CN105838902B - A kind of method based on self-propagating reaction processing concentrate of lead sulfide ore - Google Patents
A kind of method based on self-propagating reaction processing concentrate of lead sulfide ore Download PDFInfo
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- CN105838902B CN105838902B CN201610204722.8A CN201610204722A CN105838902B CN 105838902 B CN105838902 B CN 105838902B CN 201610204722 A CN201610204722 A CN 201610204722A CN 105838902 B CN105838902 B CN 105838902B
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
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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
- C22B1/00—Preliminary treatment of ores or scrap
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- 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
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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Abstract
A kind of method based on self-propagating reaction processing concentrate of lead sulfide ore, belongs to Non-ferrous Metallurgy field.It is related to the technological process for proposing lead precipitation calcining using self-propagating reaction water logging removal of impurities thermokalite and preparing lead oxide.It is characterized in that：Concentrate of lead sulfide ore powder after ore dressing and peroxidating sodium powder are thoroughly mixed uniformly, compacting, trigger self-propagating reaction.Product carries out leaching removal of impurities by leaching agent of water after reaction, and leaded enrichment slag leaches lead using hot sodium hydroxide solution, heat filtering, leaded heated alkaline leaching liquid quickly cooled down into precipitation lead hydroxide, calcining and decomposing obtains lead oxide product.The present invention has simple for process, raw material and equipment is common easily obtains and cheap, and the quick low energy consumption of course of reaction, low stain, alkali lye recycle, and realize concentrate of lead sulfide ore greenization clean manufacturing.
Description
Technical field
The invention belongs to Non-ferrous Metallurgy field, at using self-propagating reaction green, quick, low energy consumption
The method that reason concentrate of lead sulfide ore and separation prepare lead oxide.
Background technology
Lead ore raw material is divided into two kinds of sulphide ore and oxide ore, and the lead minerals in sulphide ore is mainly galena (PbS), sulphur
Change the primary raw material that lead ore refines lead now.Concentrate of lead sulfide ore main component be generally w (Pb Zn) 45~75%, w (S) 15~
20%, w (Fe) 2~10%, w (Zn) 2~8%, w (Si) 1~5%, w (Cu) 0.01~1.5%, w (Ca) 0.5~2%, w
(Al) 0.5~2%.The method of lead is extracted from concentrate of lead sulfide ore mainly two kinds, i.e. pyrometallurgical smelting of lead and wet method refining lead.At present,
Wet method refines lead still in conceptual phase, mainly uses Oxidation Leaching method, is served only for small-scale production, contemporary industry produces the side of lead
Method almost all uses pyrometallurgical smelting of lead.
Pyrometallurgical smelting of lead method include it is traditional bake with agglomeration-shaft smelting flow, directly refining splicer's skill and precipitation be molten
Refining method, wherein first two method belong to oxidation-reduction smelting category, and the latter is displacement course of reaction.Oxidation-reduction smelting (patent
201110219664.3) application includes the high-temperature oxydation of vulcanized lead and other sulfide generation oxide in concentrate of lead sulfide ore and adopted
Lead oxide is reduced into metallic lead with suitable reducing agent (such as coke) and collects two steps.Pyrometallurgical smelting of lead is generally using biography at present
- shaft smelting the flow of baking with agglomeration of system, the technique account for more than the 85% of world's production lead amount.The method treating capacity is big, produces
Cheng Wending, but big high energy consumption, returning charge amount, sulfur dioxide trapping recovery difficulty, lead steam and leaded dust polluting environment, labor be present
The problems such as dynamic condition difference.Direct lead smelting process is to release substantial amounts of heat using concentrate of lead sulfide ore rapid oxidation, makes each component in furnace charge
Between take advantage of a situation and complete all metallurgical reaction, process reaction heat is fully used, and metallurgical furnace is closed, using oxygen-enriched or pure
Oxygen is smelted, and output high-concentration sulfur dioxide flue gas is with relieving haperacidity.Though the method improves recovery and the trapping degree of sulphur, equally exist
Technological process is complicated, leaded dust pollution, the problems such as equipment is huge, investment is larger.It is gradual with high-grade lead mineral resources
Exhausted, countries in the world are to the great attention of lead contamination and the development of clean manufacturing and recycling economy, high energy consumption, the pyrogenic process of high pollution
Refining lead technology has started to be restricted in countries in the world.Meanwhile one consumption carbon industry during the oxidation-reduction smelting of concentrate of lead sulfide ore,
Reduce requirement of the energy cost with lowering carbon emission and critical challenges, urgent need exploitation low energy consumption, high efficiency, environment friend are proposed to lead smelting
Good type concentrate of lead sulfide ore smelting technique.
