CN107324358B - 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
- CN107324358B CN107324358B CN201710471108.2A CN201710471108A CN107324358B CN 107324358 B CN107324358 B CN 107324358B CN 201710471108 A CN201710471108 A CN 201710471108A CN 107324358 B CN107324358 B CN 107324358B
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- 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 methods that resource is separately recovered, it is that iron vitriol slag is carried out to predecomposition in cryogenic heat exchanger, obtains sulfuric acid iron powder and ammonia；Catalyst and reducing agent is added in sulfuric acid iron powder again, after mixing, decomposition in high-temperature heat-exchanging is added and obtains high concentration sulfur oxide gas and brown iron oxide, valuable metal is recycled from brown iron oxide.The present invention can individually recycle ammonia, sulfur oxide and brown iron oxide, and compared with prior art scheme, this method can save production cost, reduce energy consumption, improve efficiency.
Description
Technical field
The present invention relates to the resource utilization fields 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 technique
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.For producing 100000 tons of wet processing Sheng electricity zinc factory per year, if zinc concentrate iron content 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 Shenghai of volume 19 the 7th wait .NaOH
Decompose the new process of iron vitriol slag containing indium [J] China YouSe Acta Metallurgica Sinica, 2009,19 (7): 1322-1331].China's lead zinc metal produces
Amount occupies the first in the world for years.While the rapid development of product production capacity, the processing of the ammonium jarosite in production process
Problem is gradually shown especially, is not only related to the comprehensive cyclic utilization of resource, but also is more related to the influence to natural environment.
It according to the thermal property of ammonium jarosite, is thermally decomposed in heating up process, the product that different temperatures is decomposed is not
Together, following reaction formula:
[Qiu electricity Yun, Ma Rongjun hot acid leach processing method [J] Hunan's nonferrous metals of iron vitriol slag in zinc hydrometallurgy,
1994,10 (3): 158-162].Therefore, ammonia, sulfur oxide and iron oxide is can be recycled into high-temperature calcination in ammonium jarosite.
In addition, ammonium jarosite is after (400 DEG C) of low temperature are decomposed, obtained intermediate product, object is not mutually also 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.
The patent of invention of Tan Hongbin et al. discloses the technique that sulphur is recycled in ammonium jarosite, including (1) uses Lead And Zinc Smelter
The ammonium jarosite of generation is as raw material, wherein additive is added, ball is made after mixing evenly in binder, atmosphere adjusting agent, water
Shape particle；(2) spherical particle is sent into column heat-treatment furnace, is aoxidized in 700~900 DEG C of reactions by oscillating feeder
Iron byproduct, the vibration discharging machine through burner hearth under shed bottom are directly collected；The exhaust outlet that the flue gas of generation passes through roof of the furnace
Discharge after being absorbed by the pickle liquor in Lead-Zinc Sintering Process, send sulfuric acid to prepare workshop, recycles sulphur；(3) iron oxide that will be collected into
Obtaining industrial raw iron oxide material after byproduct grinding, washing, drying, [Tan Hongbin, Ma little Ling, Hou little Qiang wait from yellow ammonium iron
Technique [P] number of patent application of sulphur is recycled in alum: 201310397438.3].
The patent column heat-treatment furnace generate flue gas, due to containing partial air and atmosphere adjusting agent generation gas,
The concentration of sulfur oxide is lower in flue gas, influences the efficiency for preparing sulfuric acid, increases the cost of sulfuric acid.
Summary of the invention
In order to solve the problems existing in the prior art, the present invention provides a kind of iron vitriol slag low-temperature decomposition and resource is separately recovered
Method, the present invention can individually recycle ammonia, sulfur oxide and brown iron oxide, and compared with prior art scheme, this method can be saved
Production cost reduces energy consumption, improves efficiency.
