein, the mole of the coal dust being added, desulfurizing agent Mole is 1 with the ratio of the mole of silver in yellow ammonium ferrovanadium slag:10:5, and desulfurizing agent is 1 by mass ratio:1 limestone and white Marble mixes.

Claims (3)

1. in a kind of iron vitriol slag silver recovery method it is characterised in that:By iron vitriol slag and coal dust, desulphurizer mixing pressure ball, obtain To mixing spheroid, then mixing spheroid is loaded in vacuum distillation furnace in 1100-1300 DEG C of heating to isolate in iron vitriol slag Silver, wherein, in the mole of the coal dust being added, the mole of desulfurizing agent and ferrovanadium slag, the ratio of the mole of silver is 1:(2~ 10):(0.1~10);
Described ferrovanadium slag adopts Jarosite Residues or yellow ammonium ferrovanadium slag;
The concrete grammar of the described silver isolated in iron vitriol slag is:Be loaded into mixing spheroid in vacuum distillation furnace with less than etc. Vacuum in 20Pa is incubated 1-8h in 1100-1300 DEG C, and insulation terminates, vacuum breaker of then lowering the temperature, and collects vacuum distillation furnace The silver inside isolated;
Temperature during described vacuum breaker is less than 100 DEG C;
Described desulfurizing agent adopts the mixture of one or more of Calx, limestone, dolomite arbitrary proportion;
When described desulfurizing agent is mixed with iron vitriol slag, batch mixing is carried out using grinder, extruder or cylindrical mixer.
2. in iron vitriol slag according to claim 1 silver recovery method it is characterised in that:The granularity of described desulfurizing agent is little In 50mm.
3. in iron vitriol slag according to claim 1 silver recovery method it is characterised in that:The diameter of described mixing spheroid Less than 100mm.
CN201410799623.XA 2014-12-18 2014-12-18 Method for recycling silver from jarosite residue Active CN104532013B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108251651B (en) * 2018-02-10 2019-12-13 西安建筑科技大学 method for separating zinc-cadmium-lead alloy materials from copper-cadmium slag and nickel-cobalt slag generated in zinc smelting process

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08134557A (en) * 1994-11-14 1996-05-28 Takamichi Iida Operation of dust treatment by vacuum reaction furnace
CN102162035A (en) * 2011-04-07 2011-08-24 赵志强 Vacuum distillation process for extracting silver from silver zinc slag
CN103993182A (en) * 2014-05-07 2014-08-20 西安建筑科技大学 Comprehensive recovery method for secondary resources in iron vitriol slag

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08134557A (en) * 1994-11-14 1996-05-28 Takamichi Iida Operation of dust treatment by vacuum reaction furnace
CN102162035A (en) * 2011-04-07 2011-08-24 赵志强 Vacuum distillation process for extracting silver from silver zinc slag
CN103993182A (en) * 2014-05-07 2014-08-20 西安建筑科技大学 Comprehensive recovery method for secondary resources in iron vitriol slag

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