CN101786659A - Method for recovering arsenic sulfide from arsenic-containing waste residue - Google Patents
Method for recovering arsenic sulfide from arsenic-containing waste residue Download PDFInfo
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Abstract
The invention discloses a method for recovering arsenic sulfide from arsenic-containing waste residue, which comprises the following steps: taking arsenic sulfide residue with the arsenic content of 7.1-16.8%, stirring and mixing with water, wherein the water content is calculated by 100-150mL/100g residue; evenly mixing, and gradually adding alkali at the temperature of room temperature-60 DEG C for carrying out leaching treatment, wherein the alkali content is calculated by 2.0-3.5g/g arsenic sulfide; further continuously maintaining the leaching process for 40-120 min after completing the addition of the alkali, and filtering; using water which is calculated by 50mL/100g arsenic sulfide residue for washing the residue step by step, merging filtrate and washing solution, using sulfuric acid with the concentration of 93-98% for neutralization, controlling the pH to be 9-11, filtering, further using the sulfuric acid with the concentration of 93-98% for neutralization till the pH is 1-3.5, adding sodium sulfide for leading the pH to be 2-4, then filtering, carrying out 2-3 times of repulping washing and filtering washing on sediment, obtaining secondary sediment, and drying for obtaining an arsenic sulfide finished product. The method can reduce the reaction temperature, shorten the leaching time and improve the recovery rate of arsenic.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to the method for handling the arsenic-containing waste residue that the eliminating arsenic by fluosilicic acid process obtains.
Background technology
The eliminating arsenic by fluosilicic acid process obtains a kind of arsenic-containing waste residue after filtering, and its arsenic content is at 2～16%.Because this slag belongs to dangerous solid waste, must carry out particular processing, just can store up.Usually adopt and seal the curing technology processing, make pulpous state Tricalcium arsenate and environment isolated, prevent to produce secondary pollution.This processing mode not only increases business burden, and causes the significant wastage of resource.Along with development of science and technology, the market requirement of arsenic constantly increases, and the processing of arsenic-containing waste is handled from " Gu arsenic " and changed the recycling processing gradually into.
The method of handling arsenic-containing waste residue at present can be divided into two kinds: a kind of is pyrogenic process, promptly handles with oxidizing roasting, reducing roasting and vacuum baking etc., and arsenic directly reclaims with the white arsenic form; Another kind is a wet method, promptly adopts acidleach, alkali to soak or salt soaks etc. and to handle, and earlier arsenic is separated from slag, and then is further reclaimed the arsenic product or carry out harmless treatment.
The white arsenic of pyrogenic attack drying regime, thereby be difficult to guarantee the good working environment.This method carries that the arsenic cost is lower, and treatment capacity is big, if but bad second environmental pollution and the safety problem of very easily causing of production process control.
Wet method does not produce dust, can satisfy environmental requirement, has less energy-consumption, less contamination, efficient advantages of higher, but flow process is comparatively complicated, and processing cost is higher relatively.
Chinese patent publication number CN1079004 on December 01st, 1993 disclose a kind of " removing and reclaim the technology of orpiment in the difficult metallurgical ore deposit of self-contained arsenic " with the ore deposit levigate after, ammoniacal liquor furnishing pulp solids concentration with 3～8% (weight) is 20～50% (weight), dissolves 1～2h under 10～80 ℃ in encloses container.When being one section dissolving, As
2S
3Dissolution rate be～78%; It is two periods whens dissolving about 91%; When being the dissolving of three sections adverse currents about 100%.Contain As with vapor distillation
2S
3Ammonia solution, distill out ammonia and recycle, the raffinate sulfuric acid acidation makes its pH＜4, obtains the higher As of purity
2S
3Precipitation.
