CN110195162A - Antimony in a kind of arsenic alkaline slag, arsenic, the separation of alkali leaching simultaneously method - Google Patents
Antimony in a kind of arsenic alkaline slag, arsenic, the separation of alkali leaching simultaneously method Download PDFInfo
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- CN110195162A CN110195162A CN201910603764.2A CN201910603764A CN110195162A CN 110195162 A CN110195162 A CN 110195162A CN 201910603764 A CN201910603764 A CN 201910603764A CN 110195162 A CN110195162 A CN 110195162A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/07—Preparation from the hydroxides
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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
- C22B1/11—Removing sulfur, phosphorus or arsenic other than by roasting
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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
- C22B13/045—Recovery from waste materials
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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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
- 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
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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Abstract
Antimony in a kind of arsenic alkaline slag, arsenic, the separation of alkali leaching simultaneously method, the following steps are included: being soaked adding water, glycerol and caustic soda by the arsenic alkaline slag of crushing and grinding or being sent into the slurry after arsenic alkaline slag and water, glycerol and caustic soda together grinding in molten tank, control pH value, it carries out soaking molten extraction, it is separated by solid-liquid separation, obtains siulica-alumina mineral slag and alkali glycerine water solution；After gained alkali glycerine water solution successively carries out dearsenification, de- lead, de- antimony and purification precipitation process, arsenic acid salt crystal, lead skim, antimony oxide, phytate precipitates and glycerol soda ash aqueous solution are obtained；Gained glycerol soda ash aqueous solution row nanofiltration or reverse osmosis membrane analyse to obtain nanofiltration concentrate and dialyzate glycerine water solution；Gained dialyzate glycerine water solution, which returns, soaks molten arsenic alkaline slag；The spray drying of gained nanofiltration concentrate is made soda ash or lime causticization is added to produce caustic soda；Gained antimony oxide is for returning to antimony refining or processing antimony or purification antimony oxide and stibate.Antimony, arsenic, alkali in arsenic alkaline slag of the present invention can leaching simultaneously separation, and solvent is can be recycled.
Description
Technical field
The present invention relates to antimony, arsenic, alkali in environmental protection and waste utilization technical field of resource comprehensive utilization more particularly to a kind of arsenic alkaline slag are same
Step leaches isolated resource utilization method.
Background technique
Arsenic alkaline slag is generated a kind of containing natrium arsenicum, sodium antimonate, sodium carbonate in the antimony refining arsenic removal process of antimony pyrometallurgical smelting
Based on and contain the melting waste slags of the compounds such as a certain amount of aluminosilicate mineral and lead, bismuth, because of natrium arsenicum sodium arsenite severe toxicity
And it is soluble easily in water, easily lead to Environment Pollution Event, is difficult to the solid hazardous waste dealt carefully with all the time, to a certain degree
On constrain the sound development of antimony smelting industry.
For being difficult to the arsenic alkaline slag dealt carefully with, domestic and international scientific worker has been continued for a large amount of research and reality
It tramples, the various technical methods of existing arsenic alkaline slag processing substantially can be summarized as solidification landfill, wet-treating and pyrogenic attack three categories
Method.
The solidification burying method of arsenic alkaline slag include using cement solidification, lime/calcium salt solidification, molysite solidification, plastics solidification,
Then bitumen solidification, melting/vitrification solidifying etc. fill, although solidification landfill can to a certain extent, it is real in certain time
The fixation of existing arsenic, but these solidification burying methods all need a large amount of landfills than the big, later period in the presence of solidification front and back increase-volume and deposit
The long-term pollution hidden danger the problems such as.
The wet treatment method of arsenic alkaline slag mainly can be dissolved in water using alkali, natrium arsenicum and the sodium arsenite in arsenic alkaline slag,
And antimonious acid sodium and sodium antimonate indissoluble or property not soluble in water realize the separation of arsenic antimony, dissolve out arsenic, then use chemical precipitation
Method such as arsenic acid calcium precipitate, precipitated ferric arsenate, arsenones precipitating etc. or the method for direct crystallization natrium arsenicum and soda ash salt-mixture are into one
Step processing leachate.Existing wet treatment method can be summarized as follows:
1) water logging-natrium arsenicum mixed salt method: being crushed arsenic alkaline slag material with hot water leaching, be separated into leached mud containing antimony and solution, leaching
Slagging tap send blast furnace to handle after drying, solution after evaporating completely is dry for natrium arsenicum salt-mixture (containing natrium arsenicum, sodium carbonate,
Sodium sulphate and a small amount of antimony), mainly as glass fining agent.
2) water logging-calcium slag method: arsenic alkaline slag wet type being crushed, then, is leached with hot water stirs, exhausted most arsenic therein
Sour sodium and sodium carbonate enter solution, are separated into leached mud containing antimony and leachate, send blast furnace to handle after leached mud drying, leachate
Add calcium hydroxide causticization, then is separated into calcium slag (calcium arsenate calcium carbonate) and soda bath.Though the rate of deposition of arsenic reachable 98%, calcium
Arsenic still reaches to 13~126mg/L in aqueous solution in slag, and solubility is bigger under acidic environment, and being still to be processed must have
Malicious danger solid waste.And liquid alkaline or piece alkali is made in soda bath after being concentrated by evaporation, and containing arsenic up to 3% or so, returns and is used as needle antimony essence
It is very unsatisfactory to refine Hydrodearsenic Catalyst effect, causes circulation of the arsenic in smelting system.
