CN107760873B - A kind of method and apparatus of explosion type acidleach metal alloy compositions - Google Patents
A kind of method and apparatus of explosion type acidleach metal alloy compositions Download PDFInfo
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- CN107760873B CN107760873B CN201710975895.4A CN201710975895A CN107760873B CN 107760873 B CN107760873 B CN 107760873B CN 201710975895 A CN201710975895 A CN 201710975895A CN 107760873 B CN107760873 B CN 107760873B
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- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/065—Nitric acids or salts thereof
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- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- 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
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a kind of method and apparatus of explosion type acidleach metal alloy compositions, belong to resource reclaim with using technical field, can be applied to the acidleach recycling hydrogen technique of the multiple materials alloy such as nickel, cobalt, chromium, zinc, iron.The purpose of the present invention is replace reaction principle using acid concentration and active metal, carry out steam heat triggering starting chain reaction principle, by designing bumping reactor, reaction rate is improved, the heat rationally released using reaction simultaneously utilizes the high concentration hydrogen generated during bumping.Groundwork is design acidleach bumping reactor, expander, steam trigger device and hydrogen purification and recyclable device and linkage valve, control outburst degree and frequency, by the time and the temperature change that rationally determine chain reaction in different-alloy acidleach, keep acid leaching process reaction rapider, more thoroughly.The efficiency and saving heat energy of acidleach work can be improved, and can realize the resource utilization of hydrogen.
Description
Technical field
The invention belongs to resource reclaims and the technical field utilized, and in particular to a kind of explosion type acidleach metal alloy compositions
Method and apparatus, can be applied to the acid leaching process of the material alloys such as nickel, cobalt, chromium, zinc, iron, while the dress of high efficiente callback hydrogen
It sets.
Background technique
Acidleach is separated as a kind of effective method applied to metalliferous mineral, the fields such as material purification.Currently used acid
Soaking technology includes vitriol lixiviation, hydrochloric acid acidleach, nitric acid acidleach etc., and reaction condition is mostly to be heated to 70~150 DEG C, to improve reaction
Rate.The process that metal is reacted with acid is exothermic reaction, key reaction equation M+2HXy=MXz+H2+ Q (heat), acid group
Difference, concentration is different, redox side reaction can occur according to Redox Condition difference.Rationally using during acidleach
The hydrogen that heat and recycling reaction generate can be with effective use of energy sources, and having reduces acid leaching process energy consumption, and resource rationally recycles benefit
Practical significance.
For Leaching Systems, nitric acid system reaction speed is fast, but the nitrogen oxides generated will cause pollution to environment, it is necessary to
Carry out post-processing.Hydrochloric acid system loses very little to the leaching of insoluble metal, but there are volatile, at high cost, operating environment is poor
The disadvantages of.Sulfuric acid system is more widely applied at low cost, good operational environment.
1988, Dai Yuanning (Chinese patent, 86108798A) with dilute sulfuric acid leach crush zinc ore, by zinc ore wet-milling to-
100 mesh, room temperature leach 40~80 minutes, filtration washing after discharging；2007, Hu Guohua (Chinese patent,
200710034327.0) design produces chrome green from carbon ferrochrome, using the sulfuric acid of concentration 20%~60% to carbon
Ferrochrome is dissolved, and 80-150 DEG C of solution temperature, dissolution time 0.5-2h.2008, Han Denglun etc. (Chinese patent,
200810233849.8) with 7~8% dilution heat of sulfuric acid, wash non-calcium chromium slags, 6~8h is stirred at room temperature, it is separately that ferrochrome grinding is thin
Change and be added to -100 mesh~-20 mesh powder in the dilution heat of sulfuric acid that mass fraction is 38~40%, is heated to 90~105 DEG C, it is molten
8~12h is solved, carbon ferrochrome lysate is obtained.
In previous dilute sulfuric acid leaching alloy material, do not consider that exothermic heat of reaction utilizes, and do not carry out hydrogen retrieval work, mainly
Because reaction time is longer, density of hydrogen is low, not easily collecting, and exothermic reaction and external heat energy envelope.
Existing acidleach alloy technology, by reaction controlling in suitable temperature, prevent its bumping overflow, not to bumping work into
Row further research and utilization.
These means form company standard although entering the production routine of enterprise early period, but as China's environment is wanted
Raising and energy saving requirement are asked, these disadvantages have become the restraining factors of current enterprise's production.The high efficiente callback of hydrogen and saving energy
Source has been must sternly requiring for modernization industry, the necessary means of enterprise transformation upgrading.
