CN1120018A - Method of wet-extraction for arsenic - Google Patents
Method of wet-extraction for arsenic Download PDFInfo
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- CN1120018A CN1120018A CN 94110976 CN94110976A CN1120018A CN 1120018 A CN1120018 A CN 1120018A CN 94110976 CN94110976 CN 94110976 CN 94110976 A CN94110976 A CN 94110976A CN 1120018 A CN1120018 A CN 1120018A
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- Prior art keywords
- arsenic
- reaction
- wet
- extraction
- white
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Abstract
The wet process for extracting As includes such steps as oxidizing decomposition of arsenic sulfide with sulfuric acid, raising reaction temp. to separate out suspended simple substance sulfur, fused simple substance sulfur or sulfur dioxide gas from arsenic sulfide and transform As into solid As2O3, collecting solid As2O3, and reducing it with acidic solution containing stannous ions to obtain single As substance with 99.9% of As content, and features low cost, high efficiency and no pollution. It is also suitable to produce As2O2 product with 99.9% purity.
Description
The present invention be relevant from arsenic sulfide (as As
2S
2, As
2S
3) and contain wet-extraction for arsenic in the arsenic industrial residue (As) and (contain and carry white arsenic As
2O
3) method.
Elemental arsenic (As) or white arsenic (As
2O
3) be the very important industrial chemicals of a class, just be widely used in industries such as semi-conductor, metallurgy, glass, agricultural chemicals, process hides, printing and dyeing, medicine at present.The pozzuolite owner will derive from natural mineral, as arsenic disulfide (As
2S
2) and arsenic trisulfide (As
2S
3) etc., also derive from and contain the arsenic industrial residue, (be mainly As the arsenic filter residue of handling arsenic-containing waste water
2S
3), arsenic-containing smoke dust and contain arsenic metallurgical slag etc.From arsenic sulfide, contain the method for carrying arsenic the arsenic industrial residue, be broadly divided into pyrogenic process and wet method two big classes.Traditional pyrometallurgical smelting at high temperature produces a large amount of white arsenic (As
2O
3) hypertoxic flue dust and deleterious sulfurous gas (SO
2) gas, seriously poison HUMAN HEALTH and contaminate environment, be under an embargo or limit production in many countries.Existing wet production and research method have: (1) copper-bath lixiviation process, the 12-17 page of " non-ferrous metal (smelting) " the 6th phase in 1984 reported " the arsenic evil is administered with white arsenic and extracted process Selection " literary composition, wherein reported " copper-bath lixiviation process " for the 13rd page, this technology is that (major ingredient is As with sulfuration arsenous filter residue
2S
3) produce white arsenic for raw material, its principle is to adopt copper sulfate (CuSO
4) solution replace arsenus acid (As (III)), blowing air is oxidized to arsenic acid (As (V)) and is dissolved in the water, and uses sulfurous gas (SO then
2) gas reduction and produce white arsenic product.Its main chemical reactions is:
(5)
This method is owing to adopt the high copper sulfate (CuSO of price
4) be converted into the low cupric sulfide of price (CuS), make As (III) be oxidized to As (V) earlier, restore and make As
2O
3Product, thereby cost height, long flow path, investment is big, and consumption is many, has increased the chemical treatment expense greatly, the direct yield of arsenic only 75-80%.(2) ferric sulphate method, " Chinese patent communique " on May 10th, 1986, disclosed number of patent application was 851042205A, and name is called the patent application specification of " arsenic filter cake method of comprehensive utilization ", and specification sheets has been introduced this method with ferric sulphate (Fe
2(SO
4)
3) make oxygenant, moltenly in acidic aqueous solution soak arsenic filter cake (effective ingredient is As
2S
3), arsenic trisulfide is oxidized to arsenus acid (HAsO
2) and arsenic acid (H
3AsO
4), and the arsenic in the solution mainly exists with arsenic acid (As (V)) form (solubleness height), and sulphur is stayed in the slag with elemental sulfur (S) form, with sulfurous gas (SO
