CN107760873A - 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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- CN107760873A CN107760873A CN201710975895.4A CN201710975895A CN107760873A CN 107760873 A CN107760873 A CN 107760873A CN 201710975895 A CN201710975895 A CN 201710975895A CN 107760873 A CN107760873 A CN 107760873A
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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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Abstract
The invention provides a kind of method and apparatus of explosion type acidleach metal alloy compositions, belongs to resource reclaim and utilizes technical field, can be applied to the acidleach recovery hydrogen technique of the multiple material alloy such as nickel, cobalt, chromium, zinc, iron.The purpose of the present invention is to utilize acid concentration and active metal displacement reaction principle, carry out steam heat triggering and start chain reaction principle, by designing bumping reactor, reaction rate is improved, rationally utilization reacts liberated heat and utilizes caused high concentration hydrogen during bumping.Groundwork is design acidleach bumping reactor, expander, steam trigger device and hydrogen cleaning and retracting device and linkage valve, outburst degree and frequency are controlled in different-alloy acidleach, by the time and the temperature change that rationally judge chain reaction, make acid leaching process reaction rapider, more thoroughly.The efficiency and saving heat energy of acidleach work can be improved, and the recycling of hydrogen can be realized.
Description
Technical field
The invention belongs to resource reclaim 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
Put.
Background technology
Acidleach separates as a kind of effective method applied to metalliferous mineral, the field 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
Speed.The process of metal and acid reaction 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 is different.Rationally using during acidleach
Hydrogen caused by heat and recovery reaction can be with effective use of energy sources, and having reduces acid leaching process energy consumption, and resource rationally reclaims profit
Practical significance.
For Leaching Systems, nitric acid system reaction speed is fast, but caused nitrogen oxides can pollute to environment, it is necessary to
Carry out post-processing.Leaching loss very little of the hydrochloric acid system to insoluble metal, but have that volatile, cost is high, operating environment is poor
The shortcomings of.Sulfuric acid system is low to cost, good operational environment, is more widely applied.
1988, Dai Yuanning (Chinese patent, 86108798A) with dilute sulfuric acid leach crush zinc ore, by zinc ore wet-milling to-
100 mesh, normal 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, 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 to the mesh powder of -100 mesh~-20, be added in the dilution heat of sulfuric acid that mass fraction is 38~40%, be heated to 90~105 DEG C, it is molten
8~12h is solved, obtains carbon ferrochrome lysate.
In conventional 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 from overflowing, bumping is not worked into
Row further research and utilization.
These means form company standard although entering the production routine of enterprise early stage, but as China's environment will
Raising and energy saving requirement are asked, these shortcomings have turned into the restraining factors of current enterprise 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.
The content of the invention
The purpose of the present invention is to trigger chain reaction principle using chemical heat release, by designing bumping reactor, with
Reaction rate is improved, rationally utilizes and reacts liberated heat, while collect caused high concentration hydrogen during bumping.Main work
It is not enter line replacement reaction with alloy using the concentrated sulfuric acid as principle, and displacement reaction just occurs for dilute sulfuric acid, 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 judging that chain type is anti-
The time answered and temperature change, determine optimal explosion temperature and frequency.Arranged outside expander and hydrogen when the device is provided with outburst
Purifier, make acid leaching process reaction rapider, more thoroughly.The efficiency and saving heat energy of acidleach work can be improved, and can be real
The recycling of existing hydrogen.
Method And Principle：
M+2HXy=MXz+H2+ Q (heat)
When metal alloy acid leaching process is carried out to equilibrium temperature, solution is locally heated up using external trigger,
Trigger circumferential metal alloy that acutely displacement reaction release hydrogen, while discharge heat occurs, caused by metal alloy powders surface
Hydrogen carry powder to solution top float, in motion process heat release cause peripheral temperature to raise, local temperature rise triggering
The powder nearby contacted with acid continues to occur acutely displacement and reacted, and the heat release simultaneously of release hydrogen, so moves in circles, forms chain type
Reaction, causes solution bumping；The substantial amounts of heat of bumping process release triggers itself chain reaction, while discharges a large amount of hydrogen, convenient
Collect.
Bubble carries powder and gradually accumulates rise, have left liquid surface and is moved to reactor top dead zone, is moved to swollen
In swollen device, in expander being not only due to volume is released, while plays the waste heat effect of steam water, reduces and departs from solution
The moisture that region is taken away, primary dewatering is carried out to hydrogen.With liquid volume increase and the reduction of temperature, reacted 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 recovers substantially, be passed through steam again and carry out next triggering,
Trigger bumping chain reaction, and open the recovery valve of hydrogen.Repeatedly triggering can be achieved, reach raising reaction efficiency and collect hydrogen
The purpose of gas.