3) water logging-CO is aoxidized2Separation arsenic alkaline process: being crushed using hot water Oxidation Leaching or the arsenic alkaline slag of wet-milling, is separated into
Leachate (solution of containing sodium carbonate, natrium arsenicum, sodium sulphate, schlippe's salt etc.) and leached mud (contain sodium antimonate, antimonious acid sodium
With the solids of the gangue minerals such as metallic antimony and other silica).Then, the sodium carbonate in leachate is turned with carbon dioxide
The lower sodium bicarbonate of solubility is turned to, after the sodium bicarbonate (containing arsenic) for isolating crystallization, then Hydrodearsenic Catalyst is added in the solution and sinks
Form sediment natrium arsenicum out (containing alkali).Sodium bicarbonate heat treatment is converted into sodium carbonate (containing arsenic) and is back to antimony refining arsenic removal.
4) the heavy arsenic method of oxidation water logging-neutralization-vulcanization: with molten broken or wet-milling the arsenic alkaline slag of hot water oxidation leaching, it is separated into leaching
It slags tap (containing stibate etc.), leachate, leached mud is dry to return to blast furnace processing；Then, (containing natrium arsenicum, sodium arsenite, carbon
Sour sodium, sodium sulphate etc.) it a large amount of acid (generally with sulfuric acid or hydrochloric acid) is added in leachate neutralizes alkali therein, solution is adjusted to acid
Property, then plus H2S, Na2S sulfides by the arsenic in solution be converted into arsenones precipitating (As2S3).This method not only needs to consume
A large amount of acid goes to neutralize the alkali in leachate, and waste water still contains a certain amount of arsenic and a large amount of inorganic salts.
5) aoxidize water logging-ammonium arsenate metal salts as precipitator: after the oxidation water logging of broken or wet-milling arsenic alkaline slag, be separated by solid-liquid separation for containing
Leachate based on sodium carbonate and natrium arsenicum and containing the leached mud based on stibate；Then, metal ammonium complexing is added in leachate
Solion and crystal growth promoters are reacted, are aged, are crystallized, are precipitated, then solid-liquid separation ammonium arsenate metal salt；Again will
Solution heats de- ammonium, then, then is passed through carbon dioxide reaction and sodium bicarbonate crystal is precipitated, the sodium bicarbonate isolated is through thermally decomposing
For sodium carbonate (containing arsenic) reuse.Such removed with the wet-precipitated dearsenification method of metal-ammonia complex ion solution increase new metal from
Sub outer, dearsenification still has certain limitation, best (effect is optimal in molybdenum acid ammonia purification) the arsenic acid ammonia of even current effect
Magnesium processes, 0.038 gram of solubility in 20 DEG C of water of 6 water outlet arsenic acid ammonia magnesium of indissoluble, the solubility in 80 DEG C of water is 0.024 gram.
And the zinc ammonia precipitation effect in technology is inferior to ammonia magnesium precipitate effect at present.
Existing wet processing process requires to be dissolved in arsenic alkaline slag in a large amount of water, and precipitation method separation can generate body
The huge arsenious waste solution of product, direct emission can bring huge pollution to environment, advanced treating needed to can be only achieved discharge standard, locate
Manage at high cost, energy consumption height.Wherein the method for direct crystallization natrium arsenicum and soda ash is also to need to evaporate the liquid containing arsenic of large volume, and steam
Micro- foam containing arsenic that hair process is difficult to avoid that splashes, severe operational environment；In addition the natrium arsenicum product impurity content of output is higher, and
The limited backlog of the products market demand such as common natrium arsenicum, arsenones is big, and wet processing operation is unsatisfactory on the whole.
The basic technology of the pyrogenic attack of arsenic alkaline slag is " arsenic alkaline slag blast furnace volatile smelting+reduction smelting in reverberatory furnace refining "
Arsenic alkaline slag investment stibium blast furnace is carried out volatile smelting, while being incorporated enough flux and coke by method, arsenic in arsenic alkaline slag,
Antimony is oxidized together enters flue gas cooling device, thick three oxidation two of the high arsenic of cooling recycling with high-temperature flue gas in the form of the oxide
Antimony reenters addition reducing agent in reverberatory furnace and is reduced to needle antimony, and soda ash then is added in reverberatory furnace again or piece alkali air blast is repeatedly smart
Refining obtains qualified antimony slab.The advantage of pyrogenic attack arsenic alkaline slag is that processing capacity is big, high production efficiency, can use antimony smelting
The equipment of system.But because raw material/return product are high containing arsenic, first operating environment is poor, and personal safety risk is big, and second high arsenic needle antimony is anti-
The return product that multiple refining generates are higher containing arsenic, form the vicious circle of arsenic, moreover require to have perfect, closed cooling to gather dust and be
System.
CN102965517A discloses a kind of processing method of arsenic alkaline slag glass solidification, in the molten state by arsenic alkaline slag first
Sodium antimonate is selectively reduced to metallic antimony for reduction with carbon agent and arsenic is present in slag with arsenic acid na form；Then in slag containing arsenic
Middle addition glass melting dosage form is at low temperature glass phase, and water quenching is at cullet block or the founding directly in ingot mould after glass phase is released
At glass ingot, convenient for storing up and returning pit landfill.
CN104073644B discloses refining lead slag-removed by antimony fire refining process reduction smelting method synchronous with arsenic alkaline slag proportion, including with
Lower step: (1) it is lead slag-removed with arsenic alkaline slag by weight, according to sodium ion in the content and arsenic alkaline slag of lead slag-removed middle phosphate anion
Content, determine lead slag-removed with arsenic alkaline slag proportion, wherein the quality of sodium ion and lead slag-removed middle phosphate anion in arsenic alkaline slag
Than for 60~80:90~120；(2) the lead slag-removed and arsenic alkaline slag matched by step (1) is uniformly mixed, anthracite is added, it is added
Anthracite is lead slag-removed 3~15% with arsenic alkaline slag total weight, in 800~1000 DEG C of constant temperature processing 30~after sixty minutes, is cooled to
Room temperature separates antimony arsenical lead and tertiary sodium phosphate dross,.