Invention applies self-propagating reaction technology, water logging removal of impurities, alkali extraction lead.Avoid existing pyrogenic process wet processing band
The problems such as high temperature that comes, high pressure, high energy consumption, high cost, complex procedures such as peracid, self-propagating reaction speed is exceedingly fast, and product is stable,
The generation of the sulfur-bearing toxic gas such as sulfur dioxide is avoided, realizes cleanliness without any pollution, is cleaned using water, alkali extraction lead,
The problems such as overcoming the next environment of concentrate of lead sulfide ore HTHP wet-leaching process bands, energy consumption, equipment, has good environment
Economic benefit.The present invention has simple for process, and raw materials used and equipment is common easily to be obtained and cheap, and energy consumption is low, green nothing
Pollution.
The content of the invention
The present invention seeks to the high energy consumption for solving to bring in existing wet method and pyrogenic process lead metallurgical process, high cost, high investment,
The problems such as high pollution, tediously long complex process.Therefore, the present invention be a kind of low power consuming is disclosed, pollution-free, technique is simple, cost is low
The method that concentrate of lead sulfide ore is handled under honest and clean normal temperature and pressure conditionses.
The present invention it has been investigated that：Self-propagating reaction can occur after being mixed with sodium peroxide after igniting for vulcanized lead, reaction
Plumbite is generated, and the sulphur of-divalent is converted into sodium sulphate in self propagating high temperature reaction.Found according to more than, present invention process should
With self-propagating reaction technology, the redox reaction of vulcanized lead and sodium peroxide is set to be carried out by itself chemical energy, without external
Additional-energy is provided, realizes low energy consumption, efficiently quick processing concentrate of lead sulfide ore, while avoids the generation of SOx dusty gas, thoroughly
Solve fume treatment disposal and the problem of environmental pollution that existing roasting technology is brought；Cleaned using water logging, alkali extraction lead, technique mistake
Journey is with more the advantage such as quick, cheap, efficient, low energy consumption, pollution-free.
A kind of method based on self-propagating reaction processing concentrate of lead sulfide ore of the present invention is as follows：
Step 1：Self-propagating reaction
Fine grinding is crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried, 30~200 microns of powder particle size, preferably 74 is micro-
Rice.Then miberal powder and peroxidating sodium powder are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel.Using chemistry
One or more in the methods of igniting, combustion wave igniting, laser ignition, thermal explosion igniting or microwave are lighted a fire ignite method initiation certainly
Sprawling reaction.React once igniting with the spontaneous progress of the waveshape that burns, without providing additional-energy, terminate until reacting.
Particularly, concentrate of lead sulfide ore powder and sodium peroxide mass ratio are 1:1~1:5, it is desirable to thing is carried out in dry environment
Material mixing and compacting process.
