CN107460330B - A kind of method that potassium salt system pressure oxidation prepares sodium pyroantimonate - Google Patents
A kind of method that potassium salt system pressure oxidation prepares sodium pyroantimonate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/02—Working-up flue dust
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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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- 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
A kind of method that potassium salt system pressure oxidation prepares sodium pyroantimonate, antimony cigarette ash is passed through oxygen pressing oxidation water soaking dearsenication in high temperature aqueous solution, pressure oxidation water logging slag is passed through oxygen pressing alkali oxide leaching dissolving antimony in potassium hydroxide system, then potassium sulfide is added into pressurised oxygen choline immersion liquid again and removes lead, sodium hydroxide pellets antimony, sediment output sodium pyroantimonate product after washing and drying is finally added into liquid after purification under an increased pressure.The essence of the present invention is to realize the precipitation of the dissolving of arsenic, the dissolving of antimony and antimony respectively using pressure oxidation water logging, the leaching of pressurised oxygen choline and three kinds of modes of pressurized precipitation, pressure oxidation water logging process arsenic leaching rate reaches 85.0% or more, the leaching rate of the dipped journey antimony of pressurised oxygen choline reaches 90.0% or more, the rate of deposition of pressurized precipitation process antimony reaches 95.0% or more, realizes the purpose for removing arsenic from antimony cigarette ash and preparing sodium pyroantimonate.The present invention has the advantages that high antimony direct yield, good product quality and at low cost.
Description
Technical field
The present invention relates to heavy metal metallurgy processes in nonferrous metallurgy field, especially effectively in potassium salt system from antimony cigarette ash
Middle pressure oxidation prepares the Wet-process metallurgy method of sodium pyroantimonate.
Background technology
Antimony is the silvery white non-ferrous metal of a kind of crisp property, electric conductivity and poor heat conduction, is mainly used for alloy, war industry, resistance
Fire the industries such as agent and glass.China is that the maximum country of antimony yield, global antimony yield in 2010 are 16.7 ten thousand tons in the world,
And China's antimony yield in 2010 reaches 15.0 ten thousand tons, accounts for 89% or more of world's antimony yield, China is upper equal in antimony resource and production
With the advantage that do not replace.The mineral raw material that antimony is smelted mainly has stibnite, Sb-Au ore and jamesonite etc., and antimony cigarette ash
It is then the important secondary raw material for recycling antimony, often producing 100,000 tons of lead can 500 tons of antimony metal amount of output.
Antimony cigarette ash main source is the by-product that heavy metal is smelted, since antimony and the usually mutual association of arsenic are smelted in heavy metal
Raw material in, so, arsenic is typical impurity element in antimony cigarette ash, since arsenic and antimony are adjoining element of the same clan, physical chemistry
Property is similar, causes its separation difficult.There is antimony higher economic value, the presence of arsenic to make the recycling of antimony tired in antimony cigarette ash
Difficulty, and environment is caused to seriously endanger.Therefore the removing of arsenic and the recycling of antimony have the important value of environmental protection and warp in antimony cigarette ash
Ji value.
The processing of antimony cigarette ash at present mainly has a thermal process and wet processing two major classes, wherein thermal process it is more mature
Industrially it is used widely.Arsenic stibium fire separating technology mainly makes arsenic trioxide volatilization separation using the methods of roasting,
But since arsenic antimony property is similar, usually there is arsenic and antimony is detached and is not thorough, in addition, there is building rings for pyrogenic process volatilization separation arsenic
The problems such as border is poor, environmental pollution is big and high energy consumption.The method that metallargist has been working hard exploitation wet separation antimony and arsenic, it is main
The method to be studied has the four systems such as aqueous systems, hydrochloric acid system, sodium hydroxide system and vulcanized sodium system.These systems are
Using the difference of antimony and arsenic compound solubility property, efficiently separating for antimony and arsenic is realized in leaching or subsequent process, however it remains
The disadvantage that separating by extraction is low, wastewater flow rate is big, reagent consumption is big and processing cost is high.So selection antimony cigarette ash reasonably detaches
The method of arsenic is particularly important.