Summary of the invention
The purpose of the present invention is triggering chain reaction principle using chemical heat release, by designing bumping reactor, with
Reaction rate is improved, the heat rationally released using reaction is collected simultaneously the high concentration hydrogen generated during bumping.Main work
It is not carry out displacement with alloy using the concentrated sulfuric acid to react, and displacement reaction just occurs for dilute sulfuric acid as principle, design acidleach bumping is anti-
Device is answered, steam-type trigger device is set, outburst degree and frequency are controlled in different-alloy acidleach, by rationally determining that chain type is anti-
The time answered and temperature change determine optimal explosion temperature and frequency.The device is equipped with expander and hydrogen outlet when breaking out
Purification device keeps acid leaching process reaction rapider, more thoroughly.The efficiency and saving heat energy of acidleach work can be improved, and can be real
The resource utilization of existing hydrogen.
Method And Principle:
M+2HXy=MXz+H2+ Q (heat)
When metal alloy acid leaching process is carried out to equilibrium temperature, locally heated up using external trigger to solution,
Cause circumferential metal alloy and acutely displacement reaction release hydrogen occurs, while discharging heat, what metal alloy powders surface generated
Hydrogen carries powder and floats to solution top, and heat release causes peripheral temperature to increase during the motion, and local temperature increases triggering
The powder nearby contacted with acid continues to occur acutely to replace to react, and the heat release simultaneously of release hydrogen loops back and forth like this, forms chain type
Reaction, leads to solution bumping；The a large amount of heat of bumping process release triggers itself chain reaction, while discharging a large amount of hydrogen, convenient
It collects.
Bubble carries powder and is gradually accumulated raising, has left liquid surface to the movement of reactor top dead zone, is moved to swollen
In swollen device, volume is not only due in expander and is released, while playing the waste heat effect of steam water, reduce and be detached from solution
The moisture that region is taken away carries out primary dewatering to hydrogen.As liquid volume increases the reduction with temperature, react in solution
Group gradually decrease, chain reaction is controlled；The hydrogen of release is reduced simultaneously, closes hydrogen recovery valve.When in expander
Solution and foam fall back to the bottom of reactor, when liquor capacity restores substantially, be passed through steam again and carry out next triggering,
Cause bumping chain reaction, and opens the recycling valve of hydrogen.Repeatedly triggering can be achieved, reach and improve reaction efficiency and collect hydrogen
The purpose of gas.
Hydrogen recycling recycles hydrogen after water cooling primary cooling, using the dehydration of calcium oxide second level, and concentration can achieve
90% or more.
Based on principles above, explosive reaction device and explosion type reaction method are designed.
Technical solution of the present invention:
A kind of device of explosion type acidleach metal alloy compositions, which is characterized in that the device includes steam generator
1, inlet opening 2, feed opening 3, agitating device 4, gas cleaning plant 5, condenser 6, defoaming paddle 7, heating mantle 8, aeration head are condensed
9, the first valve 10a, the second valve 10b and discharge port 11；Outburst device is divided into lower reaction zone and top defoaming falls area after rise, under
The sectional area of portion's reaction zone is 4 times of the sectional area that top defoaming falls area after rise, and the total volume of lower reaction zone is that top defoams back
The total volume 1/4 settled in an area；The lower reaction zone of outburst device is surrounded by the heating mantle 8 of half-packaging；Break out bottom of device and side wall
It is respectively equipped with discharge port 11 and steam generator entrance, steam generator entrance is controlled by the second valve 10b by steam generation
The steam flow that device 1 generates；Condensation inlet opening 2 and feed opening 3 are respectively equipped at the top of outburst device, condensation inlet opening 2 is connected to
Condenser 6；The hydrogen in device is broken out after 6 primary dewatering of condenser, and alkali is sequentially entered by the first valve 10a control
Property filler filter bed 5a and calcium oxide adsorbent bed 5b is collected after being further processed；
It breaks out bottom of device inner wall and is equipped with multiple aeration heads 9；The top defoaming that agitating device 4 stretches to outburst device is fallen after rise
Area is equipped with defoaming paddle 7 thereon.
A kind of method of explosion type acidleach metal alloy compositions, steps are as follows:
Alloy material is ground into 50~200 mesh powders, with defoaming fall after rise area outburst device in be added powder with
Concentrated acid adds 3g powder in every ml concentrated acid, after thorough impregnation wetting；It is passed through high steam, starting displacement reaction again；Break out device
It is passed through the high-temperature steam that temperature is 150~300 DEG C, causes chain reaction；
Moment has a large amount of hydrogen to generate after displacement reaction starting, and solution and foam increase to 3~7 times of original volumes, steep
Foam layer rises to defoaming falling area and is defoamed, and high concentration hydrogen is overflowed；
Defoaming falls the multiple defoaming paddles 7 being arranged in area after rise, and the foam of rising is smashed；
Defoaming falls area top after rise and is used to cool down equipped with condenser 6, so that primary dewatering after the vapor condensation in hydrogen, just
The dewatered gas of grade is passed into alkaline filler filter bed 5a, removes sour gas, then pass through calcium oxide adsorbent bed 5b second dehydration,
After so that the concentration of hydrogen is greater than 93%, it is compressed in air collector and recycles；
Automatic valve is set on the pipeline for collecting hydrogen, the automatic valve on automatic valve and steam generator 1 links,
Can repeatedly it be started automatically using the two linkage；
The water inlet of steam generator 1 carries out heat recovery by the condenser 6 that defoaming falls area after rise, realizes lower
The purpose with high concentration hydrogen recycling is quickly dissolved under energy consumption.
