CN102031381B - Process for preparing sodium pyroantimonate from arsenic- and stibium-containing smoke ash - Google Patents
Process for preparing sodium pyroantimonate from arsenic- and stibium-containing smoke ash Download PDFInfo
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- CN102031381B CN102031381B CN2010105742067A CN201010574206A CN102031381B CN 102031381 B CN102031381 B CN 102031381B CN 2010105742067 A CN2010105742067 A CN 2010105742067A CN 201010574206 A CN201010574206 A CN 201010574206A CN 102031381 B CN102031381 B CN 102031381B
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Abstract
The invention discloses a process for preparing sodium pyroantimonate from arsenic- and stibium-containing smoke ash and belongs to the field of wet-process metallurgy. The production process for preparing the sodium pyroantimonate is characterized by comprising the following steps of: using NaOH and Na2CO3 or mixing the NaOH and Na2CO3, and performing wet-process pretreatment to remove arsenic; precipitating arsenic in arsenic-containing leaching liquor by using Na2S to obtain an arsenic sulfide byproduct; leaching arsenic- and stibium-containing leaching residues by mixing the Na2S and NaOH, returning lead residue, smelting, and recovering lead, silver and other valuable metals; blowing oxygen-rich compressed air into stibium-containing leaching liquor to prepare a sodium pyroantimonateproduct; and concentrating and crystallizing oxidized liquor to prepare Na2S2O3. The process has the advantages of no environmental pollution, simple equipment, low investment, high comprehensive utilization rate, low cost, suitability for industrial production, and the like.
Description
Technical field
The present invention relates to a kind of usefulness and contain the technique that arsenic antimony cigarette ash prepares sodium pyroantimoniate, belong to the hydrometallurgy field.
Technical background
At present, the rare precious metal products such as China's most of precious metal smelting silver that enterprise produces, bismuth, very major part reclaims from copper, lead anode slurry.My company produces a large amount of arsenic antimony cigarette ashes that contain, and contains the valuable metals such as a certain amount of lead, silver when reclaiming silver from lead anode slurry in the process of bessemerizing.Wherein, contain Sb:30%～40%, As:5%～10%, Pb:20%～25%, Ag:1%～2%; As, Sb mainly exist with oxide morphology.If can not effectively be used, not only affect production efficiency, and easily environment has been caused secondary pollution, the valuable metal utilization ratio is low, has affected the economic benefit of company.It is a great problem that nonferrous smelting producer faces that the processing that contains arsenic antimony cigarette ash that the silver converter produces is reclaimed, and now domestic report seldom and fails to accomplish to separate more thoroughly and comprehensive recovery.About containing the wet-leaching technique of arsenic antimony cigarette ash, relevant report is also not yet arranged at present in related documents.
Summary of the invention
Technical problem to be solved by this invention is: develop a kind of usefulness and contain the technique that arsenic antimony cigarette ash prepares sodium pyroantimoniate, by cigarette ash is processed, As and Sb in the Separation and Recovery cigarette ash, the comprehensive valuable element that reclaims, and the sodium pyroantimoniate product of preparation high added value, reduce the soot amount of Returning smelting, the economical efficiency so that height is produced solves the secondary pollution to environment.
Technical scheme of the present invention is: a kind of usefulness contains the technique that arsenic antimony cigarette ash prepares sodium pyroantimoniate, is finished by following technological process.