PbS+Na2O2→NaxPbOy+Na2SO4
Step 2：Water logging cleans
It is placed in after being reacted in step 1 after product cooling in alkali resistance reaction vessel, carrying out leaching as leaching agent using water removes
Miscellaneous, foreign ion is with ZnO2 2-、SiO3 2-、AlO2 -、Ca(OH)2Form is dissolved in leachate, and lead, iron, copper are then with oxide shape
Formula is precipitated, and leaching process is stirred continuously, and is filtered, filtrate A and leaded enrichment slag；
Lead oxide enrichment slag is rinsed with sig water, washing lotion is incorporated to leachate；Filtrate A by adjusting pH precipitated impurities elements,
Filtering, obtains liquor B and reclaims filter residue, and for liquor B by adding sodium hydroxide and then sodium sulphate being recovered by filtration, filtrate is remaining hydrogen-oxygen
Change sodium solution A to recycle；
Leaching condition is：Reaction product is controlled 1 with water by solid-to-liquid ratio:50~1:200 (g/mL), extraction temperature 20~50
DEG C, 1~4h of extraction time.Particularly, can be 9~12 by controlling leaching process leachate pH in leaching process.
It is as follows to leach dedoping step reaction equation：
NaxPbOy+H2O→Pb(OH)2+NaOH
Pb(OH)2→PbO+H2O
ZnO+NaOH→Na2ZnO2(aq)+H2O
Al2O3+NaOH→NaAlO2(aq)+H2O
CaO+H2O→Ca(OH)2(aq)
SiO2+NaOH→Na2SiO3(aq)+H2O
Step 3：Alkali extracts lead
The main component contained in leaded enrichment slag in step 2 is PbO, Fe2O3And CuO, using heat alkali liquid as leaching
Go out liquid and leach alternative lead, leaching process is stirred continuously, filtered while hot, is rinsed and precipitated with heat alkali liquid, and washing lotion is incorporated to heat alkali liquid
Leachate, filtering, obtaining leaded filtrate, filter residue comes back for leaching again simultaneously；
Leaching condition：Alkali lye is sodium hydroxide solution, and naoh concentration control is 5~30%, extraction temperature 50~110
DEG C, 1~10h of extraction time.
Thermokalite leaching process reaction equation is as follows：
PbO+NaOH+H2O→Na2Pb(OH)4
Step 4：Precipitation prepares lead oxide
Heated alkaline leaded filtrate in step 3 is quickly cooled to 5~20 DEG C, solubility of the lead in alkaline solution is rapid
Reduce, separated out in the form of lead hydroxide, said mixture is separated by filtration after the completion of to be precipitated, lead hydroxide filter residue is 150~300
DEG C calcining and decomposing obtains lead oxide product, and the Strong oxdiative sodium liquor B containing a small amount of lead is back to the leachate in step 3.
Remaining sodium hydroxide solution A also can be as the leachate in step 3.
The present invention have it is following a little：
1st, because invention employs self-propagating reaction technology, the vulcanized lead in concentrate of lead sulfide ore is made to occur certainly with sodium peroxide
Sprawling reaction, without providing additional-energy, reaction speed is exceedingly fast, overcome high temperature, high pressure that existing pyrogenic process wet processing brings,
The problems such as high energy consumptions such as peracid, high cost, complex procedures.And high temperature caused by self-propagating reaction can realize heat recovery,
Realize concentrate of lead sulfide ore low energy consumption, Quick Pretreatment.Self-propagating reaction reaction product is stable, and element sulphur is converted into sulfuric acid
Salt, the generation of the sulfur-bearing toxic gas such as sulfur dioxide is avoided, realizes cleanliness without any pollution.
3rd, for the present invention using water to leach cleaner, cost is extremely low, and dust removal rate is high, and equipment requirement is low, green non-pollution.
Lead oxide enriched product can be obtained after separation, impurity removal, using thermokalite Selectively leaching lead, leachate impurity content is few, realizes
Efficiently leach the lead resource in concentrate of lead sulfide ore.
4th, technique of the invention can be directed to all kinds concentrate of lead sulfide ore, and lead tolerance in concentrate of lead sulfide ore is required compared with
Low, concentrate of lead sulfide ore of the sulfide content higher than 50% can be applied to this technique, have wide range of applications.The present invention has work
Skill is simple and easy, and raw materials used and equipment is all relatively common and cheap, and energy consumption is extremely low, green non-pollution.
Brief description of the drawings
Fig. 1 represents a kind of flow chart of the method based on self-propagating reaction processing concentrate of lead sulfide ore.