The alloy material is aluminium, iron, zinc, tin, chromium, vanadium, manganese, nickel, the two or more mixing in cobalt, containing 30% with
Under inert substance.
Acid used is sulfuric acid and/or nitric acid when the described alloy material acidleach.
Beneficial effects of the present invention: the present invention utilizes concentrated acid dipping, the reaction of activated vapor explosion type, expander release recycling
High concentration hydrogen；Wherein in device other than being equipped with heat recovery and hydrogen drying system for hydrogen, it is equipped with activated vapor and expansion cools down
It controls linked system operation and realizes chain type explosive reaction.This method is reacted using explosion type, and it is same that alloy leaching efficiency can be improved
When, the concentration of release hydrogen is improved, recycling hydrogen is conducive to；And can using reaction release heat and vapour system link into
Row chain reaction improves in environmental standard and energy saving aspect has extensive promotional value.
Detailed description of the invention
Fig. 1 is explosion type reactor schematic diagram.
Fig. 2 is gas chromatogram.
In figure: 1 steam generator；2 condensation inlet openings；3 feed openings；4 agitating devices；
5 gas cleaning plants；6 condensers；7 defoaming paddles；8 heating mantles；9 aeration heads；
The first valve of 10a；The second valve of 10b；11 discharge ports；5a alkaline filler filter bed；5b calcium oxide adsorbent bed.
Specific embodiment
Below with reference to technical solution and attached drawing, a specific embodiment of the invention is further illustrated.
Embodiment 1: hydrogen manufacturing is dissolved in scrap iron alloy acidleach
120g scrap iron alloy is taken, is placed in destructor, 700ml deionized water is added, is slowly injected into 300ml98% sulphur
Acid is warming up to 75 DEG C, is passed through 150 DEG C of distilled water 1 minute, and chain reaction starts, and collects hydrogen in Hydrogen collection mouth, stops additional
Heat, monitoring destructor temperature are slowly raised to 93 DEG C from 75 DEG C, and liquor capacity progressivelyes reach destructor 2/3 from 1L bumping
Place, for about 20 minutes, temperature was gradually decrease to 75 DEG C for chain reaction, carries out second and breaks out, and reciprocal 3 times, time-consuming about 1 is small
When, alloy leaching rate about 95%, and the hydrogen containing 96% or more is collected, see Fig. 2.It has obtained various metallic solutions and has carried out substep
Precipitating can recycle wherein iron and other noble metals.
Embodiment 2: carbon ferrochrome alloy acidleach hydrogen manufacturing
120g carbon ferrochrome is taken, is placed in destructor, 700ml deionized water is added, is slowly injected into 300ml98% sulphur
Acid is warming up to 75 DEG C, is passed through 150 DEG C of distilled water 1 minute, and chain reaction starts, and collects hydrogen in Hydrogen collection mouth, stops additional
Heat, monitoring destructor temperature are slowly raised to 93 DEG C from 75 DEG C, and liquor capacity progressivelyes reach destructor 2/3 from 1L bumping
Place, for about 20 minutes, temperature was gradually decrease to 75 DEG C for chain reaction, carries out second and breaks out, and reciprocal 3 times, time-consuming about 1 is small
When, alloy leaching rate about 90%, waste residue is mainly undissolved carbon, dissolution part can carry out part using extraction, precipitating and
The methods of absorption carries out valuable element recycling, after carbon dioxide and sulfurous gas have passed through solution purification and calcium oxide dehydration, and
Collect the hydrogen containing 98% or more.
