CN104085903A - Method for separating and purifying sodium hydroxide from arsenic-containing sodium hydroxide solution - Google Patents
Method for separating and purifying sodium hydroxide from arsenic-containing sodium hydroxide solution Download PDFInfo
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- CN104085903A CN104085903A CN201410293728.8A CN201410293728A CN104085903A CN 104085903 A CN104085903 A CN 104085903A CN 201410293728 A CN201410293728 A CN 201410293728A CN 104085903 A CN104085903 A CN 104085903A
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Abstract
The invention discloses a method for purifying sodium hydroxide from an arsenic-containing sodium hydroxide solution, which comprises the following steps: adding an oxidizing agent into the arsenic-containing sodium hydroxide solution, reacting at 35-60 DEG C and removing the precipitate; adding lime milk, reacting at normal temperature and removing the precipitate; analyzing the content of arsenic, heating to 75-100 DEG C, adding an arsenic remover 30-50 times the weight of arsenic, reacting, cooling, standing and filtering; and adding a reagent iron sulfate, reacting at normal temperature, cooling and clarifying to obtain a purified sodium hydroxide solution, wherein the content of sodium hydroxide is 60-100g/L, and the content of arsenic is less than or equal to 0.5mg/L. The purified sodium hydroxide solution can be concentrated into solid sodium hydroxide with greater than or equal to 93% of sodium hydroxide by the prior art, and the content of arsenic is less than or equal to 0.05%. With short flow and simple equipment, the method disclosed by the invention realizes purification and recycling of the sodium hydroxide mother liquid with arsenic content of 1-5g/L, and brings good environment-friendly and economic benefits.
Description
Technical field
The present invention relates to a kind of arsenic alkali separating and purifying method, be specifically related to a kind of from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution.
Background technology
Arsenic is scattered among most of valuable mineral, and the arsenic of having stayed in slag after valuable mineral has refined is a kind of highly toxic substance, soluble in water, and the living environments such as people and animals are existed to huge potential safety hazard, is a kind of material that must carry out safe handling.Thereby refining valuable element or carrying out in product processing, generally all need arsenic to be removed.
At present, removing the most frequently used method of arsenic is the oxidation dearsenification method of hydro-oxidation sodium, but this method can produce by product arsenic alkali slag, and its major ingredient is sodium hydroxide, separately contains sodium arseniate, sodium carbonate, sodium sulfate and a small amount of antimony and selenium etc.Because arsenic is hypertoxic element, arsenic alkali slag can not arbitrarily abandon or process, and arsenic must carry out effective recycling, but the sodium hydroxide solution of having purified after arsenic is still containing arsenic 1～5g/L.In addition, also contain sodium carbonate, sodium sulfate and a small amount of antimony and selenium etc., the low price salt of selenium makes solution rubescent or be sorrel, must further administer.
The form that arsenic exists in arsenic alkali slag is generally sodium arseniate or Sodium metaarsenite, the general method that reclaims arsenic and sodium hydroxide is, first low price arsenic is oxidized to high price arsenic, selenolite turns to high price selenium, reconcentration at a low price, crystallisation by cooling, be recyclable most of sodium arseniate, the alkali lye after dearsenification is made thick alkali through condensing crystal, can return to former smelting system recycling, but thick alkali is higher containing arsenic, system is caused to the poor circulation of arsenic.The method of Steppecd crystallization Separation and Recovery sodium arseniate as disclosed in patent application CN 200410013369.2 and alkali, after first it separate sodium arseniate, remaining mother liquor is further concentrated and makes thick alkali, thick alkali is containing sodium hydroxide 78.88～83.49%, containing sodium carbonate 8.96～12.36%, containing arsenic 2.09～2.65%, then thick alkali is returned to smelting system recycle.But the method has the arsenic of larger residual in thick alkali after processing, caused the vicious cycle of arsenic in system.
Summary of the invention
Technical problem to be solved by this invention is, provide a kind of operating process easy, environmental protection from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, large with arsenic content in thick alkali after solving prior art and processing, alkali and impurity element are difficult to the problem reclaiming.