In related antimony cigarette ash antimony with which kind of product form using be also it is extremely important, the major product of antimony have metal antimony slab,
Stibium trioxide and sodium pyroantimonate, wherein sodium pyroantimonate are mainly used as the fining agent and decolorising agent of industrial glass, with its glass obtained
Product has transparency high, and the advantage of illumination invariant color, small toxicity is widely used in television picture tube, high-grade glass, wards off
The fields such as porcelain industry, electronics industry semiconductor, account for very high proportion in antimony product, are a kind of finings that economic prospect is wide
Chemical product.Since antimony mainly exists with oxide in antimony cigarette ash, so, it is to close very much to prepare sodium pyroantimonate product using antimony cigarette ash
Reason.
According to raw material chemical property, two classes can be divided by producing the raw material used in sodium pyroantimonate, one kind be with industrial star antimony,
Industrial stibium trioxide is the high-purity antimony product raw material of representative, and one kind is former as the high impurity antimony resource of representative using stibnite, antimony cigarette ash
Material.The existing method for preparing sodium pyroantimonate mainly has sodium nitrate oxidizing process, hydrogen peroxide oxidation method, sylvite method, chloridising and air
Oxidizing process.Pyrometallurgical smelting process is wherein belonged to sodium nitrate oxidizing process, remaining belongs to wet method smelting process.
Sodium nitrate oxidizing process is aoxidized with sodium nitrate under the conditions of high-temperature alkaline using metallic antimony or antimony oxide as raw material
The conventional method of sodium antimonate is prepared, first mixes metallic antimony with excessive sodium nitrate, being roasted under rotary furnace high temperature makes antimony
It is oxidized to pentavalent, drying and crushing after removing sodium nitrate is finally washed with water, sodium pyroantimonate product is made.Sodium nitrate oxidizing process has work
The advantages that skill is simple, flow is short and operation is easy, but impurity cannot be removed effectively in process of production, and in production process
Exhaust gas cannot thoroughly effect a radical cure, product quality is of low grade, institute in this way at present substantially do not have producer use.
Hydrogen peroxide oxidation method is that hydrogen peroxide direct oxidation antimony oxide is used in sodium hydroxide solution, prepared by one-step method
The method of sodium pyroantimonate.Antimony oxide, sodium hydroxide and water are proportionally added into reactor by this method, when slurries heat
Hydrogenperoxide steam generator is added dropwise after to certain temperature and carries out oxidation back flow reaction, rear drying sodium antimonate is washed with water in reaction product
Product.Hydrogen peroxide oxidation method has many advantages, such as that simple for process, flow is short and easy to operate, but there are poor product quality and is produced into
This high disadvantage.Many researchs at present are dedicated to the problems such as solving adaptability to raw material, technique purification capacity and improving product quality.
Sylvite method is that solubility is larger in aqueous solution based on potassium pyroantimonate, and sodium pyroantimonate be almost not dissolved in water this
One property prepares sodium pyroantimonate, and Sb (III) is oxidized to Sb (V) dissolving, liquid with hydrogen peroxide first in potassium hydroxide system
Gu sodium hydroxide pellets output sodium pyroantimonate product is added after separation into solution.The major advantage of sylvite method is sodium pyroantimonate production
Quality is good, and major defect is that potassium hydroxide system consumes a large amount of hydrogen peroxide, and sylvite is mingled with loss seriously in intermediate product, causes
Production cost is excessively high.
Chloridising is will to contain antimony raw material to be leached with chlorine oxidation in hydrochloric acid system, leachate sodium hydroxide neutralizing hydrolysis
Output sodium pyroantimonate precipitates, and sodium pyroantimonate product is obtained after washing and drying.Chloridising has ingredient requirement low and product
High-quality advantage, but have the shortcomings that long technological process, equipment seriously corroded and wastewater flow rate are big.
