CN102650000A - Method for recovering bismuth and arsenic from bismuth and arsenic-containing solution - Google Patents
Method for recovering bismuth and arsenic from bismuth and arsenic-containing solution Download PDFInfo
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- CN102650000A CN102650000A CN2012101318173A CN201210131817A CN102650000A CN 102650000 A CN102650000 A CN 102650000A CN 2012101318173 A CN2012101318173 A CN 2012101318173A CN 201210131817 A CN201210131817 A CN 201210131817A CN 102650000 A CN102650000 A CN 102650000A
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Abstract
The invention discloses a method for recovering bismuth and arsenic from a bismuth and arsenic-containing solution. The method is characterized by comprising the steps as follows: adjusting the pH value of the bismuth and arsenic-containing solution to be in a certain range so as to deposit out the bismuth and the arsenic in the solution in a form of bismuth arsenate; processing the obtained bismuth arsenate deposit by a strong base solution to effectively separate the arsenic from the bismuth; and respectively recovering the bismuth and the arsenic from a basic leached residue and a basic leached solution. According to the method, the solution does not need to be subjected to arsenic removal before the bismuth deposition of the leached solution containing higher arsenic and bismuth, so that the bismuth loss in the arsenic removal process is avoided to increase the recovery rate of the bismuth in the solution; the arsenic and the bismuth in the solution are co-deposited in the form of the bismuth arsenate, and the purpose of effectively separating the arsenic from the bismuth is achieved by the basic leached bismuth arsenate deposit according to the characteristic that the arsenate deposit easily acts with strong base and is converted into soluble arsenate and insoluble metal oxide or hydroxide; the arsenic is recovered in a form of sodium arsenate while the bismuth is recovered; and due to small bismuth loss in the arsenic and bismuth co-deposition and bismuth arsenate base leaching processes, the total recovery rate of the bismuth in the whole process is guaranteed to be not less than 90%.
Description
Technical field
The invention discloses a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic.Belong to resource recovery technology field.
Technical background
Bismuth is a kind of rare metal, the mineral of bismuth mostly with metalliferous mineral symbiosis such as tungsten, molybdenum, lead, tin, copper, seldom be formed with the mineral deposit of independent extraction value, thus need be in other main metal ore dressing process the separation of Bismuth concentrate.In addition, bismuth also often gets in the by product of other main metal smelting processes, like flue dust of lead anode slurry, copper melting and blowing etc.Therefore, bismuth is normally recycled as by product in the production process of metals such as copper, lead, zinc.
When from the anode sludge or various smelting smoke dust, reclaiming bismuth, adopt the Technology of hydrometallurgy usually, promptly handle making bismuth get into the solution phase through acidleach, the pH value through adjustment solution makes it that hydrolytic precipitation take place again.In order to improve the leaching yield of bismuth, generally contain a large amount of cl ionss in the acid solution of leaching usefulness, like H
2SO
4-NaCl solution, H
2SO
4-FeCl
3Solution etc., the hydrolysate that obtains thus is BiOCl normally.This hydrolysate is dissolved in the acid back can obtains sponge bismuth through the iron replacement reaction.Research shows; Only the bismuth in the solution could hydrolysis generate BiOCl under the lower situation of arsenic content; And when the arsenic content in the solution when higher; Before heavy bismuth, primarily will carry out dearsenification and handle, thereby this treating processes tends to cause the loss of bismuth that the recovery of bismuth in the whole technological process is descended solution.
For the higher flue dust or the anode sludge of arsenic content, when carrying out acidleach and handle,, could reclaim bismuth after needing complicated dearsenicating technology that it is done further processing because arsenic also can be leached in the solution with other metal.Therefore, study and a kind ofly need not carry out independent dearsenification and handle, directly from the higher bismuth-containing solution of arsenic concentration, reclaim the method for bismuth and arsenic, realize the high efficiency separation and the recycling of two kinds of elements, very necessity solution.
Summary of the invention
The objective of the invention is to propose a kind of method that from the solution that contains arsenic and bismuth, reclaims bismuth and arsenic; Emphasis is to reclaim from the pickling liquor of bismuth-containing materials such as the anode sludge, smelting cigarette ash to reclaim arsenic and bismuth; Make leach liquor can access efficient utilization, improve the economic results in society that melting waste slag is handled.
A kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic of the present invention comprises the steps:
The first step: selectivity codeposition
The pH value that will contain the solution of arsenic bismuth adjusts to 0～1, stirs to be no less than 30 minutes, filters, the win filter residue and first filtrating, and said first filter residue mainly contains arsenic and antimony, reclaims with conventional recovery method; First pH value of filtrate is adjusted to 2.5～4, and stirring is no less than 30 minutes, filters; Second filter residue and second filtrating, second filter residue is bismuth and the arsenic codeposit with arsenic acid bismuth form;
Second step: alkali soaks treatment process
Second filter residue of the first step gained is mixed with alkaline solution, under condition of stirring, carry out alkali in 20～95 ℃ and soak processing, obtain slurry; Filter, obtain the 3rd filter residue and the 3rd filtrate for later use; The liquid-solid ratio of the said sodium hydroxide solution and the second filter residue mixture is (3-6): 1; Alkali soaks the treatment time and is no less than 60 minutes;
The 3rd step: the 3rd filtrating evaporative crystallization, reclaim arsenate
50～95 ℃ of evaporation concentration, sodium arseniate is separated out in crystallization with the 3rd filtrating; Mother liquor behind the recovery sodium arseniate returns alkali and soaks treatment process;
The 4th step: bismuth is reclaimed in the displacement of the 3rd filter residue
The 3rd filter residue is dissolved in the salpeter solution of chloride ion-containing, adds the Bi in reduced iron powder and the solution
3+Carry out replacement(metathesis)reaction and prepare sponge bismuth.
The present invention is a kind of to reclaim from the solution that contains the arsenic bismuth in the method for bismuth and arsenic, and the said solution that contains the arsenic bismuth is meant the pickling liquor that the mineral that contain bismuth and arsenic or metallurgical slag obtain.
A kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic of the present invention, in the said the first step, the adjustment of pH value adopts ammoniacal liquor or sodium hydroxide solution to carry out.
A kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic of the present invention, in the said the first step, the pH value that will contain the solution of arsenic bismuth adjusts to 0～1; First pH value of filtrate is adjusted to 2.5～4.
A kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic of the present invention, the alkaline solution in said second step is an alkali hydroxide soln, concentration is 1～10mol/L; Preferred sodium hydroxide solution.
A kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic of the present invention; In said the 4th step; The salpeter solution of chloride ion-containing is the mixing solutions of nitric acid and sodium-chlor or iron(ic)chloride, and wherein chlorine ion concentration is 0.5～1mol/L, and concentration of nitric acid is 1.15～1.25mol/L.
A kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic of the present invention, in said the 4th step, the add-on of reduced iron powder is no less than 1.5 times of stoichiometric ratio.
The present invention is owing to adopt above-mentioned process method, except that containing bismuth and arsenic, also contains other metals ions such as antimony, iron, copper, zinc in the pickling liquor that obtains according to the mineral that contain bismuth and arsenic or metallurgical slag, and its pH value is generally less than 0.Therefore, at first in solution, add ammoniacal liquor or sodium hydroxide solution, the pH value of solution is transferred between 0～1, preferably between 0～0.8, stir 30 minutes after-filtration, filter residue mainly contains arsenic and antimony, recycles with conventional recovery method; Filtrating is used to reclaim arsenic and bismuth.Make bismuth, arsenic and other separation of metal ions in the pickling liquor.
Then, continue in filtrating, to add ammoniacal liquor or sodium hydroxide solution, its pH value is transferred between 2.5～4; Preferably between 3.2～3.5; Stirring reaction 30 minutes makes bismuth and arsenic in the solution with the form co-precipitation of arsenic acid bismuth, in this process in the solution as have an iron ion; It also can precipitate in the lump separates out, and other ions then are retained in the solution.
The coprecipitate of getting bismuth and arsenic carries out alkali and soaks processing, realizes separating of arsenic and bismuth.In order to reduce production costs, the used alkaline solution of this process is preferably sodium hydroxide solution, and the concentration range of sodium hydroxide solution is preferably 1-5mol/L.Alkali soaks service temperature and is preferably 50～95 ℃, to improve the solubleness of sodium arseniate.Confirm that according to the concentration of used sodium hydroxide solution alkali soaks the initial liquid-solid ratio in the process, it is excessive 10% that the consumption of sodium hydroxide needs at least, and extraction time should be greater than 30 minutes under condition of stirring, with the leaching yield of arsenic in guaranteeing to precipitate greater than 95%.