2) gas reduction obtains white arsenic product, the direct yield of arsenic has only 83-85%.In addition, in August, 1993, " Central-South China Institute of Mining and Metallurgy's journal " the 24th rolled up the 483-489 page of the 4th phase and delivered the paper that is entitled as " preparing white arsenic from arsenic-containing waste residue ", and it also is to utilize the desulfurization of ferric sulphate method to prepare white arsenic, and different is at circulation fluid (leach liquor SO
2As is extracted in reduction
2O
3After, with the Fe in the solution
2+Form Fe through regeneration
3+Continue to use) the middle certain density As (V) of maintenance, utilize the Fe (III) in the solution, the acting in conjunction of As (V) removes As
2S
3In sulphur, produce As
2O
3Its main chemical reactions is:
(8)
(10)
This method still is oxidized to As (V) for As (III) owing to put forward the arsenic process, is reduced into As (III) again, and technical process is long, and chemical depletion is big, adopts sulfurous gas (SO
2) gas reduction is gas-liquid phase reaction, reaction kinetics is little, and water consumption is big, and cost is also higher.(3) chlorination process, volume " U.S. chemical abstract " the 115th page reported " wet method system arsenic " processing method in 1977 the 87th, this method is to adopt the chlorine (Cl of extremely strong oxidisability
2) processing As
2S
3Or As
2O
3, oxidation forms arsenic acid (As (V)), uses tin protochloride (SnCl then
2) be reduced to elemental arsenic (As).Its main chemical reactions is:
(11)
(12)
(13)
Obviously, adopt chlorine to make oxygenant, oxidisability is excessive, and As (III) is oxidized to As (V), is reduced into As (III) again, and chemical depletion is big, Cl
2With As
2S
3Or As
2O
3Be gas-solid state reaction, reaction kinetics is less, and Cl
2Corrosion to equipment is very big.In addition, wet method also has ion exchange method, organic solvent extractionprocess etc.
In sum, carry in the arsenic method above-mentioned, the weak point of pyrogenic process is that environmental pollution is serious, and the resource recycling rate is low, so that is under an embargo or limit production.The weak point of wet method then is: 1. putting forward the arsenic process is As (III) → As (V) → As (III) → As (simple substance), and technical process is longer, has increased the consumption of pharmaceutical chemicals greatly, and efficient is low; 2. adopt gas-liquid phase or gas-solid state reaction in oxidation or reduction process, reaction kinetics is little; 3. water consumption is big, the cost height.Therefore industrial, develop a kind of novel method of wet-extraction for arsenic for being badly in need of.
The object of the present invention is to provide a kind of wet-extraction for arsenic (contain and carry white arsenic) method, have technology simple, consume less, cost is low, efficient is high, characteristics such as pollution-free.
Solution of the present invention is to adopt sulfuric acid (H
2SO
4) the molten arsenic sulfide (As that soaks of solution
2S
2Or As
2S
3), vitriolic concentration 〉=70%, the liquid-solid ratio of sulfuric acid and arsenic sulfide material is (1.5-6) L: 1kg, the temperature of sulfuric acid and the reaction of arsenic sulfide is 40 ℃～280 ℃, mechanical stirring, reaction times is 0.5-5 hours, after arsenic sulfide decomposes, generate the white arsenic solid, sulphur is along with the rising of reaction control temperature, respectively with the suspension elemental sulfur, molten elemental sulfur or sulfur dioxide gas form are separated from arsenic sulfide, the white arsenic throw out that reaction generates is collected from the mixture of reaction, through washing, filter, obtain the white arsenic solid, the white arsenic solid that obtains is further reduced with containing Ya Xi (Sn (II)) ionic acidic solution, the consumption of stannous ion surpasses its chemical reaction metering, the concentration of acid is (1-12) N/L in the acidic solution, contain the acidic solution of stannous ion and the liquid-solid ratio of white arsenic and be (1.5-6) L: 1kg, mechanical stirring, temperature of reaction is 10 ℃-95 ℃, and the reaction times is 0.5-1.5 hours, after the reaction, from reaction mixture, collect elemental arsenic, through washing, filter, oven dry gets final product.