Air oxidation process be using stibnite concentrate or fragile S-Pb-Sb concentrate as raw material, with vulcanized sodium and leaching with sodium hydroxide,
Antimony enters solution with Sodium thioantimonite, blast air by Sodium thioantimonite be oxidized to sodium pyroantimonate precipitation, by washing and
It is dried to obtain sodium pyroantimonate product, oxidated solution recycles sodium thiosulfate byproduct after neutralization, removal of impurities and condensing crystallizing.It is empty
Gas oxidizing process directly produces sodium pyroantimonate using sulphide ore, cost is greatly reduced, but there are technological process length and products
Ropy disadvantage.Also there is the time researched and proposed and shorten air oxidation using pressure oxidation mode, achieve certain effect.
According to the advantage and disadvantage of above-mentioned each method, which kind of method is selected to prepare sodium pyroantimonate product, on the one hand needs to overcome biography
On the other hand the low disadvantage of the leaching rate of system needs to realize the purpose for reducing production cost, institute by the dosage for reducing oxidant
With it is proposed that preparing sodium pyroantimonate product using pressure oxidation method in potassium hydroxide system.
Invention content
In order to overcome the shortcomings of that antimony cigarette ash tradition prepares sodium pyroantimonate method, the present invention provides a kind of potassium salt system pressurised oxygen
Change mode prepares sodium pyroantimonate, and antimony direct yield height, good product quality and Wet-process metallurgy method at low cost from antimony cigarette ash.
The technical solution adopted by the present invention is in order to achieve the above objectives：Antimony cigarette ash is passed through oxygen pressing in high temperature aqueous solution
Water logging is aoxidized, so that various arsenic oxides is dissolved in the form of arsenic acid and enters infusion, then pressure oxidation water logging slag is in potassium hydroxide
It is passed through the leaching of oxygen pressing alkali oxide in system, so that trivalent antimony is oxidized to potassium pyroantimonate dissolving and enters alkali immersion liquid, then again to pressurization
Potassium sulfide is added in alkali oxide immersion liquid, so that the potassium plumbite of dissolving is generated vulcanized lead precipitation, finally under an increased pressure to after purification
Be added sodium hydroxide pellets antimony in liquid, sediment output sodium pyroantimonate product after washing and drying, after precipitation liquid return plus
Press the dipped journey of alkali oxide.The essence of the present invention is using pressure oxidation water logging, the leaching of pressurised oxygen choline and three kinds of modes of pressurized precipitation
Three purposes of precipitation for realizing the dissolving of arsenic, the dissolving of antimony and antimony respectively finally prepare qualified sodium pyroantimonate product, this
A little process tight associations, collective effect realize the purpose for removing arsenic from antimony cigarette ash and preparing qualified sodium pyroantimonate product.
Specific technical process and technological parameter are as follows：
1 pressure oxidation water logging
Antimony cigarette ash is passed through oxygen pressing oxidation water logging in high temperature aqueous solution；Antimony cigarette ash presses liquid-solid ratio（Water volume L and antimony cigarette
The ratio between grey quality kg）2~6/1 add water slurry, then mixed slurry are added in stainless steel autoclave, into reaction kettle
Oxygen is passed through so that remaining air is discharged, ventilate 1~5min when controlling 0.2~0.5MPa of oxygen partial pressure, and then heating increases temperature
For degree to 150~225 DEG C, control oxygen partial pressure is that 0.5~1.0MPa reacts 1~5h, reaction complete it is cooling reduce temperature to 60~
At 80 DEG C, solid-liquor separation is realized using vacuum filtration mode, for curing arsenic, pressure oxidation water logging slag is sent pressure oxidation infusion
Pressurised oxygen choline soaks process, and the main chemical reactions of pressure oxidation water logging process are as follows：