To achieve the above objectives, this invention takes following technical solutions:
A kind of iron vitriol slag low-temperature decomposition and the method that resource is separately recovered, comprising the following steps:
Iron vitriol slag is subjected to predecomposition in 400~450 DEG C of cryogenic heat exchanger, sufficiently reaction obtains sulfuric acid iron powder and ammonia
Gas collects ammonia；Catalyst and reducing agent is added in sulfuric acid iron powder again, after mixing, 500~600 DEG C of high temperature is added
Decomposition reaction in heat exchanger, sufficiently reaction obtain sulfur oxide gas and brown iron oxide, collect sulfur oxide gas and brown iron oxide, from
Valuable metal is recycled in brown iron oxide；Wherein, catalyst is copper oxide, manganese oxide or iron oxide, and additional amount is iron vitriol slag quality
0.01~0.05%；Reducing agent be zinc sulphide, vulcanized lead, kerosene or bornite, additional amount be iron vitriol slag quality 15~
20%.
As a further improvement of the present invention, in the cryogenic heat exchanger, the material of heat exchanger tube is stainless steel；High temperature changes
In hot device, the material of heat exchanger tube is ceramic tube.
As a further improvement of the present invention, sulfur oxide content is all larger than in the flue gas that the high-temperature heat-exchanging is released
40%.
As a further improvement of the present invention, the ammonia that cryogenic heat exchanger is released is directly used in heavy alum technique, in zinc metallurgy work
It is recycled in skill.
As a further improvement of the present invention, the sulfur oxide that recycling high-temperature heat-exchanging is released is used for Sulphuric acid.
As a further improvement of the present invention, the ammonium chloride solution that the brown iron oxide mass concentration obtained is 5% impregnates
Afterwards, the valuable metal being easy in recycling brown iron oxide, wherein the rate of recovery of zinc is greater than 90%；Iron oxide after recycling valuable metal
Powder, 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.
Compared with the existing technology, the present invention have it is following a little:
In method of the invention, segmentation decomposition reaction is carried out, ammonia, sulfur oxide and brown iron oxide can be individually recycled；Favorably
It is sufficiently recycled in resource.Catalyst is especially added in sulfuric acid iron powder, the electronics of catalyst is easy to pass to sulphur iron slag, burns
Hexavalent sulfur in slag obtains electronics, is easy to be changed into tetravalence, is conducive to the decomposition of sulphur iron slag, reduces decomposition temperature.Reducing agent with
Sulphur iron slag decomposes the oxygen reaction generated, generates sulfur oxide gas, further increases 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 recycling of zinc in iron oxide.With prior art side
Case is compared, and this method can save production cost, is reduced energy consumption, is improved efficiency.The production efficiency and product of sulfuric acid can be significantly improved
Quality reduces production cost, energy-saving, has significant economic benefit and social benefit.
Heat exchanger, for the column tube bank for erectting placement 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 outer wall of stylostome is heated with the hot fume that coal generates.Outside due to stylostome
The hot fume of wall not with inside stylostome sulfur oxide gas or ammonia contact, ensure that the concentration or ammonia of sulfur oxide gas
Purity.
The present invention decomposes the sulfur oxide gas generated, and concentration is high, can be used for Sulphuric acid；The brown iron oxide generated is decomposed, is returned
After receiving valuable metal, the raw material of cement plant or steel mill can be used as.Ammonia in smelting process can be recycled, resource it is further
It makes full use of.
Specific embodiment
Below in conjunction with specific embodiment, invention is further described in detail.