The technical solution adopted for the present invention to solve the technical problems is: a kind of from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, comprise the following steps:
(1) oxidation: adding oxygenant containing in arsenic sodium hydroxide solution, in 35～60 ℃ of reaction 25～60min, elimination precipitation, the filtrate after being oxidized;
(2) removal of impurities: in the filtrate after the oxidation of step (1) gained, add lime milk solution, stirring reaction 50～90min under normal temperature, elimination precipitation, obtains the filtrate after removal of impurities;
(3) deeply removing arsenic: the mass content of arsenic in the filtrate after analytical procedure (2) gained removal of impurities, be heated to 75～100 ℃, add the dearsenic agent that is equivalent to 30～50 times of contained arsenic weight in filtrate, stirring reaction 25～50min, be cooled to after room temperature, standing 2～5h, elimination precipitates, and obtains the sodium hydroxide solution of degree of depth dearsenification;
(4) solution purification: in the sodium hydroxide solution of every liter of degree of depth dearsenification of step (3) gained, add 5～10g ferric sulfate, stirring reaction 60～90min under normal temperature, clarification 24～72h, elimination precipitation, obtains limpid sodium hydroxide solution.
Further, in step (1), described containing arsenic sodium hydroxide solution, its main component is: sodium hydroxide 120～220g/L, arsenic 1～5g/L; Described oxygenant is hydrogen peroxide, and concentration is 27.5 wt%, and the amount adding is 1.0～2.0 v/v% containing arsenic sodium hydroxide solution.
Further, in step (1), the temperature of described reaction is 40～50 ℃, and the time of reaction is 30min.
Further, in step (2), described lime milk solution is saturated solution, and add-on is 19～40 v/v % of the filtrate after the oxidation of step (1) gained; In described precipitation, contain unreacted excessive milk of lime, this precipitation can be used for configuring milk of lime saturated solution, is back to step (2).
Preferably, in step (2), the reaction times is 60～70min.
Preferably, in step (3), temperature of reaction is 80～90 ℃, and the reaction times is 30～40min, and time of repose is 3～4h.
Further, in step (3), described dearsenic agent is hydrated barta.
Further, in step (3), in described precipitation, contain dearsenic agent, reusable edible, when arsenic mass content reaches 15% in precipitation, changes dearsenic agent.
Further, in step (3), make up water in reaction process, to control naoh concentration at 60～100g/L.
Preferably, in step (4), settling time is 72h.
Further, in step (1), (2), (3) or (4), what elimination precipitation adopted is vacuum filtration, and filter cloth aperture is 350 orders.
Indication of the present invention refers to that containing arsenic sodium hydroxide solution sodium hydrate content is at 120～220g/L, and arsenic content is at 1～5g/L; The mixing solutions that separately contains sodium carbonate, sodium sulfate, sodium arseniate and micro-antimony, selenium.
The chemical equation of above-mentioned steps is as follows:
Step (1):
NaSbO
2﹢H
2O
2﹦NaSbO
3↓﹢H
2O
Na
3AsO
3﹢H
2O
2﹦Na
3AsO
4﹢H
2O
Na
2SeO
3﹢H
2O
2﹦Na
2SeO
4﹢H
2O
Step (2):
Na
2CO
3﹢Ca(OH)
2﹦CaCO
3↓﹢2NaOH
Na
2SO
4﹢Ca(OH)
2﹦CaSO
4↓﹢2NaOH
2Na
3AsO
4﹢3Ca(OH)
2﹦Ca
3(AsO
4)
2↓﹢6NaOH
Na
2SeO
4﹢Ca(OH)
2﹦CaSeO
4↓﹢2NaOH
Step (3):
Na
2CO
3﹢Ba(OH)
2﹦BaCO
3↓﹢2NaOH
Na
2SO
4﹢Ba(OH)
2﹦BaSO
4↓﹢2NaOH
2Na
3AsO
4﹢3Ba(OH)
2﹦Ba
3(AsO
4)
2↓﹢6NaOH
Na
2SeO
4﹢Ba(OH)
2﹦BaSeO
4↓﹢2NaOH
Step (4):
Fe
2(SO
4)
3﹢3Ba(OH)
2﹦3BaSO
4↓﹢2Fe(OH)
3↓
The present invention is to purifying containing arsenic sodium hydroxide solution of producing use sodium hydroxide dearsenification in mineral are smelted after from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution.The present invention, by oxidation step, makes part trivalent arsenic be oxidized to pentavalent arsenic, and oxidation efficiency reaches 99.5%, to more thoroughly react completely with dearsenic agent, up hill and dale arsenic is removed; Trivalent antimony is oxidized to quinquevalence antimony precipitation, to reach the object that removes antimony; Divalence selenolite turns to tetravalence selenium, and oxidation efficiency is 99.5%, to remove in the lump selenium in dearsenification process in the back.In removal step, carbonate, part of sulfuric acid root and the arsenate existing in the filtrate after the milk of lime adding and oxidation generates precipitation and is removed, and total clearance is greater than 70%.In deeply removing arsenic step, the filtrate after using dearsenic agent to removal of impurities is carried out advanced treatment, and it is fast that dearsenic agent hydrated barta has dearsenification, the feature reacting completely, and effective clearance of arsenic reaches 99.9%, after dearsenification, can not bring new impurity into.In filtrate after degree of depth dearsenification, still also remain a small amount of dearsenic agent, need to add reagent of sulfuric acid iron to carry out solution purification, and reagent of sulfuric acid iron has source extensively, the feature that price is low, its use can not introduced new impurity.In sodium hydroxide solution after purification, sodium hydrate content is 60～100g/L, arsenic content≤0.5mg/L, and sodium hydroxide yield is more than 90%, can be directly used in SO
