CN107324358A - A kind of iron vitriol slag low-temperature decomposition and the method that resource is separately recovered - Google Patents
A kind of iron vitriol slag low-temperature decomposition and the method that resource is separately recovered Download PDFInfo
- Publication number
- CN107324358A CN107324358A CN201710471108.2A CN201710471108A CN107324358A CN 107324358 A CN107324358 A CN 107324358A CN 201710471108 A CN201710471108 A CN 201710471108A CN 107324358 A CN107324358 A CN 107324358A
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- China
- Prior art keywords
- iron
- oxide
- vitriol slag
- resource
- iron oxide
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/026—Preparation of ammonia from inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/745—Preparation from sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a kind of iron vitriol slag low-temperature decomposition and the method that resource is separately recovered, it is that iron vitriol slag is carried out into predecomposition in cryogenic heat exchanger, obtains sulfuric acid iron powder and ammonia;Catalyst and reducing agent are added in sulfuric acid iron powder again, after being well mixed, decomposition in high-temperature heat-exchanging is added and obtains high concentration sulfur oxide gas and brown iron oxide, valuable metal is reclaimed from brown iron oxide.The present invention can individually reclaim ammonia, sulfur oxide and brown iron oxide, compared with prior art scheme, and this method can save production cost, reduce energy consumption, improve efficiency.
Description
Technical field
The present invention relates to the recycling field of iron vitriol slag, and in particular to a kind of iron vitriol slag low-temperature decomposition and is separately recovered
The method of resource.
Background technology
Nearly ten years, China's lead zinc metallurgy maintains the impetus of rapid growth, and 2010, lead zinc total output reached 958.10
Ten thousand tons.Wet processing Sheng electricity zinc factory for producing 100000 tons per year, if zinc concentrate iron content is in terms of 8%, the yellow ammonium iron of annual output
Alum (iron vitriol slag) is about 5.3 ten thousand tons, and [Chen Yongming, Tang Motang, the interim state's non-ferrous metal journal Yang Sheng seas of volume 19 the 7th, wait .NaOH
Decompose the new technology of iron vitriol slag containing indium [J] China YouSe Acta Metallurgica Sinicas, 2009,19 (7):1322-1331].China's lead zinc metal production
Amount occupies the first in the world for years.While product production capacity is developed rapidly, the processing of the ammonium jarosite in production process
Problem is progressively shown especially, is not only related to the comprehensive cyclic utilization of resource, and is more related to the influence to natural environment.
According to the thermal property of ammonium jarosite, thermally decomposed in heating up process, the product that different temperatures is decomposed is not
Together, following reaction equation:
[Qiu electricity Yun, Ma Rongjun hot acids leach processing method [J] Hunan's nonferrous metals of iron vitriol slag in zinc hydrometallurgy,
1994,10 (3):158-162].Therefore, by ammonium jarosite in high-temperature calcination, recyclable ammonia, sulfur oxide and iron oxide.
In addition, ammonium jarosite is after (400 DEG C) of low temperature is decomposed, obtained intermediate product, its thing mutually also not it is clear that some
Document is named as sulphur iron slag;Because of the related substances of the main sulfur acid iron of intermediate product, intermediate product is named by the application
For sulfuric acid iron powder.
Patent of invention refined et al. Tan Hong, discloses the technique that sulphur is reclaimed in ammonium jarosite, including (1) uses Lead And Zinc Smelter
As raw material, wherein adding additive, binder, atmosphere adjusting agent, water, after stirring, ball is made in the ammonium jarosite of generation
Shape particle;(2) spherical particle is sent into column heat-treatment furnace, aoxidized in 700~900 DEG C of reactions by oscillating feeder
Iron byproduct, the vibration discharging machine through burner hearth under shed bottom is directly collected;The exhaust outlet that the flue gas of generation passes through roof of the furnace
Discharge, after the pickle liquor in Lead-Zinc Sintering Process absorbs, send sulfuric acid to prepare workshop, reclaims sulphur;(3) by the iron oxide being collected into
With industrial raw iron oxide material is obtained after grinding, washing, drying, [Tan Hongbin, horse Xiao Ling, Hou little Qiang wait from yellow ammonium iron to byproduct
Technique [P] number of patent applications of sulphur are reclaimed in alum:201310397438.3].
The flue gas that the patent column heat-treatment furnace is produced, due to the gas containing partial air and atmosphere adjusting agent generation,
The concentration of sulfur oxide is relatively low in flue gas, and influence prepares the efficiency of sulfuric acid, increases the cost of sulfuric acid.