As2O3+O2+3H2O=2H3AsO4（1）
Pb(AsO2)2+O2+3H2O=2H3AsO4+PbO （2）
Pb(AsO3)2+3H2O=2H3AsO4+PbO （3）
2 pressurised oxygen cholines soak
Pressure oxidation water logging slag pressurised oxygen choline in potassium hydroxide system soaks；Compound concentration is 1.5~2.5mol/L's
Potassium hydroxide solution, by liquid-solid ratio（The ratio between liquor capacity L and pressure oxidation water logging slag amount kg）3~10/1 are added pressure oxidation
Water logging slag, which is added in autoclave, and oxygen is passed through into reaction kettle so that remaining air is discharged, controls oxygen
Divide 0.2~0.5MPa when ventilate 1~5min, then heating increase temperature to 100~109 DEG C, control oxygen partial pressure be 0.5~
1.0MPa reacts 1~5h, when reaction completes cooling reduction temperature to 85~95 DEG C, realizes that liquid divides admittedly using vacuum filtration mode
From cleaning procedure is sent in pressurised oxygen choline phase analysis Returning smelting, pressurised oxygen choline immersion liquid；The dipped journey of pressurised oxygen choline occurs main
Chemical reaction is as follows：
Sb2O3+2KOH+O2+5H2O=2KSb(OH)6（4）
PbO+2KOH+H2O=K2Pb(OH)4（5）
3 purifications
Pressurised oxygen choline immersion liquid is added potassium sulfide purification and removes lead；Pressurised oxygen choline immersion liquid keeps 80~95 DEG C of temperature, then
Solid potassium sulfide purification removing lead is added, vulcanization potassium application rate is 1.0~1.1 times of theoretical amount, while be added phase homogenous quantities and
Granularity is the activated carbon of 5.0~10.0mm, is separated by solid-liquid separation using vacuum filtration mode after reacting 0.5~2.0h, purification slag recycling
Lead, liquid send pressurized precipitation process after purification；The main chemical reactions that purification process occurs are as follows：
K2Pb(OH)4+K2S=PbS↓+4KOH （6）
4 pressurized precipitations
Sodium hydroxide pressurized precipitation output sodium pyroantimonate product is added in liquid after purification；Liquid is added to stainless steel high pressure after purification
In reaction kettle, sodium hydroxide is added into reaction kettle, sodium hydroxide concentration is 0.9~1.0 times of theoretical amount, keeps slurry temperature
95~105 DEG C, control oxygen partial pressure is that 0.1~0.3MPa reacts 1~5h, and reaction completes the cooling temperature that reduces to 85~95 DEG C
When, using vacuum filtration mode realization solid-liquor separation, liquid returns to pressurised oxygen choline leaching process after precipitation, and sediment is with temperature
80-90 DEG C of hot water presses liquid-solid ratio（The ratio between water volume L and sediment quality kg）2~5/1 washings, finally in temperature 80~100
Drying obtains sodium pyroantimonate at DEG C；The main chemical reactions that pressurized precipitation process occurs are as follows：
KSb(OH)6+NaOH=NaSb(OH)6↓+kOH （7）
Oxygen of the present invention is industrial oxygen, and oxygen purity is more than 95.0%.
The present invention is suitable for processing antimony cigarette ash, and main component range is with weight（%）：Sb10.0~
60.0, As1.0~35.0 and Pb1.0~10.0.
Compared with the present invention prepares sodium pyroantimonate method with antimony cigarette ash tradition, have the advantage that：1, it is adopted in high temperature aqueous solution
Most of arsenic is effectively stripped of in antimony cigarette ash with pressure oxidation mode, and the leaching rate of arsenic can reach 85.0% or more, chemical reagent
Consumption is few；2, pressure oxidation water logging slag is passed through oxygen pressing alkali oxide leaching antimony in potassium hydroxide system, and the leaching rate of antimony reaches
90.0% or more；3, the immersion liquid of pressurised oxygen choline is added potassium sulfide purification and removes lead, and activated carbon is added and ensures that purification can be suitable except lead process
Profit carries out；4, liquid addition sodium hydroxide pressurized precipitation goes out out sodium pyroantimonate product after purifying, and antimony rate of deposition reaches 95.0% or more；
5, the present invention has the advantages that technical process technical indicator is stable, labor intensity is small low with production cost etc..