Chemical principle of the present invention can be represented (with As with following chemical equation
2S
3Be example, other arsenic sulfide is similar):
(15)
Feature of the present invention is that also sulfuric acid is oleum.
Feature of the present invention is that also Ya Xi (Sn (II)) ionic consumption is 1.2-2 times of its chemical reaction metering.
It is tin protochloride (SnCl that feature of the present invention also is to contain Ya Xi (Sn (II)) ionic acidic solution
2) and the mixed aqueous solution of hydrochloric acid (HCl).
It is stannous sulfate (SnSO that feature of the present invention also is to contain Ya Xi (Sn (II)) ionic acidic solution
4) and sulfuric acid (H
2SO
4) mixed aqueous solution.
The present invention carries out according to the following steps: 1. desulfurization: adopt sulfuric acid (H
2SO
4) the molten arsenic sulfide (As that soaks of solution
2S
2Or As
2S
3), vitriolic concentration 〉=70%, it perhaps is oleum, the liquid-solid ratio of sulfuric acid and arsenic sulfide material is (1.5-6) L: 1kg, join sulphuric acid soln and arsenic sulfide solid in the reactor simultaneously, temperature of reaction is 40 ℃-280 ℃, mechanical stirring, reaction times is 0.5-5 hours, after arsenic sulfide decomposes, generates the white arsenic solid, sulphur is along with the rising of reaction control temperature, respectively with the suspension elemental sulfur, molten elemental sulfur or sulfur dioxide gas form are separated from arsenic sulfide, and in the mother liquor bottom, solubility in acid impurity is dissolved in the mother liquor with the form crystallization of associated complex for white arsenic and sulfuric acid.2. separate: at high temperature, the volatilization of the sulfur dioxide gas of formation is removed; In, under the low temperature, the elemental sulfur of formation is suspended on the mother liquor surface, by skimming or filtering removal.Behind the desulfuration, with the mother liquor crystallisation by cooling, decant or filter to isolate the white arsenic solid, mother liquor are handled to return through removal of impurities and are continued on for desulfurization.3. washing: white arsenic solid water or the sig water collected are washed, slough sulfuric acid and other impurity, water lotion uses through the arsenic removal cycle of treatment, will can enter next process behind the white arsenic solid filtering after the washing.If drying is handled, can obtain high-purity white arsenic product and (contain As
2O
3Reach 99.9%).4. reduction: with the white arsenic solid behind the washing filtering with contain Ya Xi (Sn (II)) ionic acidic solution and add reactor simultaneously, carry out reduction reaction, containing Ya Xi (Sn (II)) ionic acidic solution is the mixed aqueous solution of tin protochloride and hydrochloric acid, also can be stannous sulfate and vitriolic mixed aqueous solution, the consumption of stannous ion surpasses its chemical reaction metering, preferably 1.2-2 times of its chemical reaction metering, the concentration of acid is (1-12) N/L in the acidic solution, contain the acidic solution of stannous ion and the liquid-solid ratio of white arsenic and be (1.5-6) L: 1kg, mechanical stirring, temperature of reaction is 10 ℃-95 ℃, reaction times is 0.5-1.5 hours, reaction is after filtering separation can obtain elemental arsenic (As), and mother liquor can continue to serve as reductive agent through regeneration.5. wash, dry: the elemental arsenic that will from reaction mixture, collect, wash with water for several times, remove tin ion, after filtration, oven dry, can obtain high purity elemental arsenic product (contain As and can reach 99.9%).