2treating tail gas, and further obtain S-WAT product; The solid sodium hydroxide making after adopting prior art to concentrate sodium hydroxide solution, its sodium hydrate content>=93%, arsenic content≤0.05%, can be as dearsenification, deselenization agent in nonferrous metallurgical process, because its arsenic content is low, reduce the introduction volume of arsenic, well solved a left over by history difficult problem for arsenic vicious cycle in non-ferrous metal metallurgy system.The present invention is through physical and chemical processes such as element valence regulation and control, milk of lime removal of impurities, dearsenic agent deeply removing arsenics, sodium hydroxide solution has been carried out to purifying treatment, realize purification and the recycling of sodium hydroxide, reached good social benefit, environmental benefit and good economic benefit.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
embodiment 1
(1) measure containing arsenic sodium hydroxide solution 500mL(wherein, sodium hydrate content 120g/L, As content 1.0g/L, sodium carbonate 68.3g/L, sodium sulfate 27.5g/L, containing antimony 0.5g/L, selenium 0.1g/L), solution is sorrel, adds the hydrogen peroxide of 5.0mL concentration 27.5% in 40 ℃ of reaction 30min, clarification, filter, obtain the filtrate 505mL after oxidation; (2) in the filtrate after oxidation, add the saturated lime milk solution of 100mL to react 60min under normal temperature, clarification, filters, and obtains the filtrate 540mL after removal of impurities; (3) with chemical analysis, analyze, filtrate after removal of impurities, its arsenic content is 0.3g/L, and the filtrate after removal of impurities is heated to 80 ℃, add dearsenic agent hydrated barta 4.9g reaction 30min, in reaction process, constantly keep the skin wet, control naoh concentration 100g/L, accelerate settling process speed, be cooled to room temperature, clarification 3h, filters dearsenic agent, obtains the filtrate 600mL after dearsenification; (4) filtrate after dearsenification is added to 3.0g reagent of sulfuric acid iron reaction 60min in 20 ℃, be cooled to 20 ℃, clarification 24h, filter, obtain limpid liquid sodium hydroxide solution, through atom fluorescent spectrograph, detect, its sodium hydrate content 100g/L, arsenic content 0.49mg/L, adopts conventional steam concentration method, liquid sodium hydroxide is concentrated into surface and does not emit steam, pour out and be cooled to solid 58.00g, wherein sodium hydrate content 93.1%, arsenic content 0.048%, sodium hydroxide yield 90.0%.The filtration of above step all adopts Büchner funnel vacuum filtration, and filter cloth aperture is 350 orders.
embodiment 2
(1) measure containing arsenic sodium hydroxide solution 500mL(wherein, sodium hydrate content 202.34g/L, As content 3.04g/L, sodium carbonate 75.33g/L, sodium sulfate 28.05g/L, containing antimony 0.4g/L, selenium 0.15g/L), solution is sorrel, adds the hydrogen peroxide of 7.5mL concentration 27.5% in 60 ℃ of reaction 60min, clarification, filter, obtain the filtrate 507mL after oxidation; (2) after oxidation, in filtrate, add the saturated lime milk solution of 150mL to react 90min under normal temperature, clarification, filters, and obtains the filtrate 590mL after removal of impurities; (3) with filtrate after chemical analysis analysis removal of impurities, its arsenic content is 0.61g/L, filtrate after removal of impurities is heated to 100 ℃, adds hydrated barta 14.4g reaction 50min, in reaction process, constantly keep the skin wet, control naoh concentration 80g/L, accelerate settling process speed, be cooled to room temperature, clarification 3.5h, filter dearsenic agent, obtain the filtrate 1265mL after dearsenification; (4) filtrate after dearsenification is added to 9.5g reagent of sulfuric acid iron reaction 90min in 25 ℃, be cooled to 25 ℃, clarification 48h, filter to obtain limpid liquid sodium hydroxide, through atom fluorescent spectrograph, detect its sodium hydrate content 80g/L, arsenic content 0.43mg/L, adopt conventional steam heating concentration method, liquid sodium hydroxide is concentrated into surface and does not emit steam, pour out and be cooled to solid 97.10g, wherein sodium hydrate content 94.81%, arsenic content 0.05%, sodium hydroxide yield 91.0%.The filtration of above step all adopts Büchner funnel vacuum filtration, and filter cloth aperture is 350 orders.