CN108220626A discloses a kind of arsenic alkaline slag reduction melting processing method, this method by arsenic alkaline slag and carbonaceous also
Reduction melting obtains arsenic steam, needle antimony and reducing slag after former agent mixing, obtains metallic arsenic product after the condensation of arsenic steam；Reducing slag
Main component is Na2CO3, can return to antimony directly as Hydrodearsenic Catalyst and refine dearsenification process, can also pass through water logging-concentration-
Crystallization processes obtain Na2CO3 crystal.
CN106636678A discloses a kind of method that arsenic-containing material direct-reduction roasting prepares arsenic, and this method is with arsenate
For raw material, arsenate material and carbonaceous reducing agent after mixing, are placed in inertia or reducing atmosphere, under condition of negative pressure, into
Row reduction roasting collects baking flue gas to get arsenic product.
Above-mentioned pyrogenic processing method, the condition for heat-treating processing is harsh, vacuum arc furnace ignition between needing to seal, using vacuum pumping
Vacuum vacuumizes 1~8 hour in hot conditions are mandatory, the control of this intermittence fire reduction processing require it is very stringent, it is right
Equipment requirement and operation control require height, may only be adapted to laboratory or small batch Metallurgical processing, and large batch of industry is raw
The adaptability of production leaves a question open；Also it is less adapted to handle the arsenic alkaline slag containing a large amount of antimony, vacuum pump is used to continue at >=800 DEG C strong take out
Under the situation of vacuum, the volatilization of antimony steam will occur simultaneously with the distillation (615 DEG C of arsenic distillations) of arsenic, and what is frequently resulted in only can be arsenic
Antimony alloy；And be difficult to largely handle the arsenate containing stibate, using carbon as reducing agent smelting arsenic alkali slag, reduction temperature is lower than 800
DEG C when whole reducing power it is still extremely weak, 900 DEG C or more just have preferable reproducibility, and are directed to hazardous waste disposal temperature
Degree is higher, more than energy consumption height, the higher problem of equipment Requirement, and potential accident risk is bigger, and due to using closing
Reduction furnace, which is stood in its gained needle antimony lead of carbon reducing agent evacuation process, still contains arsenic, still contains not a small amount of arsenic in reducing slag
(including Soluble Arsenic hydrochlorate and insoluble arsenate) has still only achieved the purpose that partial reduction separates, either needle antimony
Return refining, or reducing slag return the circulation of arsenic is all caused as Hydrodearsenic Catalyst.Both just under strict control reaction condition
Still contain a certain amount of arsenic in the water logging slag that its reducing slag separates after water logging, be still that dangerous solid waste needs to locate
Reason；Arsenic steam or arsenic flue gas or elemental arsenic in treatment process are easily oxidized, and force to take out with vacuum pump especially out of high temperature furnace
Out to during cooling, even with the mixed atmosphere of inert gas and/or nitrogen and hydrogen and/or carbon monoxide etc.,
Extremely difficult recycling, easily leads to that economy is bad or pollution atmosphere, and is sucked by vacuum the vacuum pump pair that is relied on of arsenic flue gas
The adaptability of metal particle or exhaust gas dust is very poor, it is difficult to guarantee normal production run；Or need through strict control sodium and
The equivalent proportion of phosphate radical generates the reaction condition of tertiary sodium phosphate, by arsenic alkaline slag stibate and arsenate etc. be reduced into list simultaneously
Matter antimony and elemental arsenic, and the production of actual antimony smelting enterprise control habit is difficult to ensure that it seems simple reaction condition, and
It handles energy consumption height, and potential pollution hidden danger is big, and especially the tertiary sodium phosphate dross containing arsenic easily quietly flows into agricultural fertilizer market and leads
It causes to pollute uncontrollable diffusion.
In conclusion arsenic, antimony, the separation of alkali are more difficult in the treatment process of existing all kinds of arsenic alkaline slags, environmental protection and warp
The problems such as Ji property, is prominent.The wet processing that the country currently focuses on all concentrates on hot water and soaks molten or oxidation water logging, and with glycerol liquor
The research or practice that solution soaks molten separation arsenic alkaline slag are there is not yet any report.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide a kind of can be achieved
Antimony, arsenic in arsenic alkaline slag, the separation of alkali leaching simultaneously, and antimony, arsenic, the separation of alkali leaching simultaneously in solvent arsenic alkaline slag can be recycled
Method.
The technical solution adopted by the present invention to solve the technical problems is as follows: antimony, arsenic, alkali leaching simultaneously in a kind of arsenic alkaline slag
Isolated method, comprising the following steps: by by the arsenic alkaline slag of crushing and grinding add water, glycerol and caustic soda or by arsenic alkaline slag and water,
The slurry of glycerol and caustic soda together after grinding, which is sent into, to be soaked in molten tank, is controlled pH value, is carried out soaking molten extraction, is separated by solid-liquid separation, obtains sial
Mineral slag and alkali glycerine water solution；The alkali glycerine water solution is that the mixing of complex compound containing glycerol, caustic soda, arsenate and soda ash is molten
Liquid, gained alkali glycerine water solution successively carry out dearsenification, de- lead, de- antimony and purification precipitating divalent ion and heavy mental treatment
Afterwards, arsenic acid salt crystal, lead skim, antimony oxide, phytate precipitates and glycerol soda ash aqueous solution are obtained；Gained glycerol soda ash aqueous solution
It carries out nanofiltration and/or reverse osmosis membrane analyses to obtain concentrate and dialyzate glycerine water solution；Gained dialyzate glycerine water solution returns to leaching
Molten arsenic alkaline slag；The spray drying of gained concentrate is made soda ash or calcining magnesia or lime causticization is added to produce caustic soda；Gained oxidation
Antimony is for returning to antimony refining or processing antimony or purification antimony oxide and metaantimmonic acid product salt.