Embodiment
Embodiment 1
Fine grinding, 74 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:3 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are drawn using microwave heating method
Send out self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carries out leaching removal of impurities by leaching agent of water, instead
Product is answered to be controlled with water by solid-to-liquid ratio 1:50 (g/mL), leachate pH are 10.5.50 DEG C of extraction temperature, extraction time 1h.Cross
Filter, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter residue is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A,
Liquor B reclaims sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 25%, 85 DEG C of extraction temperature, extraction time 5h, leaching process is stirred continuously, hot mistake
Filter, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.Leaded heated alkaline leaching liquid is fast
Speed is cooled to 10 DEG C, and lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide filter residue are separated by filtration after the completion of to be precipitated
Lead oxide product is obtained in 300 DEG C of calcining and decomposings, the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 2
Fine grinding, 38 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:4 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are lighted a fire and triggered using thermal explosion
Self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, leaching removal of impurities is carried out by leaching agent of water, is reacted
Product is controlled 1 with water by solid-to-liquid ratio:100 (g/mL), leachate pH are 10.7.45 DEG C of extraction temperature, extraction time 1.5h.Cross
Filter, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter residue is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A,
Liquor B reclaims sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 10%, 105 DEG C of extraction temperature, extraction time 4h, leaching process is stirred continuously, heat
Filtering, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.By leaded heated alkaline leaching liquid
15 DEG C are quickly cooled to, lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide filter are separated by filtration after the completion of to be precipitated
Slag obtains lead oxide product in 275 DEG C of calcining and decomposings, and the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 3
Fine grinding, 180 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:5 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, using drip type chemical point
Fire triggers self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carrying out leaching as leaching agent using water removes
Miscellaneous, reaction product is controlled 1 with water by solid-to-liquid ratio:150 (g/mL), leachate pH are 9.40 DEG C of extraction temperature, extraction time 2h.
Filtering, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A
Slag, liquor B reclaim sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag is using warm
Sodium hydroxide solution leaches lead, and naoh concentration 5%, 110 DEG C of extraction temperature, extraction time 3h, leaching process is stirred continuously,
Heat filtering, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.By leaded heated alkaline leaching
Liquid is quickly cooled to 12 DEG C, and lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide are separated by filtration after the completion of to be precipitated
Filter residue obtains lead oxide product in 225 DEG C of calcining and decomposings, and the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 4
Fine grinding, 53 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:2 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are triggered using electric heat ignition
Self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, leaching removal of impurities is carried out by leaching agent of water, is reacted
Product is controlled 1 with water by solid-to-liquid ratio:200 (g/mL), leachate pH are 11.3.35 DEG C of extraction temperature, extraction time 2.5h.Cross
Filter, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter residue is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A,
Liquor B reclaims sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 10%, 100 DEG C of extraction temperature, extraction time 2h, leaching process is stirred continuously, heat
Filtering, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.By leaded heated alkaline leaching liquid
6 DEG C are quickly cooled to, lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide filter are separated by filtration after the completion of to be precipitated
Slag obtains lead oxide product in 175 DEG C of calcining and decomposings, and the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 5
Fine grinding, 62 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:1 is thoroughly mixed uniformly, compacting, is placed in high temperature resistant reaction vessel, is drawn using combustion wave igniting
Send out self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carries out leaching removal of impurities by leaching agent of water, instead
Product is answered to be controlled with water by solid-to-liquid ratio 1:75 (g/mL), leachate pH are 9.5.30 DEG C of extraction temperature, extraction time 3h.Cross
Filter, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter residue is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A,
Liquor B reclaims sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 15%, 95 DEG C of extraction temperature, extraction time 1h, leaching process is stirred continuously, hot mistake
Filter, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.Leaded heated alkaline leaching liquid is fast
Speed is cooled to 15 DEG C, and lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide filter residue are separated by filtration after the completion of to be precipitated
Lead oxide product is obtained in 300 DEG C of calcining and decomposings, the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 6
Fine grinding, 86 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:3.5 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are drawn using laser ignition
Send out self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carries out leaching removal of impurities by leaching agent of water, instead