Alkali soaked handle the slurry obtain and carry out liquid-solid separation; With the immersion liquid of gained alkali 50～95 ℃ of evaporation concentration; Sodium arseniate is reclaimed in crystallization; Confirm cycles of concentration according to the consumption of institute's hydro-oxidation sodium in this process, the mother liquor behind the recovery sodium arseniate then returns alkali and soaks operation to make full use of wherein unreacted sodium hydroxide, also reduces the discharging of arsenic-containing waste water simultaneously.
It is rich bismuth material that alkali soaks slag, and bi content can surpass 50%.It is dissolved in aqueous nitric acid, the preparation bismuth nitrate solution.In order to improve its dissolution rate, should contain a certain amount of cl ions in the used salpeter solution, the mixing solutions of available nitric acid and sodium-chlor or nitric acid and iron(ic)chloride.In bismuth nitrate solution, add iron powder, can obtain sponge bismuth.Consider the recovery that will improve bismuth in the solution on the one hand, also will improve the purity of gained sponge bismuth simultaneously, iron powder consumption best excessive 50%～100%.The total yield of bismuth can reach more than 90% in the whole technological process.
Advantage of the present invention is: 1) do not need separately solution to be carried out dearsenification before bismuth is handled and handle in that arsenic, bi content are all sunk than higher leach liquor, avoided the dearsenification process to cause the loss of bismuth, thereby improved the recovery of bismuth in the solution; 2) make arsenic and bismuth in the solution with the form generation codeposition of arsenic acid bismuth; Utilize arsenate deposition to be converted into the characteristics of the MOX or the oxyhydroxide of solubility arsenate and indissoluble easily with the highly basic effect, carry out alkali and soak the purpose that processing reaches effective separation arsenic and bismuth through gained arsenic acid bismuth is precipitated; 3) can when reclaiming the solution bismuth, the form of the arsenic in the solution with sodium arseniate be reclaimed; 4) because to soak in the process loss amount of bismuth at the co-precipitation of arsenic bismuth and arsenic acid bismuth alkali very little, guaranteed that the total yield of bismuth in the whole technological process is not less than 90%.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Specific embodiment
Embodiment one
Sulfuric acid leaches in certain metallurgical slag gained leach liquor and mainly contains As:14.72g/L; Bi:14.28g/L; Cu:6.78g/L; Fe:3.11g/L; Pb:2.17g/L; Sb:2.12g/L.
In the churned mechanically while, the ammoniacal liquor of (mass concentration, below identical) is transferred about the pH value to 0.5 of solution with 15%, keeps mechanical stirring reaction 30 minutes, and suction filtration obtains deposition and filtrating.The filtrating sampling analysis, the deposition rate that calculates each element according to filtrate component is As 24%, and Bi 3.3%, and Cu 3.2%, and Fe 2.8%, and Pb 36%, and Sb 85%.
Continue to regulate pH value of filtrate to 3.2 with 15% ammoniacal liquor, keep mechanical stirring reaction 30 minutes, suction filtration obtains deposition and filtrating.The gained deposition is carried out XRD analysis find that it is mainly the arsenic acid bismuth.Deposition rate according to bismuth and arsenic in the filtrating sampling analysis calculating solution all surpasses 95%.
With the sodium hydroxide solution of 2mol/L above-mentioned deposition being carried out alkali and soak processing, is 5: 1 in liquid-solid ratio, and agitation leach is 1 hour under the condition that temperature is 50 ℃.The leaching yield that arsenic and bismuth were analyzed and calculated in liquid-solid separation back to leach liquor is As＞97%, Bi＜1%.
Alkali soaked the leach liquor that obtains in the process 80 ℃ of evaporation concentration, reclaim sodium arseniate.Arsenic content is about 22% in the gained sodium arseniate crystal.
Mixing solutions dissolving alkali with nitric acid and sodium-chlor soaks slag, is mixed with to contain Bi 0.05mol/L, Cl
-0.8mol/L liquid before the displacement of pH ≈ 0 adds the Bi in reduced iron powder and the solution
3+Carry out replacement(metathesis)reaction and prepare sponge bismuth, Bi＞90% in the sponge bismuth for preparing under the situation of iron powder excessive 50%, the recovery of bismuth is about 99%.The total yield of whole technological process bismuth is 93%.