It is 20～30% (weight) with the ammoniacal liquor furnishing pulp solids concentration of levigate mining 3～8% (weight) to 80～95%＜44 μ m that Chinese patent publication number CN1103669 discloses a kind of " reclaiming the method for gold and silver and orpiment in the metallurgical ore deposit of arsenical difficulty " June 14 nineteen ninety-five, add 0.1% sodium lignosulfonate and SULPHUR POWDER of mineral aggregate weight, after in encloses container, stirring 2～6h under 80～100 ℃, obtain containing As
2S
3Ammonia solution and the slag after the dearsenification, handle by patent CN92103508 again and obtain As
2S
3Waste water adopts the lime causticization arsenic removal.
Two above-mentioned patents, the temperature of reaction height that process adopts, leaching time is long, needs just can reach higher arsenic-removing rate, the process complexity with the multistage counter current leaching.
Summary of the invention
The objective of the invention is to overcome above-mentioned shortcoming and provide a kind of and can reduce temperature of reaction, shorten leaching time, improve the method that from arsenic-containing waste residue, reclaims red arsenic of the rate of recovery of arsenic.
A kind of method that reclaims red arsenic from arsenic-containing waste residue of the present invention comprises:
Get arsenic content and be 7.1～16.8% arsenic sulfide slag and water and mix, wherein the water yield is by 100～150mL/100g slag; After mixing, ℃ progressively add alkali in room temperature～60 and leach processing, wherein alkali number is by 2.0～3.5g/g red arsenic; Continue to keep leaching process 40～120min and filtration again after waiting to add alkali; And use by the moisture step of 50mL/100g arsenic sulfide slag and wash residue, merging filtrate and washings are also used the neutralization of concentration 93～98% sulfuric acid, control pH is 9～11, filter, it is 1～3.5 that filtrate continues to be neutralized to pH with concentration 93～98% sulfuric acid again, and it is 2～4 that interpolation sodium sulphite makes pH, filter then, precipitation is washed and starched through 2～3 times again and is washed and filtration washing, obtains secondary sedimentation, and drying obtains the red arsenic finished product.Above-mentioned a kind of method that reclaims red arsenic from arsenic-containing waste residue, wherein: the alkali that is used to dissolve leaching is one of yellow soda ash, sodium hydroxide or sodium sulphite or their mixture.
Above-mentioned a kind of method that reclaims red arsenic from arsenic-containing waste residue, wherein: the alkali that is used to dissolve leaching is sodium hydroxide.
Above-mentioned a kind of method that reclaims red arsenic from arsenic-containing waste residue, wherein: the pH of the arsenic containing solution that the alkali leaching obtains is more preferably greater than 10.
Because arsenic sulfide slag mainly is an arsenic trisulfide.As
2S
3Can think the acid anhydrides of thioarsenous acid, be insoluble in water (solubleness 5.17 * 10 18 ℃ the time
-5), also be insoluble to mineral acid; Be dissolved in ethanol and alkaline solution; Be soluble in alkali metal hydroxide, carbonate, the sulfide, therefore, available yellow soda ash, sodium bicarbonate, sodium hydroxide, ammonia, sodium sulphite or other alkali dissolution red arsenic.Therefore the present invention adopts with the alkaline purification arsenic-containing waste residue, should add enough alkali numbers, makes pH be higher than 11, so that better dissolve red arsenic, improves the red arsenic leaching rate; Separating the first-time filtrate that obtains behind the residue, be used for further handling and reclaim red arsenic.First-time filtrate to pH7～8, deposits primary sedimentation with acid treatment.The filtering separation primary sedimentation obtains secondary filtrate, continues to make pH be lower than 4.5 with the acid neutralization again, deposits the red arsenic secondary sedimentation.Filtering separation obtains that secondary sedimentation is washed through washing and starching again, drying obtains arsenic content at the red arsenic finished product more than 50%.Three filtrates of separated secondary post precipitation are used for the arsenic sulfide slag leaching process after treatment and regulate the leaching liquid-solid ratio.
Any acid all can be used for neutralization.From considering economically, preferentially adopt strong solution, because reach needed pH, the acid amount that needs is less.