Embodiment 1
100Kg iron vitriol slag is subjected to predecomposition in 400 DEG C of cryogenic heat exchanger, obtains sulfuric acid iron powder and ammonia, is decomposed
The ammonia of generation can be recycled in smelting process；0.01Kg catalyst copper oxide and 15Kg is added also in sulfuric acid iron powder again
Former agent vulcanized lead is added decomposition in 550 DEG C of high-temperature heat-exchanging and obtains sulfur oxide gas and brown iron oxide after mixing, from
Valuable metal is recycled in brown iron oxide.Sulfur oxide content is all larger than 40% in the flue gas that high-temperature heat-exchanging is released.Sulfur oxide gas
For Sulphuric acid；After the ammonium chloride solution that obtained brown iron oxide mass concentration is 5% impregnates, having in brown iron oxide is recycled
Valence metal, the brown iron oxide after recycling valuable metal, 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 slag is subjected to predecomposition in 430 DEG C of cryogenic heat exchanger, obtains sulfuric acid iron powder and ammonia, is decomposed
The ammonia of generation can be recycled in smelting process；0.05Kg catalyst copper oxide and 20Kg is added also in sulfuric acid iron powder again
Former agent vulcanized lead is added decomposition in 500 DEG C of high-temperature heat-exchanging and obtains sulfur oxide gas and brown iron oxide after mixing.From
Valuable metal is recycled in brown iron oxide.Sulfur oxide content is all larger than 40% in the flue gas that high-temperature heat-exchanging is released.Sulfur oxide gas
For Sulphuric acid；After the ammonium chloride solution that obtained brown iron oxide mass concentration is 5% impregnates, having in brown iron oxide is recycled
Valence metal, the brown iron oxide after recycling valuable metal, 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 slag is subjected to predecomposition in 450 DEG C of cryogenic heat exchanger, obtains sulfuric acid iron powder and ammonia, is decomposed
The ammonia of generation can be recycled in smelting process；0.04Kg catalyst copper oxide and 16Kg is added also in sulfuric acid iron powder again
Former agent vulcanized lead is added decomposition in 600 DEG C of high-temperature heat-exchanging and obtains sulfur oxide gas and brown iron oxide after mixing.From
Valuable metal is recycled in brown iron oxide.Sulfur oxide content is all larger than 40% in the flue gas that high-temperature heat-exchanging is released.Sulfur oxide gas
For Sulphuric acid；After the ammonium chloride solution that obtained brown iron oxide mass concentration is 5% impregnates, having in brown iron oxide is recycled
Valence metal, the brown iron oxide after recycling valuable metal, 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 number is 1-15, other specific steps lead to embodiment 1.
It in all embodiments, is analyzed by exhaust gas components, sulfur oxide content is all larger than 40% in flue gas.Iron vitriol slag decomposes
Obtained brown iron oxide recycles valuable metal by 5% ammonium chloride solution, wherein the mass ratio of brown iron oxide and ammonium chloride solution
For 1:2, the rate of recovery of zinc is all larger than 90% in embodiment.
Claims (6)
1. a kind of iron vitriol slag low-temperature decomposition and the method that resource is separately recovered, which comprises the following steps:
Iron vitriol slag is subjected to predecomposition in 400~450 DEG C of cryogenic heat exchanger, sufficiently reaction obtains sulfuric acid iron powder and ammonia,
Collect ammonia；Catalyst and reducing agent is added in sulfuric acid iron powder again, after mixing, 500~600 DEG C of high temperature heat exchange is added
Decomposition reaction in device, sufficiently reaction obtain sulfur oxide gas and brown iron oxide, sulfur oxide gas and brown iron oxide are collected, from oxidation
Valuable metal is recycled in iron powder；Wherein, catalyst is copper oxide, manganese oxide or iron oxide, and additional amount is iron vitriol slag quality
0.01~0.05%；Reducing agent is zinc sulphide, vulcanized lead, kerosene or bornite, and additional amount 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, which is characterized 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 ceramic tube.
3. a kind of iron vitriol slag low-temperature decomposition according to claim 1 and the method that resource is separately recovered, which is characterized in that institute
Sulfur oxide gas content is all larger 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, which is characterized in that low
The ammonia that warm heat exchanger is released is directly used in heavy alum technique, recycles 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, which is characterized in that return
It receives the sulfur oxide that high-temperature heat-exchanging is released and 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, which is characterized in that
After the ammonium chloride solution that the brown iron oxide mass concentration arrived is 5% impregnates, the valuable metal in brown iron oxide is recycled, recycling has
Brown iron oxide after valence metal, 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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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
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 |
|---|---|---|---|---|
| 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 |
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