Embodiment two
Used leach liquor composition and operating process are the pH value to 0 of solution being transferred solution with 15% ammoniacal liquor with embodiment one, and the deposition rate that filters a post analysis element is As 16.2%, and Bi 3.3%, and Cu 3.2%, and Fe 2.2%, and Pb 27.5%, and Sb 78.9%.
Continue to regulate pH value of filtrate to 3.5 with 15% ammoniacal liquor, keep mechanical stirring reaction 30 minutes, suction filtration obtains deposition and filtrating.The gained deposition is carried out XRD analysis find that it is mainly the arsenic acid bismuth.Deposition rate according to bismuth and arsenic in the filtrating sampling analysis calculating solution all surpasses 98%.
With the sodium hydroxide solution of 4mol/L above-mentioned deposition being carried out alkali and soak processing, is 3: 1 in liquid-solid ratio, and agitation leach is 1 hour under the condition that temperature is 90 ℃.The leaching yield that arsenic and bismuth were analyzed and calculated in liquid-solid separation back to leach liquor is As＞97%, Bi＜1%.
Alkali soaked the leach liquor that obtains in the process 50 ℃ of evaporation concentration, reclaim sodium arseniate.Arsenic content is about 21.2% in the gained sodium arseniate crystal.
Mixing solutions dissolving alkali with nitric acid and sodium-chlor soaks slag, is mixed with to contain Bi 0.05mol/L, Cl
-0.8mol/L liquid before the displacement of pH ≈ 0 adds the Bi in reduced iron powder and the solution
3+Carry out replacement(metathesis)reaction and prepare sponge bismuth, Bi＞90% in the sponge bismuth for preparing under the situation of iron powder excessive 100%, the recovery of bismuth is about 99%.The total yield of whole technological process bismuth is 95%.
Embodiment three
Used leach liquor composition and operating process are the pH value to 0.8 of solution being transferred solution with 15% ammoniacal liquor with embodiment one, and the deposition rate that filters a post analysis element is As 33.2%, and Bi 4.2%, and Cu 4.2%, and Fe 3.5%, and Pb 44.2%, and Sb 88.9%.
Continue to regulate pH value of filtrate to 3.5 with 15% ammoniacal liquor, keep mechanical stirring reaction 30 minutes, suction filtration obtains deposition and filtrating.The gained deposition is carried out XRD analysis find that it is mainly the arsenic acid bismuth.Deposition rate according to bismuth and arsenic in the filtrating sampling analysis calculating solution all surpasses 98%.
With the sodium hydroxide solution of 1mol/L above-mentioned deposition being carried out alkali and soak processing, is 6: 1 in liquid-solid ratio, and agitation leach is 1 hour under the condition that temperature is 70 ℃.The leaching yield that arsenic and bismuth were analyzed and calculated in liquid-solid separation back to leach liquor is As＞97%, Bi＜1%.
Alkali soaked the leach liquor that obtains in the process 70 ℃ of evaporation concentration, reclaim sodium arseniate.Arsenic content is about 21.8% in the gained sodium arseniate crystal.
Mixing solutions dissolving alkali with nitric acid and sodium-chlor soaks slag, is mixed with to contain Bi 0.05mol/L, Cl
-1mol/L, liquid before the displacement of pH ≈ 0 adds the Bi in reduced iron powder and the solution
3+Carry out replacement(metathesis)reaction and prepare sponge bismuth, Bi＞90% in the sponge bismuth for preparing under the situation of iron powder excessive 80%, the recovery of bismuth is about 99%.The total yield of whole technological process bismuth is 91%.