A, pre-treatment dearsenification:
To contain arsenic antimony cigarette ash and NaOH solution and Na
2CO
3Solution is stirring heating in reactor together, reacts after 0.5～4 hour, filters; Processing condition are: solid-to-liquid ratio 1: 3～8; 80～100 ℃ of temperature; NaOH concentration 40～120g/L; Na
2CO
3Concentration 10～40g/L;
B, heavy arsenic:
The filtrate stirring of A step is added Na
2S sinks arsenic, filters to get the red arsenic product, and filtrate is returned pretreatment process; Heavy arsenic processing condition are: 50～80 ℃ of temperature, and 0.5～2 hour time, the sodium sulphite add-on is 1～2 times that solution contains the arsenic quality;
C, Sodium Sulphide soak:
The crystalline mother solution that A step gained filter residue is added water or uses the back operation to return is sized mixing, and uses Na
2S, NaOH mixing solutions leach, and are incubated after 2～5 hours and filter; Processing condition are: solid-to-liquid ratio 1: 4～10; 80～100 ℃ of temperature; PH value 10～11; Na
2S concentration 80～150g/L; NaOH concentration 10～50g/L;
D, send smelting system with the leached mud of C step, further reclaim lead, silver-colored valuable element with common process;
E, oxidation:
C step leach liquor is passed into the oxygen enrichment compressed air oxidation 0.5～5 hour, produce crystallization; Oxygen containing concentration of volume percent is 30%～60% in the oxygen enrichment pressurized air; The compressed-air actuated pressure 0.4～0.6Mp of oxygen enrichment; 60～80 ℃ of temperature of reaction; Filtration makes solid-liquid separation, with crystallizing and washing, drying and obtain the sodium pyroantimoniate product;
F, condensing crystal:
With liquid condensing crystal behind the E stage oxidation, obtain purer Sulfothiorine product, crystalline mother solution returns C step Sodium Sulphide and soaks operation and do adjusting slurry and use.
Technical thought of the present invention is: the present invention is handled to be contained in the arsenic antimony cigarette ash, and arsenic, antimony major part exist with trivalent, and plumbous major part exists with the plumbous oxide form.Take full advantage of the difference of the chemical property of three's oxide compound, accomplish to separate to greatest extent the three, realize the efficient recovery of valuable element.The pretreatment stage alkaline purification utilizes white arsenic more to be soluble in the characteristic of alkaline solution than antimonous oxide, plumbous oxide, realizes preliminary dearsenification.If arsenic containing solution is directly made sodium arseniate, then energy consumption is high; If be prepared into Tricalcium arsenate, then uneconomical; The present invention utilizes antimonous oxide to be soluble in the character of sodium sulfide solution, soaks separation of lead antimony with Sodium Sulphide.Leach liquor control processing condition prepare the sodium pyroantimoniate product with oxygen enrichment pressurized air.Oxidated solution crystalline Sulfothiorine.By the enforcement of this invented technology, control suitable processing condition, can more thorough separation of lead, arsenic, antimony valuable element, realize effectively comprehensive the recovery, obtain good economic benefit.
Relevant reaction in the invention is as follows:
The pre-treatment dearsenification:
As
2O
3+6NaOH＝2Na
3AsO
3+3H
2O
Heavy arsenic:
2Na
3AsO
3+5Na
2S+8H
2O+O
2＝As
2S
5↓+16NaOH
Sodium Sulphide soaks:
As
2O
3+6Na
2S+3H
2O＝2Na
3AsS
3+6NaOH
PbO+Na
2S+H
2O＝PbS+2NaOH
Sb
2O
3+6Na
2S+3H
2O＝2Na
2SbS
3+6NaOH
Oxidation:
2Na
3SbS
3+7O
2+2NaOH+5H
2O＝2NaSbO
3·3H
2O↓+3Na
2S
2O
3
In the process implementing process of the present invention, by the control processing condition, during the pre-treatment dearsenification, arsenic decreasing ratio＞95%, and plumbous, antimony leaching yield＜10%.When Sodium Sulphide soaks, by the control pH, can make the Sulfothiorine product of follow-up condensing crystal preparation very pure.
The enforcement of this invented technology, output the byproducts such as sodium pyroantimoniate, red arsenic, Sulfothiorine, realized the effective separation of each valuable element.Whole process does not have waste water, waste gas to efflux, and does not produce solid waste yet and need to stack processing, has solved well this and has contained the processing problem of arsenic converter cigarette ash.In addition, this processing unit requires simply, investment is low, be easy to realize industrialization.