Description of the drawings
Fig. 1：Present invention process flow diagram.
Fig. 2：The SEM of sodium pyroantimonate product of the present invention schemes.
Fig. 3：The XRD diagram of sodium pyroantimonate product of the present invention.
Specific implementation mode
Embodiment 1：Antimony cigarette ash main component is with weight（%）：Sb48.5, As18.4 and Pb5.7.Antimony cigarette
Ash is added to by liquid-solid ratio 4/1 plus water slurry, slurry in stainless steel autoclave, and oxygen gas is passed through into reaction kettle to be discharged
Remaining air, ventilate 2min when controlling oxygen partial pressure 0.4MPa, and then heating increases temperature to 200 DEG C, controls oxygen partial pressure
2.0h is reacted for 0.8MPa to realize solid-liquor separation when reaction completes cooling reduction temperature to 75 DEG C using vacuum filtration mode, add
Arsenic content is reduced to 2.4% after pressure oxidation water logging slag drying, and the removal efficiency of arsenic reaches 91.32%.
Compound concentration is the potassium hydroxide solution of 2.0mol/L, by liquid-solid ratio（Liquor capacity L and pressure oxidation water logging slag
Measure the ratio between kg）5/1 is added pressure oxidation water logging slag, which is added in autoclave, control oxygen partial pressure 0.1MPa
Shi Tongqi 1min, then heating increase temperature to 108 DEG C, and control oxygen partial pressure is that 0.9MPa reacts 2h, and cooling drop is completed in reaction
When low temperature is to 90 DEG C, solid-liquor separation, pressurised oxygen choline phase analysis Returning smelting, the leaching rate of antimony are realized using vacuum filtration mode
Reach 91.8%；Pressurised oxygen choline immersion liquid keeps 90 DEG C of temperature, and solid potassium sulfide purification removing lead is then added, vulcanizes potassium application rate
It is 1.0 times of theoretical amount, while the activated carbon that phase homogenous quantities and granularity are 5.0~10.0mm is added, is used after reacting 1.0h
Vacuum filtration mode is separated by solid-liquid separation, and purification slag recycles lead.
Liquid is added in stainless steel autoclave after purification, and sodium hydroxide, sodium hydroxide concentration are added into reaction kettle
It it is 0.98 times of theoretical amount, it is that 0.1MPa reacts 2h to keep 100 DEG C of slurry temperature, control oxygen partial pressure, and cooling drop is completed in reaction
When low temperature is to 90 DEG C, using vacuum filtration mode realization solid-liquor separation, liquid returns to pressurised oxygen choline leaching process, precipitation after precipitation
The hot water that object temperature is 85 DEG C presses liquid-solid ratio（The ratio between water volume L and sediment quality kg）3/1 washing, finally in 95 DEG C of temperature
Lower drying obtains sodium pyroantimonate.
Chemical composition, microscopic appearance and the crystal habit of sodium pyroantimonate product are shown in Table 1, Fig. 2 and Fig. 3 respectively.It can be with from table 1
Find out, requirement of the content of trivalent antimony well below HG/T3254-2001 standards in the cubic sodium pyroantimonate product.Fig. 2
Show that the product is that overall distribution is uniform, single is cube but agglomeration is serious.Fig. 3 shows the NaSb that it is well-crystallized
(OH)6Crystal.