Further, the arsenic alkaline slag: water: glycerol: caustic soda is 1:1~8:0.5~5:0.3~3 in mass ratio.
Further, control pH=14.It consumes caustic soda when soaking molten reaction, when caustic soda surplus is insufficient, pH value is lower than 14
When, 10~30% caustic soda amount is added, in time to maintain the stability of leaching molten ability and glycerol antimony complex to antimonial.
Further, the molten extraction of the leaching soaks molten 0.5h~8h for 60 DEG C~150 DEG C stirrings；The molten extraction of leaching uses single-stage
Soak it is molten or it is multistage leaching it is molten or leaching trough counter-current leaching it is molten.Sufficiently to extract the antimony in arsenic alkaline slag, arsenic and soda ash, or keep alkali glycerol water-soluble
Antimony complex, arsenate, soda ash in liquid reach saturation under the leaching solubility temperature of setting.
Further, the mesh number of the sieving of the arsenic alkaline slag by crushing and grinding be 160 mesh~800 mesh (preferably 200~
400 mesh).
Further, partial size < 100 μm of the slurry.
Further, the dearsenification is by alkali glycerine water solution crystallisation by cooling, separation, and the alkali for obtaining arsenic acid salt crystal and dearsenification is sweet
Oil solution；The alkali glycerine water solution of the dearsenification is the mixed solution of antimonial lead bismuth glycerol complex compound, caustic soda and soda ash.
Further, the de- lead is that the alkali glycerine water solution of dearsenification is added dropwise to sodium sulfide solution reaction to generate vulcanized lead, sulphur
Change bismuth precipitating, separates sulfide precipitation, obtain the alkali glycerine water solution of the lead skim and de- lead based on lead-containing compounds；The de- lead
Alkali glycerine water solution is the mixed solution of antimony complex containing glycerol, caustic soda and soda ash.
Further, the purification precipitating divalent ion and heavy mental treatment are 10 DEG C~90 DEG C glycerol liquors in de- antimony
Be added dropwise phytic acid in solution, react whole divalent ions and heavy metal ion in precipitation solution, separation, obtain phytate precipitates,
Glycerol soda ash aqueous solution.
Further, the de- antimony is that carbon dioxide is passed through in the alkali glycerine water solution of de- lead at 5 DEG C~95 DEG C, neutralizes fire
Alkali, reaction are reduced to 11.5~11.7 to pH value, and the glycerol antimony complex parsing for reacting generation is settled out oxidation antimony powder, separate,
Obtain the glycerine water solution of antimony oxide, de- antimony；
Further, the de- antimony is in the alkali glycerine water solution of de- lead plus hydrochloric acid is neutralized to pH value 6~7.8, separates, obtains antimony oxygen
The glycerine water solution of compound and de- antimony.
Further, mannitol or xylose alcohol part substitution or replacing whole can be used in the glycerol；The caustic soda can
It is substituted using potassium hydroxide.
Further, resulting siulica-alumina mineral slag, through detecting: predominantly aluminosilicate mineral, antimony content < 1.0%, arsenic content <
0.1%, lead content < 1.0%, the experiment of soda content < 2.0%, TCLP detect arsenic content < 5mg/L in solution, are general solid waste, can use
As production of construction materials raw material.
Further, alkali glycerine water solution soaks the product arsenate separated after molten arsenic alkaline slag leaching simultaneously, lead bismuth sulphide, antimony
Oxide, soda ash or salt can directly be taken out, or as produce antimony product, arsenic product, purification alkali or salt raw material, sb oxide and
Soda ash or caustic soda also may be used.
The invention has the advantages that:
(1) dissolved in using antimony (leaded bismuth) oxide and sodium antimonate antimonite in the glycerine water solution of excessive caustic soda formed it is sweet
Oily complex compound, and natrium arsenicum, sodium arsenite, soda ash, sodium bicarbonate can be directly dissolved in glycerine water solution under certain condition,
Molten arsenic alkaline slag is directly soaked with caustic soda glycerine water solution, soaks the molten antimony isolated in arsenic alkaline slag, lead, bismuth, arsenic and soda ash, and can be more
Grade soaks molten mode and is kept completely separate out antimony (leaded, bismuth), arsenic and soda ash in alkaline residue；
(2) solubility with temperature using arsenate in caustic soda glycerine water solution increases and increases, and its solubility with temperature
Variation is more sensitive, in a manner of crystallisation by cooling dearsenification, preferentially isolates arsenate arsenite crystal；
It (3) can be in sulfidion (such as H for lead, the bismuth glycerol complex compound in caustic soda glycerine water solution2S、Na2S under) interfering
Decomplexing be converted into the vulcanized lead of indissoluble, bismuth sulfide precipitating, and highly basic effect under will not generate thioantimonate the characteristics of, add
Na2S precipitation and separation goes out incident lead bismuth；
(4) using glycerol antimony complex in the case that lose caustic soda strong basicity support, complex structure disintegrate, antimony ion with
Antimony powder form precipitating is aoxidized, with CO2The NaOH neutralized in solution is converted into Na2CO3, and controlling pH value of solution is 11.5~11.7, is prevented
Only there is analysis alkali (NaHCO3) antimony oxide purity increase purification difficulty is influenced, and isolate antimony；
(5) using the phytic acid of extracted form natural plant can quick complex-precipitation all bivalent metal ions and heavy metal ion spy
Point, remove the molten separation lead of leaching, arsenic, all bivalent metal ions and heavy metal remaining in the glycerol soda ash aqueous solution after antimony from
Son.And the soda ash solution of isolated glycerine water solution and concentration is analysed using nanofiltration and/or reverse osmosis membrane.Glycerine water solution returns
The molten arsenic alkaline slag of leaching is returned, concentration soda ash liquid (being free of arsenic antimony lead) is for refining pure alkali product or adds calcining magnesia or lime causticization
Produce caustic soda；
(6) technique is simpler, and investment is less, and good separating effect, treating capacity is big, and can easily realize no dust work, without secondary
Pollution；
(7) a kind of completely new technical thought is provided for the processing that efficiently separates of arsenic alkaline slag, is also soda ash, caustic soda, arsenic product, antimony
The raw material that the production of product etc. provides convenient for utilizing.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Chemical reagent used in the embodiment of the present invention is obtained by routine business approach unless otherwise specified.