Acidity is very strong although the arsenic-containing waste residue that the eliminating arsenic by fluosilicic acid process produces is owing to contain silicofluoric acid, the washing of this arsenic-containing waste residue is unwanted before processing, because, sodium ion by leaching agent, sedimentation silicofluoric acid more completely, thereby can reduce the fluorine content in the red arsenic precipitation greatly, and can improve the strainability of slag.Present method can reduce temperature of reaction, shortens leaching time, improves the rate of recovery of arsenic.The higher red arsenic of the dna purity of high extraction from arsenic sulfide slag, this not only provides the suitable red arsenic product that utilizes again, and has solved the resource utilization problem of waste residue, greatly reduces and stores up refuse danger, for the utilization again of waste residue is laid a good foundation.
Embodiment
Embodiment 1
After getting arsenic content and be 16.8% arsenic sulfide slag 800g and adding 1200mL water and stir, at room temperature progressively add 288g sodium hydroxide and leach processing.Continue to keep leaching process 1h and filtration again after waiting to add alkali, to wash residue with the 400mL moisture step.Level of residue is 713.9g, and its arsenic content is 0.09%.The leaching rate of arsenic is 95%.Merging filtrate and washings 1657g control pH 10～12 with the neutralization of concentration 93～98% sulfuric acid, filter and obtain primary sedimentation 255g, and its water content is 70.1%, arsenic content 1.01% (butt); Filtrate continues to be neutralized to pH 2～3 with concentration 93～98% sulfuric acid again, add sodium sulphite 30g, pH rises to 3～4, filter then, precipitation is washed and starched through secondary again and is washed and filtration washing, obtains secondary sedimentation 593g, and its water content is 58.8%, drying obtains the red arsenic finished product, and its arsenic content is 50.5% (butt).Filtrate arsenic content is 0.01g/L.The arsenic rate of recovery is 91.3%.
Embodiment 2
After getting arsenic content and be 16.8% arsenic sulfide slag 100g and adding 100mL water and stir, earlier with in the 8.5g yellow soda ash and after, add 25g sodium hydroxide again and further leach.Leaching 2h after-filtration, and with 50mL water washing residue.Residue arsenic content is 0.1%.Merging filtrate and washings are neutralized to pH 11 separate part post precipitation filtrates with concentration 93～98% sulfuric acid to continue to be neutralized to pH are 2～3, leave standstill 1h after-filtration, washing, drying and obtain precipitation, and its arsenic content is 49.6%.The arsenic rate of recovery is 90.3%.
Embodiment 3
After getting arsenic content and be 7.1% arsenic sulfide slag 800g and adding 1000mL water and stir, add the 200g sodium hydroxide down at 40 ℃ and leach processing,, and wash and starch again with the 400mL water distribution and to wash residue through the 40min after-filtration.Obtaining first-time filtrate 1495g neutralizes with 50mL concentration 93～98% sulfuric acid.Deposit the 1h after-filtration, obtain pH and be 10 secondary filtrate 1470g and water content and be 61.2% primary sedimentation 174g.It is 2.5 that the continuation of secondary filtrate is neutralized to pH with concentration 93～98% sulfuric acid, leaves standstill the 1h after-filtration, and the secondary sedimentation 100g that wash through washing and starching again, drying obtains, its arsenic content are 51.5% (butt).The arsenic rate of recovery is 90.5%.