The chemical composition of 1 cubic sodium pyroantimonate product of table
| Ingredient | Total antimony is (with Sb2O3Meter) | Na2O | Sb3+ | Fe2O3 | As2O3 |
| Content/% | 59.00 | 12.48 | ≤0.01 | 0.001 | 0.0001 |
Claims (1)
1. a kind of method that potassium salt system pressure oxidation prepares sodium pyroantimonate, it is characterised in that include the following steps：
（1）Pressure oxidation water logging
Then mixed slurry is added to by antimony cigarette ash by the liquid-solid ratio 2~6/1 plus water slurry of water volume L and antimony cigarette ash quality kg
In stainless steel autoclave, oxygen is passed through into reaction kettle so that remaining air, 0.2~0.5MPa of control oxygen partial pressure is discharged
1~5min of Shi Tongqi, then heating increase temperature to 150~225 DEG C, control oxygen partial pressure be 0.5~1.0MPa reaction 1~
5h realizes solid-liquor separation, pressure oxidation water logging when reaction completes cooling reduction temperature to 60~80 DEG C using vacuum filtration mode
Liquid send pressurised oxygen choline to soak process for curing arsenic, pressure oxidation water logging slag；
（2）Pressurised oxygen choline soaks
Compound concentration is the potassium hydroxide solution of 1.5~2.5mol/L, by liquor capacity L's and pressure oxidation water logging slag amount kg
Pressure oxidation water logging slag is added in liquid-solid ratio 3~10/1, which is added in autoclave, oxygen is passed through into reaction kettle
With the remaining air of discharge, ventilate 1~5min when controlling 0.2~0.5MPa of oxygen partial pressure, then heating increase temperature to 100~
109 DEG C, control oxygen partial pressure is that 0.5~1.0MPa, 1~5h of reaction are adopted when reaction completion is cooling to reduce temperature to 85~95 DEG C
Realize that solid-liquor separation, pressurised oxygen choline phase analysis Returning smelting, pressurised oxygen choline immersion liquid send cleaning procedure with vacuum filtration mode；
（3）Purification
Pressurised oxygen choline immersion liquid keeps 80~95 DEG C of temperature, and solid potassium sulfide purification removing lead is then added, and vulcanization potassium application rate is
1.0~1.1 times of theoretical amount, while the activated carbon that phase homogenous quantities and granularity are 5.0~10.0mm is added, reaction 0.5~
It is separated by solid-liquid separation using vacuum filtration mode after 2.0h, purification slag recycles lead, and liquid send pressurized precipitation process after purification；
（4）Pressurized precipitation
Liquid is added in stainless steel autoclave after purification, and sodium hydroxide is added into reaction kettle, and sodium hydroxide concentration is reason
0.9~1.0 times of stoichiometric, it is that 0.1~0.3MPa reacts 1~5h to keep 95~105 DEG C of slurry temperature, control oxygen partial pressure, instead
When should complete cooling reduction temperature to 85~95 DEG C, using vacuum filtration mode realization solid-liquor separation, liquid returns to pressurization after precipitation
Alkali oxide soak process, sediment with temperature be 80-90 DEG C hot water by water volume L and sediment quality kg liquid-solid ratio 2~5/1
Washing, finally drying obtains sodium pyroantimonate at 80~100 DEG C of temperature.
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| CN108455670A (en) * | 2018-03-08 | 2018-08-28 | 中南大学 | A kind of method that potassium hydroxide system prepares pyroantimonic acid lithium |
| CN108394933A (en) * | 2018-03-08 | 2018-08-14 | 中南大学 | A kind of method that potassium hydroxide system prepares hexafluoro-antimonic acid lithium |
| CN114574716B (en) * | 2022-02-28 | 2023-03-24 | 中南大学 | Method for removing arsenic from antimony-containing high-arsenic soot and recovering valuable antimony |
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| CN1194237A (en) * | 1997-03-24 | 1998-09-30 | 张至德 | Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore |
| CN101693553A (en) * | 2009-10-19 | 2010-04-14 | 株洲安特锑业化工有限公司 | Production process for preparing ultra-white nanometer sodium pyroantimonate |
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| CN1194237A (en) * | 1997-03-24 | 1998-09-30 | 张至德 | Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore |
| CN101693553A (en) * | 2009-10-19 | 2010-04-14 | 株洲安特锑业化工有限公司 | Production process for preparing ultra-white nanometer sodium pyroantimonate |
| CN105886769A (en) * | 2015-01-26 | 2016-08-24 | 昆明冶金高等专科学校 | Method for enriching precious metal by dissolving multi-metal alloy material through nitric acid |
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