Description of drawings
Fig. 1: process flow sheet of the present invention
Embodiment
Embodiment 1:
Get cigarette ash 200g, contain As:9.4%, Sb:33.8%, Pb:22.3%.During the pre-treatment dearsenification, pressed solid-to-liquid ratio 1: 5, NaOH concentration 80g/L, Na
2CO
3Concentration 20g/L, 85～90 ℃ of temperature, 2 hours reaction times control reaction conditions.Reach As leaching yield 95.42%, Pb leaching yield 6.36%, the treatment effect of Sb leaching yield 4.87%.During the heavy arsenic of leach liquor sodium sulphite, temperature is 70 ℃, and the sodium sulphite dosage is 1.5 times that solution contains the arsenic quality, the deposition rate 89.73% of arsenic, and red arsenic contain As:51.82%.When Sodium Sulphide soaks the pre-treatment leached mud, solid-to-liquid ratio 1: 8, Na
2S concentration 120g/L, NaOH concentration 20g/L, 95 ℃ of temperature, 3 hours reaction times.The antimony leaching yield is 95.37%, lead enters slag rate 99.65%.When passing into the oxygen-rich air oxidation, oxygen concentration of volume percent 43%, pressure 0.4Mp, oxidization time 3 hours, filtration, washing, the dry sodium pyroantimoniate product that gets, the antimony percent crystallization in massecuite reaches 99.53%, contains Sb
2O
5: 64.90%, Na
2O:12.84%, As:0.0037%, Pb:0.0009%, Fe:0.0042%, Cu:0.0009%, Sulfothiorine percent crystallization in massecuite 91%, Na
2S
2O
3% 〉=93%.
Embodiment 2:
The cigarette ash 200g of present embodiment contains As:6.08%, Sb:35.46%, Pb:21.39%.During the pre-treatment dearsenification, by solid-to-liquid ratio 1: 4, NaOH concentration 100g/L, Na
2CO
3Concentration 10g/L, 90～95 ℃ of temperature, 4 hours reaction times control reaction conditions.Reach the treatment effect of As leaching yield 98.35%, Pb leaching yield 7.12%, Sb leaching yield 5.25%.During the heavy arsenic of leach liquor sodium sulphite, temperature is 60 ℃, and the sodium sulphite dosage is 2 times that solution contains the arsenic quality, the deposition rate 93.74% of arsenic, and red arsenic contain As:48.68%.When Sodium Sulphide soaks the pre-treatment leached mud, solid-to-liquid ratio 1: 10, Na2S concentration 110g/L, NaOH concentration 10g/L, 90 ℃ of temperature, 4 hours reaction times.The antimony leaching yield is 96.18%, lead enters slag rate 99.43%.When passing into the oxygen-rich air oxidation, oxygen concentration of volume percent 52%, pressure 0.4Mp, oxidization time 2 hours, filtration, washing, the dry sodium pyroantimoniate product that gets, the antimony percent crystallization in massecuite reaches 99.52%, contains Sb
2O
5: 64.85%; Na
2O:12.87%; As:0.0040%; Pb:0.0010%; Fe:0.0045%; Cu:0.0010%.Sulfothiorine percent crystallization in massecuite 90%, Na
2S
2O
3% 〉=95%.