Embodiment 4
Get arsenic content and be 8.8% arsenic sulfide slag 600g in the 1500mL beaker, add the 400mL washing water and carry out pulp, under agitation progressively add sodium hydroxide 244g then, and after keeping 30min under 30～60 ℃, carry out vacuum filtration; The slag that filtration obtains is washed and starched with 250mL water again, refilters, and obtains water content and be 38.3% slag 438g, and its arsenic content is 0.18%.Also with the neutralization of 93～98% sulfuric acid, pH is 9～12 in control, filters and obtains primary sedimentation 295g for merging filtrate and washings, and its water content is 74.4%, arsenic content 1.4% (butt); Filtrate continues to be neutralized to pH 1～3.5 with concentration 93～98% sulfuric acid again, add sodium sulphite 42g, pH rises to 2～4, filter then, precipitate to wash and starch for three times again and wash and filtration washing, obtain secondary sedimentation 258g, its water content is 61.8%, drying obtains the red arsenic finished product, and its arsenic content is 52.6% (butt).Filtrate arsenic content is 0.01g/L.The arsenic rate of recovery is 90.2%.
Claims (4)
1. method that reclaims red arsenic from arsenic-containing waste residue comprises:
Get arsenic content and be 7.1～16.8% arsenic sulfide slag and water and mix, wherein the water yield is by 100～150mL/100g slag; After mixing, ℃ progressively add alkali in room temperature～60 and leach processing, wherein alkali number is by 2.0～3.5g/g red arsenic; Continue to keep leaching process 40～120min and filtration again after waiting to add alkali; And use by the moisture step of 50mL/100g arsenic sulfide slag and wash residue, merging filtrate and washings are also used the neutralization of concentration 93～98% sulfuric acid, control pH is 9～11, filter, it is 1～3.5 that filtrate continues to be neutralized to pH with concentration 93～98% sulfuric acid again, and it is 2～4 that interpolation sodium sulphite makes pH, filter then, precipitation is washed and starched through 2～3 times again and is washed and filtration washing, obtains secondary sedimentation, and drying obtains the red arsenic finished product.
2. a kind of method that reclaims red arsenic from arsenic-containing waste residue as claimed in claim 1, wherein: the alkali that is used to dissolve leaching is one of yellow soda ash, sodium hydroxide or sodium sulphite or their mixture.
3. a kind of method that reclaims red arsenic from arsenic-containing waste residue as claimed in claim 2, wherein: the alkali that is used to dissolve leaching is sodium hydroxide.
4. a kind of method that reclaims red arsenic from arsenic-containing waste residue as claimed in claim 1 or 2, wherein: the pH of the arsenic containing solution that the alkali leaching obtains is 10～11.
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| CN101954370A (en) * | 2010-09-06 | 2011-01-26 | 同济大学 | Method for recycling arsenic-containing waste residues |
| CN102115162A (en) * | 2010-12-31 | 2011-07-06 | 马艳荣 | Method for preparing arsenic trioxide by using arsenic sulfide waste slags |
| CN102115165A (en) * | 2010-12-31 | 2011-07-06 | 马艳荣 | Method for preparing arsenic trioxide by arsenic-containing waste water |
| CN102115166A (en) * | 2010-12-31 | 2011-07-06 | 马艳荣 | Method for preparing arsenic trioxide from arsenic sulfide waste |
| CN102115163A (en) * | 2010-12-31 | 2011-07-06 | 马艳荣 | Method for preparing arsenic trioxide from arsenic sulfide waste |
| CN102126753A (en) * | 2010-12-31 | 2011-07-20 | 马艳荣 | Method for preparing arsenic trioxide by using arsenic sulfide waste residue |
| CN102249609A (en) * | 2011-04-29 | 2011-11-23 | 昆明理工大学 | Arsenic-containing waste slag solidified body and preparation method thereof |
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| CN101954370B (en) * | 2010-09-06 | 2012-12-05 | 同济大学 | Method for recycling arsenic-containing waste residues |
| CN101954370A (en) * | 2010-09-06 | 2011-01-26 | 同济大学 | Method for recycling arsenic-containing waste residues |
| CN102115162A (en) * | 2010-12-31 | 2011-07-06 | 马艳荣 | Method for preparing arsenic trioxide by using arsenic sulfide waste slags |
| CN102115165A (en) * | 2010-12-31 | 2011-07-06 | 马艳荣 | Method for preparing arsenic trioxide by arsenic-containing waste water |
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