Hydrogen recovery reclaims hydrogen after water cooling primary cooling, using the dehydration of calcium oxide two level, and concentration can reach
More than 90%.
Based on principles above, explosive reaction device and explosion type reaction method are designed.
Technical scheme：
A kind of device of explosion type acidleach metal alloy compositions, it is characterised in that described device includes steam generator
1st, inlet opening 2, charge door 3, agitating device 4, gas cleaning plant 5, condenser 6, defoaming oar 7, heating mantle 8, aeration head are condensed
9th, electronic switch 10 and discharging opening 11；Outburst device is divided into lower reaction zone and top defoaming falls area after rise, and lower reaction zone is cut
Area is 4 times of the sectional area that top defoaming falls area after rise, and the cumulative volume of lower reaction zone is the cumulative volume that top defoaming falls area after rise
1/4；The lower reaction zone of outburst device is surrounded by the heating mantle 8 of half-packaging；Outburst bottom of device and side wall are respectively equipped with discharging
Mouth 11 and steam generator entrance, steam generator entrance pass through the second valve 10b and control the steam as caused by steam generator 1
Flow；Condensation inlet opening 2 and charge door 3 are respectively equipped with the top of outburst device, condensation inlet opening 2 is connected to condenser 6；Outburst dress
Hydrogen in putting after the primary dewatering of condenser 6, by the first valve 10a controls sequentially enter alkaline filler filter bed 5a and
Calcium oxide adsorbent bed 5b is collected after further handling；
Outburst bottom of device inwall is provided with multiple aeration heads 9；The top defoaming that agitating device 4 stretches to outburst device falls after rise
Area, defoaming oar 7 is installed thereon.
A kind of method of explosion type acidleach metal alloy compositions, step are as follows：
Alloy material is ground into 50~200 mesh powders, with defoaming fall after rise area outburst device in add powder with
Concentrated acid, 3g powders are often added in ml concentrated acids, after thorough impregnation wetting；High steam is passed through again, starts displacement reaction；Break out device
The high-temperature steam that temperature is 150~300 DEG C is passed through, triggers chain reaction；
Moment has a large amount of hydrogen to produce after displacement reaction starts, and solution and foam increase to 3~7 times of original volumes, steeps
Foam layer rises to defoaming falling area and defoamed, and high concentration hydrogen is overflowed；
Defoaming falls the multiple defoaming oars 7 set in area after rise, and the foam of rising is smashed；
Defoaming falls area top after rise and is provided with condenser 6 for cooling so that primary dewatering after the water vapor condensation in hydrogen, just
Gas after level dehydration is passed into alkaline filler filter bed 5a, removes sour gas, then by calcium oxide adsorbent bed 5b second dehydrations,
After the concentration of hydrogen is more than 93%, it is compressed in air collector and reclaims；
Automatic valve is set on the pipeline for collecting hydrogen, automatic valve links with the automatic valve on steam generator 1,
Linked and can repeatedly started automatically using both；
The condenser 6 that the described water inlet of steam generator 1 falls area after rise by defoaming carries out heat recovery, realizes relatively low
The purpose of quick dissolving and high concentration hydrogen recovery under energy consumption.
Described alloy material is the two or more mixing in aluminium, iron, zinc, tin, chromium, vanadium, manganese, nickel, cobalt, containing 30% with
Under inert substance.
Acid used is sulfuric acid and/or nitric acid during 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 recovery
High concentration hydrogen；Wherein in device in addition to provided with heat recovery and hydrogen drying system for hydrogen, cooled down provided with activated vapor and expansion
Chain type explosive reaction is realized in control linked system operation.This method is reacted using explosion type, and it is same can to improve alloy leaching efficiency
When, the concentration for discharging hydrogen is improved, beneficial to recovery hydrogen；And can utilize react liberated heat and vapour system link into
Row chain reaction, there is extensive promotional value in terms of environmental standard improves and saves the energy.
Brief description of the drawings
Fig. 1 is explosion type reactor schematic diagram.
Fig. 2 is gas chromatogram.
In figure：1 steam generator；2 condensation inlet openings；3 charge doors；4 agitating devices；
5 gas cleaning plants；6 condensers；7 defoaming oars；8 heating mantles；9 aeration heads；10 electronic switches；
11 discharging openings；5a alkaline filler filter beds；5b calcium oxide adsorbent beds；The valves of 10a first；
The valves of 10b second.