Embodiment 3:
Get cigarette ash 200g, contain As:9%, Sb:35.2%, Pb:21.2%.During the pre-treatment dearsenification, pressed solid-to-liquid ratio 1: 3; NaOH concentration 40g/L, Na
2CO
3Concentration 40g/L, 80～90 ℃ of temperature, 0.5 hour reaction times control reaction conditions.Reach the treatment effect of As leaching yield 95.42%, Pb leaching yield 6.36%, Sb leaching yield 4.87%.During the heavy arsenic of leach liquor sodium sulphite, temperature is 50 ℃, and the sodium sulphite dosage is 1 times that solution contains the arsenic quality, the deposition rate 89.73% of arsenic, and red arsenic contain As:51.82%.When Sodium Sulphide soaks the pre-treatment leached mud, solid-to-liquid ratio 1: 4, Na
2S concentration 80g/L, NaOH concentration 50g/L, 80 ℃ of temperature, 2 hours reaction times.The antimony leaching yield is 95.37%, lead enters slag rate 99.65%.When passing into the oxygen-rich air oxidation, oxygen concentration of volume percent 30%, pressure 0.6Mp, oxidization time 0.5 hour, filtration, washing, the dry sodium pyroantimoniate product that gets, the antimony percent crystallization in massecuite reaches 99.53%, contains Sb
2O
5: 64.90%, Na
2O:12.84%, As:0.0037%, Pb:0.0010%, Fe:0.0057%, Cu:0.0008%, Sulfothiorine percent crystallization in massecuite 90%, Na
2S
2O
3% 〉=92%.
Embodiment 4:
Get cigarette ash 250g, contain As:10.1%, Sb:30%, Pb:24.6%.During the pre-treatment dearsenification, pressed solid-to-liquid ratio 1: 8; NaOH concentration 120g/L; Na
2CO
3Concentration 40g/L, 85～100 ℃ of temperature, 2 hours reaction times control reaction conditions.Reach the treatment effect of As leaching yield 95.8%, Pb leaching yield 6.56%, Sb leaching yield 4.77%.During the heavy arsenic of leach liquor sodium sulphite, temperature is 80 ℃, and the sodium sulphite dosage is 1.5 times that solution contains the arsenic quality, the deposition rate 89.73% of arsenic, and red arsenic contain As:51.82%.When Sodium Sulphide soaks the pre-treatment leached mud, solid-to-liquid ratio 1: 4, Na
2S concentration 150g/L, NaOH concentration 50g/L, 100 ℃ of temperature, 5 hours reaction times.The antimony leaching yield is 94.55%, lead enters slag rate 98.74%.When passing into the oxygen-rich air oxidation, oxygen concentration of volume percent 60%, pressure 0.6Mp, oxidization time 5 hours, filtration, washing, the dry sodium pyroantimoniate product that gets, the antimony percent crystallization in massecuite reaches 99.60%, contains Sb
2O
5: 68.11%, Na
2O:11.95%, As:0.00267%, Pb:0.0008%, Fe:0.0033%, Gu:0.00028%, Sulfothiorine percent crystallization in massecuite 94%, Na
2S
2O
3% 〉=93%.
Claims (1)
1. one kind with the technique that contains arsenic antimony cigarette ash and prepare sodium pyroantimoniate, it is characterized in that being finished by following technological process:
A, pre-treatment dearsenification:
To contain arsenic antimony cigarette ash and NaOH solution and Na
2CO
3Solution is stirring heating in reactor together, reacts after 0.5～4 hour, filters; Processing condition are: solid-to-liquid ratio 1: 3～8; 80～100 ℃ of temperature; NaOH concentration 40～120g/L; Na
2CO
3Concentration 10～40g/L;
B, heavy arsenic:
The filtrate stirring of A step is added Na
2S sinks arsenic, filters to get the red arsenic product, and filtrate is returned pretreatment process; Heavy arsenic processing condition are: 50～80 ℃ of temperature, and 0.5～2 hour time, the sodium sulphite add-on is 1～2 times that solution contains the arsenic quality;
C, Sodium Sulphide soak:
The crystalline mother solution that A step gained filter residue is added water or uses the back operation to return is sized mixing, and uses Na
2S, NaOH mixing solutions leach, and are incubated after 2～5 hours and filter; Processing condition are: solid-to-liquid ratio 1: 4～10; 80～100 ℃ of temperature; PH value 10～11; Na
2S concentration 80～150g/L; NaOH concentration 10～50g/L;
D, send smelting system with the leached mud of C step, further reclaim lead, silver-colored valuable element with common process;
E, oxidation:
C step leach liquor is passed into the oxygen enrichment compressed air oxidation 0.5～5 hour, produce crystallization; Oxygen containing concentration of volume percent is 30%～60% in the oxygen enrichment pressurized air; The compressed-air actuated pressure 0.4～0.6Mp of oxygen enrichment; 60～80 ℃ of temperature of reaction; Filtration makes solid-liquid separation, with crystallizing and washing, drying and obtain the sodium pyroantimoniate product;
F, condensing crystal:
With liquid condensing crystal behind the E stage oxidation, obtain purer Sulfothiorine product, crystalline mother solution returns C step Sodium Sulphide and soaks operation and do adjusting slurry and use.