Embodiment 1
Certain antimony smeltery arsenic alkaline slag is selected, As 9.73%, Sb 26.18%, Pb 5.79%, Na 22.76% are detected；Select city
Sell industry glycerol (content 98.5%), caustic soda (piece alkali NaOH content 96%), hydrochloric acid (content 35%), phytic acid (content 95%), liquefaction
Carbon dioxide is raw material, and water uses tap water.
The present embodiment is the following steps are included: the arsenic alkaline slag powder of grinding to 200 mesh screen residues 3% is sent into and is soaked in molten tank, in mass ratio
Arsenic alkaline slag powder: water: glycerol: water, glycerol, caustic soda is added in caustic soda=1:3:2:0.73 ratio, controls pH stable 14, Yu Chang
Molten 3h are soaked in pressure, 85 DEG C of stirrings, separate, and obtain siulica-alumina mineral slag, alkali glycerine water solution (complex compound containing glycerol, caustic soda, arsenate and pure
The mixed solution of alkali)；Alkali glycerine water solution is cooled to 0 DEG C of crystallization, and separation obtains the alkali glycerine water solution of arsenic acid salt crystal, dearsenification
(mixed solution of antimonial lead bismuth glycerol complex compound, caustic soda and soda ash)；Then, in the alkali glycerine water solution of dearsenification under room temperature
Sodium sulfide solution reaction is added dropwise and generates vulcanized lead, bismuth sulfide precipitating, separation obtains the alkali glycerine water solution of lead skim, de- lead (containing glycerol
The mixed solution of antimony complex, caustic soda and soda ash)；It is passed through carbon dioxide gas in 30 DEG C in the alkali glycerine water solution of de- lead, in
And caustic soda, reaction to pH value are reduced to 11.5~11.7, antimony complex decomposes precipitating, and separation obtains the glycerol of antimonial, de- antimony
Aqueous solution；In 30 DEG C, appropriate phytic acid is added dropwise in the glycerine water solution of de- antimony, react whole divalent ions in precipitation solution and
Heavy metal ion, separation, obtains phytate precipitates, micro-filtration filters to obtain glycerol soda ash aqueous solution；Glycerol soda ash aqueous solution is in 35 DEG C
It is handled with nano filter membrance device, UF membrane obtains nanofiltration concentrate, dialyzate glycerine water solution；It is molten that dialyzate glycerine water solution returns to leaching
Arsenic alkaline slag；Soda ash powder-product is made in nanofiltration concentrate spray drying.
Detection: the siulica-alumina mineral slag after leaching simultaneously separation: predominantly aluminosilicate mineral, antimony content 0.89%, arsenic content
0.08%, lead content 0.23%, soda content 0.87%, TCLP experiment detect arsenic content 0.37mg/L in solution, are general solid waste.
Arsenic content 0.16%, carbonate content 1.14% in antimonial；Antimony content 0.47% in lead skim, arsenic content 0.29%,
Carbonate content 1.89%；Antimony content 0.21%, carbonate content 1.89% in arsenate；Antimony content 0.0009%, arsenic contain in soda ash
Amount 0.0002%.Antimony recovery 98.79%, lead recovery 98.63%, the arsenic rate of recovery 99.55%, the soda ash rate of recovery 96.87%.Explanation
Soak that molten separation antimony, lead, arsenic, the effect of alkali are fine with alkali glycerine water solution, and antimonial after separating and recovering, arsenate, pure
Objectionable impurities in alkali, lead skim is convenient for removing.
Embodiment 2
Certain antimony smeltery arsenic alkaline slag is selected, As 11.26%, Sb 24.35%, Pb 2.77%, Na 24.12% are detected；It selects
Commercially available industry glycerol (content 98.5%), caustic soda (piece alkali NaOH content 96%), hydrochloric acid (content 35%), phytic acid (content 95%), liquid
Change carbon dioxide is raw material, and water uses tap water.