Claims (8)
1. a method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic comprises the steps:
The first step: selectivity codeposition
The pH value that will contain the solution of arsenic bismuth adjusts to 0～1, stirs to be no less than 30 minutes, filters, the win filter residue and first filtrating, and said first filter residue mainly contains arsenic and antimony, reclaims with conventional recovery method; First pH value of filtrate is adjusted to 2.5～4, and stirring is no less than 30 minutes, filters; Get second filter residue and second filtrating, second filter residue is the codeposit that bismuth and arsenic exist with arsenic acid bismuth form;
Second step: alkali soaks treatment process
Second filter residue of the first step gained is mixed with alkaline solution, under condition of stirring, carry out alkali in 20～95 ℃ and soak processing, obtain slurry; Filter, obtain the 3rd filter residue and the 3rd filtrate for later use; The liquid-solid ratio of the said sodium hydroxide solution and the second filter residue mixture is (3-6): 1; Alkali soaks the treatment time and is no less than 60 minutes;
The 3rd step: the 3rd filtrating evaporative crystallization, reclaim arsenate
50～95 ℃ of evaporation concentration, sodium arseniate is separated out in crystallization with the 3rd filtrating;
The 4th step: bismuth is reclaimed in the displacement of the 3rd filter residue
The 3rd filter residue is dissolved in the salpeter solution of chloride ion-containing, adds the Bi in reduced iron powder and the solution
3+Carry out replacement(metathesis)reaction and prepare sponge bismuth.
2. a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic according to claim 1 is characterized in that: the said solution that contains the arsenic bismuth is meant the pickling liquor that the mineral that contain bismuth and arsenic or metallurgical slag obtain.
3. a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic according to claim 2 is characterized in that: in the said the first step, the adjustment of pH value adopts ammoniacal liquor or alkali hydroxide soln to carry out.
4. a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic according to claim 3, it is characterized in that: in the said the first step, the pH value that will contain the solution of arsenic bismuth adjusts to 0～0.8; First pH value of filtrate is adjusted to 3.2～3.5.
5. a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic according to claim 4 is characterized in that: the alkaline solution in said second step is an alkali hydroxide soln, and concentration is 1～10mol/L.
6. a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic according to claim 5; It is characterized in that: in said the 4th step; The salpeter solution of chloride ion-containing is the mixing solutions of nitric acid and sodium-chlor or iron(ic)chloride; Wherein chlorine ion concentration is 0.5～1mol/L, and concentration of nitric acid is 1.15～1.25mol/L.
7. a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic according to claim 6 is characterized in that: in said the 4th step, reduced iron powder is pressed iron and Bi
3+1.5 times amount of the stoichiometric ratio of replacement(metathesis)reaction adds.
8. a kind of method that from the solution that contains the arsenic bismuth, reclaims bismuth and arsenic according to claim 7 is characterized in that: in the 3rd step, the mother liquor behind the recovery sodium arseniate returns alkali and soaks treatment process.
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| CN103014349A (en) * | 2012-12-14 | 2013-04-03 | 武汉钢铁(集团)公司 | Process for recycling bismuth from gas sludge to prepare BiOCl (Bismuth Oxychloride) |
| CN107164785A (en) * | 2017-05-24 | 2017-09-15 | 江西理工大学 | A kind of copper electrolyte precipitation to remove impurities and precipitating reagent chlorination regeneration method |
| CN108640390A (en) * | 2018-05-31 | 2018-10-12 | 阳谷祥光铜业有限公司 | A kind of processing method of stibium-containing wastewater |
| CN109312423A (en) * | 2017-01-30 | 2019-02-05 | 住友金属矿山株式会社 | The method of purification of bismuth |
| CN111876601A (en) * | 2020-06-16 | 2020-11-03 | 中南大学 | Method for treating arsenic-lead-containing anode mud by using low-grade magnesium oxide-containing soot through circulating alkaline leaching |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014349A (en) * | 2012-12-14 | 2013-04-03 | 武汉钢铁(集团)公司 | Process for recycling bismuth from gas sludge to prepare BiOCl (Bismuth Oxychloride) |
| CN109312423A (en) * | 2017-01-30 | 2019-02-05 | 住友金属矿山株式会社 | The method of purification of bismuth |
| CN107164785A (en) * | 2017-05-24 | 2017-09-15 | 江西理工大学 | A kind of copper electrolyte precipitation to remove impurities and precipitating reagent chlorination regeneration method |
| CN108640390A (en) * | 2018-05-31 | 2018-10-12 | 阳谷祥光铜业有限公司 | A kind of processing method of stibium-containing wastewater |
| CN111876601A (en) * | 2020-06-16 | 2020-11-03 | 中南大学 | Method for treating arsenic-lead-containing anode mud by using low-grade magnesium oxide-containing soot through circulating alkaline leaching |
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Application publication date: 20120829 |