embodiment 3
(1) measure containing arsenic sodium hydroxide solution 500mL(wherein, sodium hydrate content 220g/L, As content 5.0g/L, sodium carbonate 59.8g/L, sodium sulfate 20.3g/L, containing antimony 0.5g/L, selenium 0.13g/L), solution is sorrel, adds the hydrogen peroxide of 10.0mL concentration 27.5% in 50 ℃ of reaction 45min, clarification, filter, obtain the filtrate 510mL after oxidation; (2) after oxidation, in filtrate, add the saturated lime milk solution of 200mL to react 75min under normal temperature, clarification, filters, and obtains the filtrate 640mL after removal of impurities; (3) with filtrate after chemical analysis analysis removal of impurities, its arsenic content is 0.75g/L, filtrate after removal of impurities is heated to 90 ℃, adds hydrated barta 24.0g reaction 40min, in reaction process, constantly keep the skin wet, control naoh concentration 60g/L, accelerate settling process speed, be cooled to room temperature, clarification 4h, filter dearsenic agent, obtain the filtrate 1834mL after dearsenification; (4) filtrate after dearsenification is added to 18.34g reagent of sulfuric acid iron reaction 80min in 28 ℃, be cooled to 28 ℃, clarification 72h, filter to obtain limpid liquid sodium hydroxide, through atom fluorescent spectrograph, detect its sodium hydrate content 60g/L, arsenic content 0.39mg/L, adopt conventional steam heating concentration method, liquid sodium hydroxide is concentrated into surface and does not emit steam, pour out and be cooled to solid 106.49g, wherein sodium hydrate content 95.03%, arsenic content 0.043%, sodium hydroxide yield 92.0%.The filtration of above step all adopts Büchner funnel vacuum filtration, and filter cloth aperture is 350 orders.
embodiment 4
(1) measure containing arsenic sodium hydroxide solution 500mL(wherein, sodium hydrate content 220g/L, As content 5.0g/L, sodium carbonate 59.8g/L, sodium sulfate 20.3g/L, containing antimony 0.5g/L, selenium 0.13g/L), solution is sorrel, adds the hydrogen peroxide of 7.5mL concentration 27.5% in 50 ℃ of reaction 45min, clarification, filter, obtain the filtrate 507mL after oxidation; (2) the milk of lime reaction filter residue 110g in embodiment 3 is supplemented to the saturated Wingdale breast of 130mL and be made into 200mL saturated aqueous solution, add in the rear filtrate of oxidation and react 80min under normal temperature, clarification, filters, and obtains the filtrate 636mL after removal of impurities; (3) with filtrate after chemical analysis analysis removal of impurities, its arsenic content is 0.79g/L, and the filtrate after removal of impurities is heated to 90 ℃, by the hydrated barta reaction slag 22g(in embodiment 3 wherein, hydrated barta content 68.64%, arsenic content 2.18%) add in removal of impurities filtrate and react 50min, in reaction process, constantly keep the skin wet, control naoh concentration 70g/L, accelerate settling process speed, be cooled to room temperature, clarification 4h, filter dearsenic agent, obtain the filtrate 1572mL after dearsenification; (4) filtrate after dearsenification is added to 12.57g reagent of sulfuric acid iron reaction 80min in 28 ℃, be cooled to 28 ℃, clarification 72h, filter to obtain limpid liquid sodium hydroxide, through atom fluorescent spectrograph, detect its sodium hydrate content 70g/L, arsenic content 0.43mg/L, adopt conventional steam heating concentration method, liquid sodium hydroxide is concentrated into surface and does not emit steam, pour out and be cooled to solid 106.68g, wherein sodium hydrate content 93.83%, arsenic content 0.049%, sodium hydroxide yield 91.0%.The filtration of above step all adopts Büchner funnel vacuum filtration, and filter cloth aperture is 350 orders.