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| CN2010105742067A CN102031381B (en) | 2010-11-28 | 2010-11-28 | Process for preparing sodium pyroantimonate from arsenic- and stibium-containing smoke ash |
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| CN102031381B true CN102031381B (en) | 2013-04-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103290221A (en) * | 2012-02-28 | 2013-09-11 | 兰州理工大学 | Method for recovering copper, arsenium and antimony from black copper sludge |
| CN103849782B (en) * | 2012-11-28 | 2014-12-10 | 湖南宇腾有色金属股份有限公司 | High-pressure alkaline leaching arsenic-removal method for high-arsenic antimony white powder |
| CN103318959A (en) * | 2013-07-15 | 2013-09-25 | 郴州市金贵银业股份有限公司 | Production method for sodium pyroantimonate by using high-temperature high-pressure pure-oxygen oxidation |
| CN104911364B (en) * | 2015-06-26 | 2017-11-10 | 郴州市金贵银业股份有限公司 | A kind of method of antimony arsenic smoke dust green high-efficient production stibium trioxide |
| CN105063361B (en) * | 2015-08-20 | 2017-03-22 | 江西铜业股份有限公司 | Method for comprehensively recovering valuable metal from copper anode slime |
| CN106180138B (en) * | 2016-07-15 | 2018-12-11 | 深圳市深投环保科技有限公司 | A kind of processing method of arsenic-containing waste |
| CN107354301B (en) * | 2017-07-19 | 2019-01-25 | 中南大学 | A method of improving arsenic-containing material arsenic-removing rate |
| CN107523702B (en) * | 2017-08-23 | 2019-03-19 | 中南大学 | A kind of method that the pressure oxidation of sodium salt system prepares sodium pyroantimonate |
| CN107858521A (en) * | 2017-12-07 | 2018-03-30 | 郴州市金贵银业股份有限公司 | The method that cigarette ash containing antimony prepares sodium pyroantimonate |
| CN109182765A (en) * | 2018-10-18 | 2019-01-11 | 郴州市金贵银业股份有限公司 | A method of star metal is prepared with antimony cigarette ash |
| CN111118301B (en) * | 2019-12-31 | 2020-11-27 | 焱鑫环保科技有限公司 | Method for recycling arsenic slag resources by arsenic and alkali in freezing separation alkali slag water leaching solution |
| CN112375915A (en) * | 2020-10-27 | 2021-02-19 | 西北矿冶研究院 | Method for removing harmful elements arsenic and antimony in high-content bismuth-silver smelting slag |
| CN113371757B (en) * | 2021-07-09 | 2022-11-08 | 中南大学 | Method for preparing sodium pyroantimonate and regenerating and recycling mother liquor |
| CN114561558B (en) * | 2022-02-23 | 2023-08-29 | 中南大学 | Method for recycling antimony and fixing arsenic from arsenic-containing crystal |
| CN116692941A (en) * | 2023-07-06 | 2023-09-05 | 中南大学 | Method for preparing high-quality sodium pyroantimonate through gradient purification and oxidation |
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