Product is answered to be controlled with water by solid-to-liquid ratio 1:125 (g/mL), leachate pH are 10.25 DEG C of extraction temperature, extraction time 3.5h.Cross
Filter, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter residue is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A,
Liquor B reclaims sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 20%, 90 DEG C of extraction temperature, extraction time 6h, leaching process is stirred continuously, hot mistake
Filter, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.Leaded heated alkaline leaching liquid is fast
Speed is cooled to 18 DEG C, and lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide filter residue are separated by filtration after the completion of to be precipitated
Lead oxide product is obtained in 150 DEG C of calcining and decomposings, the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 7
Fine grinding, 200 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:4.5 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are drawn using thermal explosion igniting
Send out self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carries out leaching removal of impurities by leaching agent of water, instead
Product is answered to be controlled with water by solid-to-liquid ratio 1:175 (g/mL), leachate pH are 10.5.20 DEG C of extraction temperature, extraction time 4h.Cross
Filter, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter residue is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A,
Liquor B reclaims sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 23%, 80 DEG C of extraction temperature, extraction time 7h, leaching process is stirred continuously, hot mistake
Filter, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.Leaded heated alkaline leaching liquid is fast
Speed is cooled to 8 DEG C, and lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide filter residue are separated by filtration after the completion of to be precipitated
Lead oxide product is obtained in 200 DEG C of calcining and decomposings, the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 8
Fine grinding, 109 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:2.5 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are drawn using laser ignition
Send out self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carries out leaching removal of impurities by leaching agent of water, instead
Product is answered to be controlled with water by solid-to-liquid ratio 1:80 (g/mL), leachate pH are 11.Leach 40 DEG C of temperature, extraction time 2h.Filtering, with
Sig water rinses filter residue, and washing lotion is incorporated to leachate.Filter residue, liquor B is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A
Sodium sulphate is reclaimed by adding sodium hydroxide, remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot sodium hydroxide
Solution leaches lead, and naoh concentration 25%, 70 DEG C of extraction temperature, extraction time 8h, leaching process is stirred continuously, heat filtering,
Rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.By the leaded heated alkaline fast quickly cooling of leaching liquid
But to 5 DEG C, lead is separated out in the form of lead hydroxide, said mixture is separated by filtration after the completion of to be precipitated, lead hydroxide filter residue is 250
DEG C calcining and decomposing obtains lead oxide product, and the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 9
Fine grinding, 120 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:1.5 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are drawn using chemic ignition
Send out self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carries out leaching removal of impurities by leaching agent of water, instead
Product is answered to be controlled with water by solid-to-liquid ratio 1:130 (g/mL), leachate pH are 11.5.45 DEG C of extraction temperature, extraction time 2.5h.
Filtering, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A
Slag, liquor B reclaim sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag is using warm
Sodium hydroxide solution leaches lead, and naoh concentration 28%, 60 DEG C of extraction temperature, extraction time 9h, leaching process is stirred continuously,
Heat filtering, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.By leaded heated alkaline leaching
Liquid is quickly cooled to 15 DEG C, and lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide are separated by filtration after the completion of to be precipitated
Filter residue obtains lead oxide product in 280 DEG C of calcining and decomposings, and the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Embodiment 10
Fine grinding, 150 microns of powder particle size are crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried.By miberal powder and peroxide
Change sodium powder in mass ratio 1:3 are thoroughly mixed uniformly, compacting, are placed in high temperature resistant reaction vessel, are drawn using microwave heating method
Send out self-propagating reaction.It is placed in after reaction after product cooling in alkali resistance reaction vessel, carries out leaching removal of impurities by leaching agent of water, instead
Product is answered to be controlled with water by solid-to-liquid ratio 1:160 (g/mL), leachate pH are 12.50 DEG C of extraction temperature, extraction time 3h.Cross
Filter, filter residue is rinsed with sig water, washing lotion is incorporated to leachate.Filter residue is recovered by filtration by adjusting pH precipitated impurities elements in filtrate A,
Liquor B reclaims sodium sulphate by adding sodium hydroxide, and remaining sodium hydroxide solution recycles.Leaded enrichment slag uses hot hydrogen-oxygen
Change sodium solution and leach lead, naoh concentration 30%, 50 DEG C of extraction temperature, extraction time 10h, leaching process is stirred continuously, heat
Filtering, rinsed and precipitated with heat alkali liquid, washing lotion is incorporated to leachate, and filter residue comes back for secondary leaching.By leaded heated alkaline leaching liquid
10 DEG C are quickly cooled to, lead is separated out in the form of lead hydroxide, and said mixture, lead hydroxide filter are separated by filtration after the completion of to be precipitated
Slag obtains lead oxide product in 300 DEG C of calcining and decomposings, and the alkali lye containing a small amount of lead is back to thermokalite and leaches process.