The present embodiment is the following steps are included: set the leaching solute amount ratio of arsenic alkaline slag as arsenic alkaline slag: water: glycerol: caustic soda=1:
3.5: 2.5: 0.95, it is first partial size < 74 μm by arsenic alkaline slag and water, the glycerol ratio of 1:2:1 in mass ratio together grinding
Slurry is sent into and is soaked in molten tank, and water, glycerol, caustic soda amount are supplied, and control pH stable soaks molten 14 in normal pressure, 95 DEG C of stirrings
1.5h, separation, obtains siulica-alumina mineral slag, alkali glycerine water solution；Alkali glycerine water solution is cooled to 8 DEG C of crystallizations, separation, obtains arsenate crystalline substance
Body, dearsenification alkali glycerine water solution；Sodium sulfide solution, lead bismuth complex solution is added dropwise in the alkali glycerine water solution of dearsenification under room temperature
Analysis reaction generates vulcanized lead, bismuth sulfide precipitating, and separation obtains the alkali glycerine water solution of lead skim, de- lead；The alkali glycerine water solution of de- lead
It is passed through carbon dioxide gas in 60 DEG C, neutralizes caustic soda, reaction to pH value is reduced to 11.5~11.7, and the parsing of glycerol antimony complex is heavy
It forms sediment, separation obtains the glycerine water solution of antimonial, de- antimony；In 40 DEG C, appropriate phytic acid is added dropwise in the glycerine water solution of de- antimony,
React the whole divalent ions and heavy metal ion in precipitation solution, separation obtains phytate precipitates, micro-filtration filter glycerol is pure
Aqueous alkali；Glycerol soda ash aqueous solution is separated in 37 DEG C with reverse osmosis membrane apparatus, obtains concentrate, dialyzate glycerine water solution.Thoroughly
It analyses liquid glycerine water solution and returns and soak molten arsenic alkaline slag；Concentrate adds lime causticization that caustic soda is made by mature causticization process, for arsenic alkali
The synchronous of slag soaks molten separation.
Detection: the siulica-alumina mineral slag after leaching simultaneously separation: predominantly aluminosilicate mineral, antimony content 0.68%, arsenic content
0.07%, lead content 0.21%, soda content 0.59%, TCLP experiment detect arsenic content 0.38mg/L in solution, are general solid waste.
Arsenic content 0.19%, carbonate content 0.97% in antimonial；Antimony content 0.61% in lead skim, arsenic content 0.27%,
Carbonate content 1.73%；Antimony content 0.29%, carbonate content 2.11% in arsenate；Antimony content 0.0008%, arsenic contain in caustic soda
Amount 0.0002%.Antimony recovery 98.93%, lead recovery 98.97%, the arsenic rate of recovery 99.36%, alkali recovery 98.61%.Illustrate with
Alkali glycerine water solution soaks that molten separation antimony, lead, arsenic, the effect of alkali are fine, and antimonial after separating and recovering, arsenate, soda ash,
Objectionable impurities in lead skim is convenient for removing.
Embodiment 3
Certain antimony smeltery arsenic alkaline slag is selected, As 17.84%, Sb 14.87%, Pb 3.42%, Na 26.70% are detected；It selects
Commercially available industry glycerol (content 98.5%), caustic soda (piece alkali NaOH content 96%), hydrochloric acid (content 35%), phytic acid (content 95%), liquid
Change carbon dioxide is raw material, and water uses tap water.
The present embodiment is the following steps are included: set the leaching solute amount ratio of arsenic alkaline slag as arsenic alkaline slag: water: glycerol: caustic soda=1:
4: 2.5: 1.3, it is first the slurry of partial size < 74 μm by arsenic alkaline slag and water, the glycerol ratio of 1:2:1 in mass ratio together grinding
Material is sent into and is soaked in molten tank, and water, glycerol, caustic soda amount are supplied, and control pH stable soaks molten 1.2h 14, in normal pressure, 90 DEG C of stirrings,
Separation, obtains siulica-alumina mineral slag, alkali glycerine water solution；Alkali glycerine water solution is cooled to -2 DEG C of crystallizations, separation, obtain arsenic acid salt crystal,
The alkali glycerine water solution of dearsenification；In the alkali glycerine water solution of dearsenification under room temperature be added dropwise sodium sulfide solution reaction generate vulcanized lead,
Bismuth sulfide precipitating, separation obtain the alkali glycerine water solution of lead skim, de- lead；Dioxy is passed through in 80 DEG C in the alkali glycerine water solution of de- lead
Change carbon gas, neutralize caustic soda, reaction to pH value is reduced to 11.5~11.7, and antimony complex decomposes precipitating, and separation obtains antimony chemical combination
The glycerine water solution of object, de- antimony；A small amount of phytic acid is added dropwise in the glycerine water solution of de- antimony, reacts whole divalent in precipitation solution
Ion and heavy metal ion, separation, obtain phytate precipitates, micro-filtration filters to obtain glycerol soda ash aqueous solution；Glycerol soda ash aqueous solution
In 38 DEG C with nano filter membrance device UF membrane, nanofiltration concentrate, dialyzate glycerine water solution are obtained.Dialyzate glycerine water solution returns to leaching
Molten arsenic alkaline slag；Soda ash powder-product is made in nanofiltration concentrate spray drying.
Detection: the siulica-alumina mineral slag after leaching simultaneously separation: predominantly aluminosilicate mineral, antimony content 0.36%, arsenic content
0.02%, lead content 0.23%, soda content 0.39%, TCLP experiment detect arsenic content 0.17mg/L in solution, are general solid waste.
Arsenic content 0.09%, carbonate content 0.87% in antimonial；Antimony content 0.69% in lead skim, arsenic content 0.24%,
Carbonate content 1.47%；Antimony content 0.18%, carbonate content 0.89% in arsenate；Antimony content 0.0008%, arsenic contain in soda ash
Amount 0.0001%.Antimony recovery 99.21%, lead recovery 98.43%, the arsenic rate of recovery 99.51%, the soda ash rate of recovery 93.87%.Explanation
It is fine that molten separation antimony, lead, arsenic, the effect of alkali are soaked with alkali glycerine water solution.
Embodiment 4
Certain antimony smeltery arsenic alkaline slag is selected, As 8.76%, Sb 21.35%, Pb 5.32%, Na 24.74% are detected；Select city
Sell industry glycerol (content 98.5%), caustic soda (piece alkali NaOH content 96%), hydrochloric acid (content 35%), phytic acid (content 95%), liquefaction
Carbon dioxide is raw material, and water uses tap water.