The content of the invention
To solve the problem of prior art is present, the invention provides a kind of iron vitriol slag low-temperature decomposition and resource is separately recovered
Method, the present invention can individually reclaim ammonia, sulfur oxide and brown iron oxide, compared with prior art scheme, and this method can be saved
Production cost, reduces energy consumption, improves efficiency.
To achieve the above objectives, this invention takes following technical scheme:
A kind of iron vitriol slag low-temperature decomposition and the method that resource is separately recovered, comprise the following steps:
Iron vitriol slag is subjected to predecomposition in 400~450 DEG C of cryogenic heat exchanger, fully reaction obtains sulfuric acid iron powder and ammonia
Gas, collects ammonia;Catalyst and reducing agent are added in sulfuric acid iron powder again, after being well mixed, 500~600 DEG C of high temperature is added
Decomposition reaction in heat exchanger, fully reaction obtain sulfur oxide gas and brown iron oxide, collect sulfur oxide gas and brown iron oxide, from
Valuable metal is reclaimed in brown iron oxide;Wherein, catalyst is cupric oxide, manganese oxide or iron oxide, and addition is iron vitriol slag quality
0.01~0.05%;Reducing agent be zinc sulphide, vulcanized lead, kerosene or bornite, addition for iron vitriol slag quality 15~
20%.
As a further improvement on the present invention, in described cryogenic heat exchanger, the material of heat exchanger tube is stainless steel;High temperature is changed
In hot device, the material of heat exchanger tube is earthenware.
As a further improvement on the present invention, sulfur oxide content is all higher than in the flue gas that described high-temperature heat-exchanging is released
40%.
As a further improvement on the present invention, the ammonia that cryogenic heat exchanger is released is directly used in heavy alum technique, in zinc metallurgy work
Recycled in skill.
As a further improvement on the present invention, reclaiming the sulfur oxide of high-temperature heat-exchanging releasing is used for Sulphuric acid.
As a further improvement on the present invention, the brown iron oxide mass concentration obtained is soaked for 5% ammonium chloride solution
Afterwards, the valuable metal in brown iron oxide is easily reclaimed, the wherein rate of recovery of zinc is more than 90%;Reclaim the iron oxide after valuable metal
Powder, is used as cement plant or the raw material of steel mill.Wherein, the mass ratio of brown iron oxide and ammonium chloride solution is 1:2.
Relative to prior art, the present invention have it is following a little:
In the method for the present invention, segmentation decomposition reaction is carried out, ammonia, sulfur oxide and brown iron oxide can be individually reclaimed;Favorably
Fully reclaimed in resource.Catalyst is especially added in sulfuric acid iron powder, the electronics of catalyst easily passes to sulphur iron slag, burnt
Hexavalent sulfur in slag obtains electronics, is easily changed into tetravalence, is conducive to sulphur iron slag to decompose, and reduces decomposition temperature.Reducing agent with
Sulphur iron slag decomposes the oxygen reaction produced, generates sulfur oxide gas, further improves the concentration of sulfur oxide in sulfur oxide gas,
It can also be decomposed for sulphur iron slag and heat is provided.Iron vitriol slag low-temperature decomposition, is conducive to the recovery of zinc in iron oxide.With prior art side
Case is compared, and this method can save production cost, reduces energy consumption, improves efficiency.The production efficiency and product of sulfuric acid can be significantly improved
Quality, reduces production cost, energy-saving, with significant economic benefit and social benefit.
Heat exchanger, is the column tube bank that placement is erect in shell, material is added in pipe from top, after being decomposed in pipe, Gu
Body is excluded from lower end, and gas is excluded from upper end.The heat smoke that the outer wall of stylostome is produced with coal is heated.Outside due to stylostome
The heat smoke of wall is not contacted with the sulfur oxide gas or ammonia inside stylostome, it is ensured that the concentration of sulfur oxide gas or ammonia
Purity.
The present invention decomposes the sulfur oxide gas produced, and concentration is high, available for Sulphuric acid;The brown iron oxide produced is decomposed, is returned
Receive after valuable metal, cement plant or the raw material of steel mill can be used as.Ammonia reusable edible in smelting process, resource it is further
Make full use of.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1
100Kg iron vitriol slags are subjected to predecomposition in 400 DEG C of cryogenic heat exchanger, sulfuric acid iron powder and ammonia is obtained, decomposed
The ammonia of generation reusable edible in smelting process;Again 0.01Kg catalyst cupric oxide and 15Kg are added in sulfuric acid iron powder also
Former agent vulcanized lead, after being well mixed, adds decomposition in 550 DEG C of high-temperature heat-exchanging and obtains sulfur oxide gas and brown iron oxide, from
Valuable metal is reclaimed in brown iron oxide.Sulfur oxide content is all higher than 40% in the flue gas that high-temperature heat-exchanging is released.Sulfur oxide gas
For Sulphuric acid;After obtained brown iron oxide mass concentration is 5% ammonium chloride solution immersion, having in brown iron oxide is reclaimed
Valency metal, reclaims the brown iron oxide after valuable metal, is used as cement plant or the raw material of steel mill;Wherein, brown iron oxide and ammonium chloride
The mass ratio of solution is 1:2.