Embodiment
With reference to technical scheme and accompanying drawing, embodiment of the invention is further illustrated.
Embodiment 1：Hydrogen manufacturing is dissolved in the acidleach of scrap iron alloy
120g scrap iron alloys are taken, are placed in destructor, 700ml deionized waters is added, is slowly injected into 300ml98% sulphur
Acid, 75 DEG C are warming up to, are passed through 150 DEG C of distilled water 1 minute, 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 bumpings
Place, chain reaction last about 20 minutes, and temperature is gradually decrease to 75 DEG C, carry out second and break out, and reciprocal 3 times, it is small to take about 1
When, alloy leaching rate about 95%, and collect containing more than 96% hydrogen, see Fig. 2.Obtain various metallic solutions and carry out substep
Precipitation can reclaim wherein iron and other noble metals.
Embodiment 2：Carbon ferrochrome alloy acidleach hydrogen manufacturing
120g carbon ferrochromes are taken, are placed in destructor, 700ml deionized waters is added, is slowly injected into 300ml98% sulphur
Acid, 75 DEG C are warming up to, are passed through 150 DEG C of distilled water 1 minute, 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 bumpings
Place, chain reaction last about 20 minutes, and temperature is gradually decrease to 75 DEG C, carry out second and break out, and reciprocal 3 times, it is small to take about 1
When, alloy leaching rate about 90%, waste residue is mainly undissolved carbon, dissolving part can carry out part using extraction, precipitation and
The methods of absorption, carries out valuable element recovery, after carbon dioxide and sulfurous gas have passed through solution purification and calcium oxide dehydration, and
Collection contains more than 98% hydrogen.
Claims (4)
1. a kind of device of explosion type acidleach metal alloy compositions, it is characterised in that described device includes steam generator
(1), condense inlet opening (2), charge door (3), agitating device (4), gas cleaning plant (5), condenser (6), defoaming oar (7),
Heating mantle (8), aeration head (9), electronic switch (10) and discharging opening (11)；Outburst device is divided into lower reaction zone and top defoaming
Fall area after rise, the sectional area of lower reaction zone falls 4 times of the sectional area in area after rise for top defoaming, on the cumulative volume of lower reaction zone is
Portion's defoaming falls the cumulative 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 are respectively equipped with discharging opening (11) and steam generator entrance, and steam generator entrance passes through the second valve (10b)
Control steam flow as caused by steam generator (1)；Condensation inlet opening (2) and charge door are respectively equipped with 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 is received after sequentially entering alkaline filler filter bed (5a) and the further processing of calcium oxide adsorbent bed (5b)
Collection；
Outburst bottom of device inwall is provided with multiple aeration heads (9)；The top defoaming that agitating device (4) stretches to outburst device falls after rise
Area, defoaming oar (7) is installed thereon.
A kind of 2. method of explosion type acidleach metal alloy compositions, it is characterised in that step is 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 powders are added in per ml concentrated acids, after thorough impregnation wetting；High steam is passed through again, starts displacement reaction；Outburst device is passed through
Temperature is 150~300 DEG C of high-temperature steam, triggers chain reaction；
Moment has a large amount of hydrogen to produce after displacement reaction starts, and solution and foam increase to 3~7 times of original volumes, froth bed
Rise to defoaming falling area to be defoamed, high concentration hydrogen is overflowed；
Defoaming falls the multiple defoaming oars (7) set in area after rise, and the foam of rising is smashed；
Defoaming falls area top after rise and is provided with condenser (6) for cooling so that primary dewatering after the water vapor condensation in hydrogen, it is primary
Gas after dehydration is passed into alkaline filler filter bed (5a), removes sour gas, then secondary de- by calcium oxide adsorbent bed (5b)
Water, after the concentration of hydrogen is more than 93%, it is compressed in air collector and reclaims；
Automatic valve is set on the pipeline for collecting hydrogen, and automatic valve links with the automatic valve on steam generator (1), profit
Linked and can repeatedly started automatically with both；
The condenser (6) that described steam generator (1) water inlet falls area after rise by defoaming carries out heat recovery, realizes relatively low
The purpose of quick dissolving and high concentration hydrogen recovery under energy consumption.
3. according to the method for claim 2, it is characterised in that described alloy material be aluminium, iron, zinc, tin, chromium, vanadium,
Two or more mixing in manganese, nickel, cobalt, contain less than 30% inert substance.
4. according to the method in claim 2 or 3, it is characterised in that acid used is sulphur during 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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| 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 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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