For the present embodiment the following steps are included: arsenic alkaline slag crushing and grinding is to 350 mesh screen residues 12%, arsenic alkaline slag powder equivalent is sent into three
In a leaching can, setting leaching solute amount is than arsenic alkaline slag powder: water: glycerol: caustic soda=1:5:3:1.5 uses three-level in normal pressure, 87 DEG C
Molten, the first order stirring molten 0.7h of leaching is soaked, separation is filtered, alkali glycerine water solution is transferred to the second level leaching can molten 0.7h of interior stirring leaching,
Separation is filtered, alkali glycerine water solution is transferred to stirring in third level leaching can and soaks molten 0.7h, filters separation, micro-filtration filters to obtain saturation alkali
Glycerine water solution；After filtering out solution in first order pot for solvent extraction, the new alkali glycerine water solution of equal amount is added again and soaks molten 0.7h
Smoke filtrate is transferred to second level leaching can, and smoke filtrate is transferred to third level leaching can after soaking molten 0.7h, in this way, arsenic alkaline slag is through alkali glycerol liquor
Solution sufficiently soaks molten, separation, obtains siulica-alumina mineral slag, saturation alkali glycerine water solution；Saturation alkali glycerine water solution is cooled to 0 DEG C of knot
Crystalline substance, separation, obtains the alkali glycerine water solution of arsenic acid salt crystal, dearsenification；Vulcanization is added dropwise in the alkali glycerine water solution of dearsenification under room temperature
Sodium solution reaction generates vulcanized lead, bismuth sulfide precipitating, and separation obtains the alkali glycerine water solution of lead skim, de- lead；In 30 DEG C, in de- lead
Alkali glycerine water solution in plus hydrochloric acid be neutralized to pH6.5, glycerol antimony complex resolves to oxidation antimony powder precipitating, and separation must aoxidize
The glycerine water solution of antimony, de- antimony.Then, a small amount of reaction of phytic acid is added dropwise in glycerine water solution, whole two be settled out in solution
Valence ion and heavy metal ion, micro-filtration are separated by filtration, and obtain phytate precipitates, glycerol saline solution；Glycerol saline solution is in 37
DEG C nanofiltration UF membrane, obtains nanofiltration concentrate, dialyzate glycerine water solution；Dialyzate glycerine water solution, which returns, soaks molten arsenic alkaline slag, receives
Sodium chloride powder finished product is made in filter concentration liquid spray drying.
Detection: the siulica-alumina mineral slag after leaching simultaneously separation: predominantly aluminosilicate mineral, antimony content 0.24%, arsenic content
0.01%, lead content 0.19%, soda content 0.13%, TCLP experiment detect arsenic content 0.04mg/L in solution, are general solid waste.
Antimony aoxidizes arsenic content 0.01%, carbonate content 0.84% in cereal；Antimony content 0.49%, arsenic content in lead skim
0.17%, carbonate content 1.32%；Antimony content 0.14%, carbonate content 1.07% in arsenate；Antimony content in sodium chloride
0.0005%, arsenic content 0.0001%.Antimony recovery 99.6%, lead recovery 98.79%, the arsenic rate of recovery 99.71%, the soda ash rate of recovery
0%(soda ash is completely converted into sodium chloride salt).Illustrate to soak molten separation antimony, lead, arsenic, the effect of alkali with alkali glycerine water solution fine.
Embodiment 5
Certain antimony smeltery arsenic alkaline slag is selected, As 11.32%, Sb 19.72%, Pb 2.57%, Na 26.83% are detected；It selects
Commercially available industry glycerol (content 98.5%), caustic soda (piece alkali NaOH content 96%), hydrochloric acid (content 35%), phytic acid (content 95%), liquid
Change carbon dioxide is raw material, and water uses tap water.
The present embodiment soaks leaching solute amount ratio in molten tank as arsenic alkaline slag the following steps are included: setting the first order: water: glycerol:
Caustic soda=1: 3: 2:1, it is molten using three-level leaching in normal pressure, 87 DEG C.First by arsenic alkaline slag and water, glycerol 1:2:0.5 in mass ratio
Ratio together grinding be partial size < 80 μm slurry, arsenic alkaline slag slurry equivalent is sent into three molten tanks of leaching, and the first order is soaked in molten tank
Water, glycerol, caustic soda amount are supplied, for control pH stable 14, molten 1.2h is soaked in first order stirring, filters separation, alkali glycerine water solution
It is transferred to the second level and soaks the molten 1.2h of stirring leaching in molten tank, suction filtration separation, alkali glycerine water solution, which is transferred to the third level and soaks to stir in molten tank, to be soaked
Molten 1.2h filters separation, micro-filtration filters to obtain saturation alkali glycerine water solution；After filtering out solution in the molten tank of first order leaching, mend again
Add the new alkali glycerine water solution of equal amount to soak molten 1.2h smoke filtrate and be transferred to second level leaching can, soaks smoke filtrate after molten 1.2h and be transferred to the
It is water-soluble to obtain siulica-alumina mineral slag, saturation alkali glycerol in this way, arsenic alkaline slag sufficiently soaks molten, separation through alkali glycerine water solution for three-level leaching can
Liquid；Saturation alkali glycerine water solution is cooled to 0 DEG C of crystallization, separates, obtains the alkali glycerine water solution of arsenic acid salt crystal, dearsenification；Dearsenification
The reaction of dropwise addition sodium sulfide solution generates vulcanized lead, bismuth sulfide precipitating under room temperature in alkali glycerine water solution, and separation obtains lead skim, takes off
The alkali glycerine water solution of lead；It is passed through carbon dioxide gas in 35 DEG C in the alkali glycerine water solution of de- lead, neutralizes caustic soda, reaction to pH
Value is reduced to 11.5~11.7, and antimony complex decomposes precipitating, and separation obtains the glycerine water solution of antimony oxygen compound, de- antimony；In 35
DEG C, appropriate phytic acid is added dropwise in the glycerine water solution of de- antimony, reacts whole divalent ions and heavy metal ion in precipitation solution,
Separation, obtains phytate precipitates, micro-filtration filters to obtain glycerol soda ash aqueous solution；Glycerol soda ash aqueous solution is filled in 35 DEG C with nanofiltration membrane
Film analysis separation is set, nanofiltration concentrate, dialyzate glycerine water solution are obtained.Dialyzate glycerine water solution, which returns, soaks molten arsenic alkaline slag；Nanofiltration
Soda ash powder-product is made in concentrate spray drying.