Embodiment 2
100Kg iron vitriol slags are subjected to predecomposition in 430 DEG C of cryogenic heat exchanger, sulfuric acid iron powder and ammonia is obtained, decomposed
The ammonia of generation reusable edible in smelting process;Again 0.05Kg catalyst cupric oxide and 20Kg are added in sulfuric acid iron powder also
Former agent vulcanized lead, after being well mixed, adds decomposition in 500 DEG C of high-temperature heat-exchanging and obtains sulfur oxide gas and brown iron oxide.From
Valuable metal is reclaimed in brown iron oxide.Sulfur oxide content is all higher than 40% in the flue gas that high-temperature heat-exchanging is released.Sulfur oxide gas
For Sulphuric acid;After obtained brown iron oxide mass concentration is 5% ammonium chloride solution immersion, having in brown iron oxide is reclaimed
Valency metal, reclaims the brown iron oxide after valuable metal, is used as cement plant or the raw material of steel mill;Wherein, brown iron oxide and ammonium chloride
The mass ratio of solution is 1:2.
Embodiment 3
100Kg iron vitriol slags are subjected to predecomposition in 450 DEG C of cryogenic heat exchanger, sulfuric acid iron powder and ammonia is obtained, decomposed
The ammonia of generation reusable edible in smelting process;Again 0.04Kg catalyst cupric oxide and 16Kg are added in sulfuric acid iron powder also
Former agent vulcanized lead, after being well mixed, adds decomposition in 600 DEG C of high-temperature heat-exchanging and obtains sulfur oxide gas and brown iron oxide.From
Valuable metal is reclaimed in brown iron oxide.Sulfur oxide content is all higher than 40% in the flue gas that high-temperature heat-exchanging is released.Sulfur oxide gas
For Sulphuric acid;After obtained brown iron oxide mass concentration is 5% ammonium chloride solution immersion, having in brown iron oxide is reclaimed
Valency metal, reclaims the brown iron oxide after valuable metal, is used as cement plant or the raw material of steel mill;Wherein, brown iron oxide and ammonium chloride
The mass ratio of solution is 1:2.
Following table is 15 embodiments that numbering is 1-15, and other specific steps lead to embodiment 1.
In all embodiments, analyzed by exhaust gas components, sulfur oxide content is all higher than 40% in flue gas.Iron vitriol slag is decomposed
Obtained brown iron oxide, the mass ratio of valuable metal, wherein brown iron oxide and ammonium chloride solution is reclaimed by 5% ammonium chloride solution
For 1:2, the rate of recovery of zinc is all higher than 90% in embodiment.
Claims (6)
1. a kind of iron vitriol slag low-temperature decomposition and the method that resource is separately recovered, it is characterised in that comprise the following steps:
Iron vitriol slag is subjected to predecomposition in 400~450 DEG C of cryogenic heat exchanger, fully reaction obtains sulfuric acid iron powder and ammonia,
Collect ammonia;Catalyst and reducing agent are added in sulfuric acid iron powder again, after being well mixed, 500~600 DEG C of high temperature heat exchange is added
Decomposition reaction in device, fully reaction obtain sulfur oxide gas and brown iron oxide, sulfur oxide gas and brown iron oxide are collected, from oxidation
Valuable metal is reclaimed in iron powder;Wherein, catalyst is cupric oxide, manganese oxide or iron oxide, and addition is iron vitriol slag quality
0.01~0.05%;Reducing agent is zinc sulphide, vulcanized lead, kerosene or bornite, and addition is the 15~20% of iron vitriol slag quality.
2. a kind of iron vitriol slag low-temperature decomposition according to claim 1 and the method that resource is separately recovered, it is characterised in that institute
In the cryogenic heat exchanger stated, the material of heat exchanger tube is stainless steel;In high-temperature heat-exchanging, the material of heat exchanger tube is earthenware.