Claims (4)
1. a kind of device of explosion type acidleach metal alloy compositions, which is characterized in that the device includes steam generator
(1), condense inlet opening (2), feed opening (3), agitating device (4), gas cleaning plant (5), condenser (6), defoaming paddle (7),
Heating mantle (8), aeration head (9), electronic switch (10) and discharge port (11)；Outburst device is divided into lower reaction zone and top defoaming
Fall area after rise, the sectional area of lower reaction zone is 4 times of the sectional area that top defoaming falls area after rise, on the total volume of lower reaction zone is
Portion's defoaming falls the total volume 1/4 in area after rise；The lower reaction zone for breaking out device is surrounded by the heating mantle (8) of half-packaging；Break out device
Bottom and side wall is respectively equipped with discharge port (11) and steam generator entrance, and steam generator entrance passes through the second valve (10b)
Control the steam flow generated by steam generator (1)；Condensation inlet opening (2) and feed opening are respectively equipped at the top of outburst device
(3), condensation inlet opening (2) is connected to condenser (6)；The hydrogen in device is broken out after condenser (6) primary dewatering, is passed through
First valve (10a) control sequentially enters alkaline filler filter bed (5a) and calcium oxide adsorbent bed (5b) be further processed after receive
Collection；
It breaks out bottom of device inner wall and is equipped with multiple aeration heads (9)；The top defoaming that agitating device (4) stretches to outburst device is fallen after rise
Area is equipped with defoaming paddle (7) thereon.
2. a kind of method of explosion type acidleach metal alloy compositions, which is characterized in that steps are as follows:
Alloy material is ground into 50~200 mesh powders, powder and concentrated acid are added in the outburst device for falling area after rise with defoaming,
3g powder is added in every ml concentrated acid, after thorough impregnation wetting；It is passed through high steam, starting displacement reaction again；Outburst device is passed through
The high-temperature steam that temperature is 150~300 DEG C causes chain reaction；
Moment has a large amount of hydrogen to generate after displacement reaction starting, and solution and foam increase to 3~7 times of original volumes, froth bed
It rises to defoaming falling area to be defoamed, high concentration hydrogen is overflowed；
Defoaming falls the multiple defoaming paddles (7) being arranged in area after rise, and the foam of rising is smashed；
Defoaming falls area top after rise and is used to cool down equipped with condenser (6), so that primary dewatering after the vapor condensation in hydrogen, primary
Dewatered gas is passed into alkaline filler filter bed (5a), removes sour gas, then secondary de- by calcium oxide adsorbent bed (5b)
Water is compressed in air collector and recycles after so that the concentration of hydrogen is greater than 93%；
Automatic valve, the automatic valve couplet on the door on the automatic valve and steam generator (1) are set on the pipeline for collecting hydrogen
It is dynamic, can repeatedly it be started automatically using the two linkage；
Steam generator (1) water inlet carries out heat recovery by the condenser (6) that defoaming falls area after rise, realizes lower
The purpose with high concentration hydrogen recycling is quickly dissolved under energy consumption.
3. according to the method described in claim 2, it is characterized in that, the alloy material be aluminium, iron, zinc, tin, chromium, vanadium,
Manganese, nickel, the two or more mixing in cobalt, contain 30% inert substance below.
4. according to the method in claim 2 or 3, which is characterized in that acid used is sulphur when the described alloy material acidleach
Acid and/or nitric acid.
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| CN201710975895.4A CN107760873B (en) | 2017-10-19 | 2017-10-19 | A kind of method and apparatus of explosion type acidleach metal alloy compositions |
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| CN107760873B true CN107760873B (en) | 2019-02-01 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010009530A1 (en) * | 2008-07-24 | 2010-01-28 | Hatch Ltd. | Method and apparatus for temperature control in a reactor vessel |
| CN102605179A (en) * | 2012-02-24 | 2012-07-25 | 武汉理工大学 | Acid leaching equipment for vanadium-containing shales |
| JP2013194315A (en) * | 2012-03-22 | 2013-09-30 | Dowa Eco-System Co Ltd | Method for recovering valuable material from lithium ion secondary battery |
| CN105695737A (en) * | 2016-04-08 | 2016-06-22 | 金川集团股份有限公司 | Concentrated acid leaching reactor |
| CN105970006A (en) * | 2016-07-07 | 2016-09-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium dioxide through high-iron-oxide titanium concentrate |
-
2017
- 2017-10-19 CN CN201710975895.4A patent/CN107760873B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010009530A1 (en) * | 2008-07-24 | 2010-01-28 | Hatch Ltd. | Method and apparatus for temperature control in a reactor vessel |
| CN102605179A (en) * | 2012-02-24 | 2012-07-25 | 武汉理工大学 | Acid leaching equipment for vanadium-containing shales |
| JP2013194315A (en) * | 2012-03-22 | 2013-09-30 | Dowa Eco-System Co Ltd | Method for recovering valuable material from lithium ion secondary battery |
| CN105695737A (en) * | 2016-04-08 | 2016-06-22 | 金川集团股份有限公司 | Concentrated acid leaching reactor |
| CN105970006A (en) * | 2016-07-07 | 2016-09-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium dioxide through high-iron-oxide titanium concentrate |
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