Detection: the siulica-alumina mineral slag after leaching simultaneously separation: predominantly aluminosilicate mineral, antimony content 0.072%, arsenic content
0.008%, lead content 0.194%, soda content 0.874%, TCLP experiment detect arsenic content 0.05mg/L in solution, are general solid
It is useless.
Arsenic content 0.11%, carbonate content 1.03% in antimonial；Antimony content 0.37% in lead skim, arsenic content 0.17%,
Carbonate content 1.49%；Antimony content 0.26%, carbonate content 1.81% in arsenate；Antimony content 0.0009%, arsenic contain in soda ash
Amount 0.0001%.Antimony recovery 99.4%, lead recovery 98.63%, the arsenic rate of recovery 99.7%, the soda ash rate of recovery 96.87%.Illustrate with
It is fine that alkali glycerine water solution soaks molten separation antimony, lead, arsenic, the effect of alkali.
Claims (10)
1. a kind of method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag, which comprises the following steps: will be by broken
The arsenic alkaline slag of flour mill adds water, glycerol and caustic soda or the slurry after arsenic alkaline slag and water, glycerol and caustic soda together grinding is sent into leaching
In molten tank, pH value is controlled, carries out soaking molten extraction, is separated by solid-liquid separation, obtain siulica-alumina mineral slag and alkali glycerine water solution；The alkali glycerol liquor
Solution be complex compound containing glycerol, caustic soda, arsenate and soda ash mixed solution, gained alkali glycerine water solution successively carry out dearsenification,
After de- lead, de- antimony and purification precipitating divalent ion and heavy mental treatment, arsenic acid salt crystal, lead skim, antimony oxide, phytic acid are obtained
The glycerol soda ash aqueous solution of salt sediment and purification；Gained glycerol soda ash aqueous solution send nanofiltration membrane analysis or reverse osmosis membrane to analyse to obtain concentration
Liquid and dialyzate glycerine water solution；Gained dialyzate glycerine water solution, which returns, soaks molten arsenic alkaline slag；Gained concentrate spray drying system
At soda ash or calcining magnesia or lime causticization is added to produce caustic soda；Gained antimony oxide is for returning to antimony refining or processing antimony or essence
Oxygenerating antimony and metaantimmonic acid product salt.
2. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag according to claim 1, which is characterized in that the arsenic
Alkaline residue: water: glycerol: caustic soda is 1:1~8:0.5~5:0.3~3 in mass ratio.
3. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag according to claim 1 or 2, which is characterized in that institute
State control pH=14.
4. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag described according to claim 1~one of 3, feature exist
In the molten extraction of leaching soaks molten 0.5h~8h for 60 DEG C~150 DEG C stirrings；The molten extraction of leaching soaks molten or multistage leaching using single-stage
Molten or leaching trough counter-current leaching is molten.
5. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag described according to claim 1~one of 4, feature exist
In the dearsenification is by alkali glycerine water solution crystallisation by cooling, and separation obtains the alkali glycerine water solution of arsenic acid salt crystal and dearsenification；Institute
The alkali glycerine water solution for stating dearsenification is the mixed solution of antimonial lead bismuth glycerol complex compound, caustic soda and soda ash.
6. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag described according to claim 1~one of 5, feature exist
In the de- lead is that the alkali glycerine water solution of dearsenification is added dropwise to sodium sulfide solution reaction to generate vulcanized lead, bismuth sulfide precipitating, separation
Sulfide precipitation obtains the alkali glycerine water solution of the lead skim and de- lead based on lead-containing compounds；The alkali glycerine water solution of the de- lead
For the mixed solution of antimony complex containing glycerol, caustic soda and soda ash.
7. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag described according to claim 1~one of 6, feature exist
In the precipitating divalent ion and heavy mental treatment are that will be added dropwise to plant in the glycerine water solution of de- antimony at 10 DEG C~50 DEG C
Acid, reacts whole divalent ions and heavy metal ion in precipitation solution, and it is water-soluble to obtain phytate precipitates, glycerol soda ash for separation
Liquid.
8. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag described according to claim 1~one of 7, feature exist
In the de- antimony is that carbon dioxide is passed through in the alkali glycerine water solution of de- lead at 5 DEG C~95 DEG C, neutralizes caustic soda, reaction to pH
Value is reduced to 11.5~11.7, and the glycerol antimony complex parsing for reacting generation is settled out oxidation antimony powder, separates, and obtains antimony oxide, takes off
The glycerine water solution of antimony.
9. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag described according to claim 1~one of 7, feature exist
In, the de- antimony be in the alkali glycerine water solution of de- lead plus hydrochloric acid is neutralized to pH value 6~7.8, is separated, obtain antimony oxygen compound and
The glycerine water solution of de- antimony.
10. the method that antimony, arsenic, alkali leaching simultaneously separate in arsenic alkaline slag described according to claim 1~one of 9, feature exist
In the glycerol is using mannitol or xylose alcohol part substitution or replacing whole；The caustic soda is substituted using potassium hydroxide.
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