3. a kind of iron vitriol slag low-temperature decomposition according to claim 1 and the method that resource is separately recovered, it is characterised in that institute
Sulfur oxide content is all higher than 40% in the flue gas that the high-temperature heat-exchanging stated is released.
4. a kind of iron vitriol slag low-temperature decomposition according to claim 1 and the method that resource is separately recovered, it is characterised in that low
The ammonia that warm heat exchanger is released is directly used in heavy alum technique, is recycled in smelting process.
5. a kind of iron vitriol slag low-temperature decomposition according to claim 1 and the method that resource is separately recovered, it is characterised in that return
Receiving the sulfur oxide of high-temperature heat-exchanging releasing is used for Sulphuric acid.
6. a kind of iron vitriol slag low-temperature decomposition according to claim 1 and the method that resource is separately recovered, it is characterised in that
After the brown iron oxide mass concentration arrived is 5% ammonium chloride solution immersion, the valuable metal in brown iron oxide is reclaimed, recovery has
Brown iron oxide after valency metal, is used as cement plant or the raw material of steel mill;Wherein, the mass ratio of brown iron oxide and ammonium chloride solution is
1:2。
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106865504A (en) * | 2017-01-09 | 2017-06-20 | 西南科技大学 | A kind of method for reclaiming high concentration sulfur oxide gas |
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US4366127A (en) * | 1980-09-30 | 1982-12-28 | Outokumpu Oy | Hydrometallurgical process for the recovery of lead, silver and gold, as well as zinc, from impure jarosite residues of an electrolytic zinc process |
CN102134655A (en) * | 2010-12-29 | 2011-07-27 | 昆明理工大学 | Method for separating zinc and indium and iron from indium-enriched high-iron high-zinc calcine through reduction-magnetic separation |
CN102443701A (en) * | 2010-10-12 | 2012-05-09 | 中国科学院过程工程研究所 | Clean metallurgic comprehensive utilization method of iron vitriol slags |
CN102718267A (en) * | 2012-07-18 | 2012-10-10 | 广西大学 | Method for preparing black iron oxide by utilizing yellow ammonium iron alum slag |
CN103523832A (en) * | 2013-09-04 | 2014-01-22 | 陕西理工学院 | Process for recovering sulfur from ammoniojarosite |
CN103789533A (en) * | 2014-02-11 | 2014-05-14 | 陕西理工学院 | Process for treating iron vanadium slag by virtue of dry-process rotary kiln |
CN105039712A (en) * | 2015-08-14 | 2015-11-11 | 陕西理工学院 | Technology for recycling valuable metal from jarosite slag |
CN106011489A (en) * | 2016-05-23 | 2016-10-12 | 江苏省冶金设计院有限公司 | Iron vitriol slag treatment method |
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2017
- 2017-06-20 CN CN201710471108.2A patent/CN107324358B/en not_active Expired - Fee Related
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
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US4366127A (en) * | 1980-09-30 | 1982-12-28 | Outokumpu Oy | Hydrometallurgical process for the recovery of lead, silver and gold, as well as zinc, from impure jarosite residues of an electrolytic zinc process |
CN102443701A (en) * | 2010-10-12 | 2012-05-09 | 中国科学院过程工程研究所 | Clean metallurgic comprehensive utilization method of iron vitriol slags |
CN102134655A (en) * | 2010-12-29 | 2011-07-27 | 昆明理工大学 | Method for separating zinc and indium and iron from indium-enriched high-iron high-zinc calcine through reduction-magnetic separation |
CN102718267A (en) * | 2012-07-18 | 2012-10-10 | 广西大学 | Method for preparing black iron oxide by utilizing yellow ammonium iron alum slag |
CN103523832A (en) * | 2013-09-04 | 2014-01-22 | 陕西理工学院 | Process for recovering sulfur from ammoniojarosite |
CN103789533A (en) * | 2014-02-11 | 2014-05-14 | 陕西理工学院 | Process for treating iron vanadium slag by virtue of dry-process rotary kiln |
CN105039712A (en) * | 2015-08-14 | 2015-11-11 | 陕西理工学院 | Technology for recycling valuable metal from jarosite slag |
CN106011489A (en) * | 2016-05-23 | 2016-10-12 | 江苏省冶金设计院有限公司 | Iron vitriol slag treatment method |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106865504A (en) * | 2017-01-09 | 2017-06-20 | 西南科技大学 | A kind of method for reclaiming high concentration sulfur oxide gas |
CN106865504B (en) * | 2017-01-09 | 2018-12-28 | 西南科技大学 | A method of recycling high concentration sulfur oxide gas |
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