Claims (8)
- A kind of 1. method based on self-propagating reaction processing concentrate of lead sulfide ore, it is characterised in that comprise the following steps：Step 1：Self-propagating reactionFine grinding is crushed after concentrate of lead sulfide ore powder after ore dressing is fully dried, is then sufficiently stirred miberal powder with peroxidating sodium powder mixed Close uniformly, compacting, be placed in high temperature resistant reaction vessel；Using chemic ignition, combustion wave igniting, laser ignition, thermal explosion igniting or Microwave light a fire the methods of in one or more ignite method trigger self-propagating reaction；React once igniting with the waveshape that burns Spontaneous progress, without providing additional-energy, until reaction terminates；Step 2：Water logging cleansIt is placed in after being reacted in step 1 after product cooling in alkali resistance reaction vessel, leaching removal of impurities is carried out by leachate of water, Foreign ion is with ZnO2 2-、SiO3 2-、AlO2 -、Ca(OH)2Form is dissolved in solution, and lead, iron, copper then sink in the form of an oxide Form sediment, leaching process is stirred continuously, and is filtered, filtrate A and leaded enrichment slag；Lead oxide enrichment slag is rinsed with sig water, washing lotion is incorporated to leachate；Filtrate A is by adjusting pH precipitated impurities elements, filtering, Obtain liquor B and reclaim filter residue, for liquor B by adding sodium hydroxide and then sodium sulphate being recovered by filtration, filtrate is remaining sodium hydroxide A Solution recycles；Step 3：Alkali extracts leadThe main component contained in leaded enrichment slag in step 2 is PbO, Fe2O3And CuO, using heat alkali liquid as leachate Alternative lead is leached, leaching process is stirred continuously, and is filtered while hot, is rinsed and is precipitated with heat alkali liquid, and washing lotion is incorporated to heat alkali liquid leaching Liquid, filtering, obtaining leaded filtrate, filter residue comes back for leaching again simultaneously；Step 4：Precipitation prepares lead oxideHeated alkaline leaded filtrate in step 3 is quickly cooled to 5~20 DEG C, solubility of the lead in alkaline solution reduces rapidly, Separated out in the form of lead hydroxide, said mixture is separated by filtration after the completion of to be precipitated, lead hydroxide filter residue is forged at 150~300 DEG C Burn to decompose and obtain lead oxide product, the sodium hydroxide liquor B containing a small amount of lead is back to the leachate in step 3.
- 2. according to a kind of method that concentrate of lead sulfide ore is handled based on self-propagating reaction of claim 1, it is characterised in that step 1 30~200 microns of powder particle size.
- 3. according to a kind of method that concentrate of lead sulfide ore is handled based on self-propagating reaction of claim 2, it is characterised in that miberal powder grain 74 microns of degree.
- 4. according to a kind of method that concentrate of lead sulfide ore is handled based on self-propagating reaction of claim 1, it is characterised in that step 1 Concentrate of lead sulfide ore powder is 1 with sodium peroxide mass ratio:1~1:5.