Claims (9)
1. from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: comprise the following steps:
(1) oxidation: adding oxygenant containing in arsenic sodium hydroxide solution, in 35～60 ℃ of reaction 25～60min, elimination precipitation, the filtrate after being oxidized;
(2) removal of impurities: in the filtrate after the oxidation of step (1) gained, add lime milk solution, stirring reaction 50～90min under normal temperature, elimination precipitation, obtains the filtrate after removal of impurities;
(3) deeply removing arsenic: the mass content of arsenic in the filtrate after analytical procedure (2) gained removal of impurities, be heated to 75～100 ℃, add the dearsenic agent that is equivalent to 30～50 times of contained arsenic weight in filtrate, stirring reaction 25～50min, be cooled to after room temperature, standing 2～5h, elimination precipitates, and obtains the sodium hydroxide solution of degree of depth dearsenification;
(4) solution purification: in the sodium hydroxide solution of every liter of degree of depth dearsenification of step (3) gained, add 5～10g ferric sulfate, stirring reaction 60～90min under normal temperature, clarification 24～72h, elimination precipitation, obtains limpid sodium hydroxide solution.
2. according to claim 1 from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: in step (1), described containing arsenic sodium hydroxide solution, its main component is: sodium hydroxide 120～220g/L, arsenic 1～5g/L; Described oxygenant is hydrogen peroxide, and concentration is 27.5 wt%, and the amount adding is 1.0～2.0 v/v% containing arsenic sodium hydroxide solution.
According to described in claim 1 or 2 from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: in step (1), the temperature of described reaction is 40～50 ℃, and the time of reaction is 30min.
According to one of claim 1～3 Suo Shu from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: in step (2), described lime milk solution is saturated solution, and add-on is 19～40 v/v % of the filtrate after the oxidation of step (1) gained; In described precipitation, contain unreacted excessive milk of lime, this precipitation is used for configuring milk of lime saturated solution, is back to step (2).
According to one of claim 1～4 Suo Shu from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: in step (3), temperature of reaction is 80～90 ℃, and the reaction times is 30～40min, and time of repose is 3～4h.
According to one of claim 1～5 Suo Shu from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: in step (3), described dearsenic agent is hydrated barta.
According to one of claim 1～6 Suo Shu from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: in step (3), in described precipitation, contain dearsenic agent, recycle, when arsenic mass content reaches 15% in precipitation, change dearsenic agent.
According to one of claim 1～7 Suo Shu from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: in step (3), make up water in reaction process, controls naoh concentration at 60～100g/L.
According to one of claim 1～8 Suo Shu from the method containing separating-purifying sodium hydroxide arsenic sodium hydroxide solution, it is characterized in that: what in step (1), (2), (3) or (4), elimination precipitation adopted is vacuum filtration, and filter cloth aperture is 350 orders.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111450465A (en) * | 2020-03-31 | 2020-07-28 | 白银原点科技有限公司 | Method for removing arsenic from solid material |
| CN114788820A (en) * | 2022-04-18 | 2022-07-26 | 陕西省动物研究所 | Starch matrix empty capsule with biological auxiliary function pharmacological action |
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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 |
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| CN102560132A (en) * | 2012-02-03 | 2012-07-11 | 锡矿山闪星锑业有限责任公司 | Method for treating selenium alkali residues in antimony pyro-refining |
| CN102557222A (en) * | 2012-02-15 | 2012-07-11 | 天津理工大学 | Method for removing trace arsenic from aqueous solution |
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2014
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Patent Citations (4)
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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 |
| CN101899574A (en) * | 2010-08-04 | 2010-12-01 | 锡矿山闪星锑业有限责任公司 | Method for comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in antimony pyrometallurgical smelting |
| CN102560132A (en) * | 2012-02-03 | 2012-07-11 | 锡矿山闪星锑业有限责任公司 | Method for treating selenium alkali residues in antimony pyro-refining |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111450465A (en) * | 2020-03-31 | 2020-07-28 | 白银原点科技有限公司 | Method for removing arsenic from solid material |
| CN114788820A (en) * | 2022-04-18 | 2022-07-26 | 陕西省动物研究所 | Starch matrix empty capsule with biological auxiliary function pharmacological action |
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