- 5. according to a kind of method that concentrate of lead sulfide ore is handled based on self-propagating reaction of claim 1, it is characterised in that step Two, leaching condition is：Reaction product is controlled 1 with water by solid-to-liquid ratio:50~1:200g/mL, 20~50 DEG C of extraction temperature, leach 1~4h of time.
- 6. according to a kind of method that concentrate of lead sulfide ore is handled based on self-propagating reaction of claim 1, it is characterised in that step 2 By controlling leaching process leachate pH as 9~12 in leaching process.
- 7. according to a kind of method that concentrate of lead sulfide ore is handled based on self-propagating reaction of claim 1, it is characterised in that step 3 Leaching condition：Alkali lye is sodium hydroxide solution, and naoh concentration control 50~110 DEG C of extraction temperature, is leached 5~30% 1~10h of time.
- 8. according to a kind of method that concentrate of lead sulfide ore is handled based on self-propagating reaction of claim 1, it is characterised in that residual hydrogen Sodium oxide molybdena solution A is as the leachate in step 3.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85103877A (en) * | 1985-05-09 | 1986-02-10 | 云南工学院 | Lead-smelting method without pollution problem |
| CN1030444A (en) * | 1987-04-07 | 1989-01-18 | 全苏有色金属矿冶研究所 | Handle the method for lead sulfide or lead sulfide-zinc ore and/or concentrate |
| CN1045995A (en) * | 1989-03-30 | 1990-10-10 | 朱松伯 | Method with the direct extracting metals lead of sulfuration lead ore |
| CN1124297A (en) * | 1994-12-08 | 1996-06-12 | 景治熙 | Technique for producing metal by directly smelting sulphide ore |
| CN1353202A (en) * | 2000-11-10 | 2002-06-12 | 柳州市环东金属材料厂 | Process for treating metal sulfide ore |
| CN101240379A (en) * | 2007-02-08 | 2008-08-13 | 赖成章 | Method for directly smelting lead zinc sulfide ore by hydrogen |
| CN104313328A (en) * | 2014-10-11 | 2015-01-28 | 中南大学 | Method for smelting and recovering lead and gold from reduction and sulfur fixation molten pool based on refractory gold ores and lead-containing residue raw materials |
| CN104451161A (en) * | 2014-12-04 | 2015-03-25 | 中南大学 | Method for low-temperature smelting of regenerated lead |
-
2016
- 2016-04-01 CN CN201610204722.8A patent/CN105838902B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85103877A (en) * | 1985-05-09 | 1986-02-10 | 云南工学院 | Lead-smelting method without pollution problem |
| CN1030444A (en) * | 1987-04-07 | 1989-01-18 | 全苏有色金属矿冶研究所 | Handle the method for lead sulfide or lead sulfide-zinc ore and/or concentrate |
| CN1045995A (en) * | 1989-03-30 | 1990-10-10 | 朱松伯 | Method with the direct extracting metals lead of sulfuration lead ore |
| CN1124297A (en) * | 1994-12-08 | 1996-06-12 | 景治熙 | Technique for producing metal by directly smelting sulphide ore |
| CN1353202A (en) * | 2000-11-10 | 2002-06-12 | 柳州市环东金属材料厂 | Process for treating metal sulfide ore |
| CN101240379A (en) * | 2007-02-08 | 2008-08-13 | 赖成章 | Method for directly smelting lead zinc sulfide ore by hydrogen |
| CN104313328A (en) * | 2014-10-11 | 2015-01-28 | 中南大学 | Method for smelting and recovering lead and gold from reduction and sulfur fixation molten pool based on refractory gold ores and lead-containing residue raw materials |
| CN104451161A (en) * | 2014-12-04 | 2015-03-25 | 中南大学 | Method for low-temperature smelting of regenerated lead |
Non-Patent Citations (1)
| Title |
|---|
| 过氧化钠超强熔矿能力的新认识;郑大中等;《四川地质学报》;2010123;第488-491页 * |
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