The present invention since use sulfuric acid with arsenic sulfide (as As
2S
2, As
2S
3) in sulphur (as As
2S
3In S be-divalent) be oxidized to elemental sulfur or sulfurous gas (SO
2Middle S is+4 valencys) gas, and the arsenic in the arsenic sulfide is (as As
2S
3In As be+3 valencys) not oxidized, be converted into white arsenic (As
2O
3In As be+3 valencys) solid, and the white arsenic throw out can separate in a step with mother liquor, simultaneously, in containing the acidic solution of stannous ion, directly the white arsenic solid reduction is converted into elemental arsenic, rather than adopt chlorine that As (III) is oxidized to As (V) dissolving, and then be reduced to the approach of elemental arsenic, thereby whole process flow shortens greatly, the consumption of pharmaceutical chemicals, water consumption also greatly reduces, and equipment do not had corrosion, it is simple to have technology, consume few, cost is low, the efficient height, characteristics such as pollution-free, the elemental arsenic content of extraction can reach 99.9%.Simultaneously, this method can also be used to produce white arsenic (As
2O
3) product, the white arsenic throw out that generates behind the arsenic sulfide oxidation is separated with mother liquor, through washing, filtration, oven dry, can directly obtain to contain As
2O
3Reach 99.9% white arsenic product.
Embodiment 1: press processing step, get arsenic sulfide fine ore (containing As is 60～70%) 50g, add sulphuric acid soln and (contain H
2SO
4About 70%) 200ml, its liquid-solid ratio is: 4L: 1kg, temperature of reaction is 60 ℃, mechanical stirring was reacted 5 hours, and sulphur is the suspension elemental sulfur and is suspended in the mother liquor surface, the white arsenic throw out is collected from the mixture of reaction,, can be obtained the white arsenic solid and contain As through washing, filtration
2O
3Reach 99.6%; Get SnCl
2Consumption is 1.2 times of chemical reaction metering, HCl concentration is 1N/L, the mixed aqueous solution of tin protochloride and hydrochloric acid and the liquid-solid ratio of white arsenic are 3L: 1kg, mechanical stirring, temperature of reaction are 90 ℃, and the reaction times is 1.5 hours, the elemental arsenic throw out is collected from the mixture of reaction, through washing, filter, oven dry, can obtain elemental arsenic and contain As and reach 99.9%, carry arsenic rate 〉=97%.
Embodiment 2: press processing step, get arsenic sulfide fine ore 50g, add sulphuric acid soln and (contain H
2SO
4About 80%) 150ml, its liquid-solid ratio is: 3L: 1kg, temperature of reaction is 120 ℃, mechanical stirring was reacted 2.5 hours, and sulphur is molten and is suspended in the mother liquor surface, the white arsenic throw out is collected from reaction mixture,, can be obtained the white arsenic solid and contain As through washing, filtration
2O
3Reach 99.9%; Get SnCl
2Consumption is stoichiometric 1.4 times, HCl concentration is 12N/L, the mixed aqueous solution of tin protochloride and hydrochloric acid and the liquid-solid ratio of white arsenic are 2L: 1kg, mechanical stirring, temperature of reaction are 50 ℃, and the reaction times is 0.5 hour, the elemental arsenic throw out is collected from the mixture of reaction, through washing, filter, oven dry, can obtain elemental arsenic and contain As and reach 99.9%, carry arsenic rate 〉=98%.
Embodiment 3: press processing step, get arsenic sulfide fine ore 50g, add sulphuric acid soln and (contain H
2SO
4About 98%) 300ml, its liquid-solid ratio is 6L: 1kg, temperature of reaction is 170 ℃, mechanical stirring was reacted 1.5 hours, and sulphur is molten and is suspended in the mother liquor surface, the white arsenic throw out is collected from the mixture of reaction,, can be obtained the white arsenic solid and contain As through washing, filtration
2O
3Reach 99.9%; Get SnCl
2Consumption is stoichiometric 1.5 times, HCl concentration is 9N/L, the mixed aqueous solution of tin protochloride and hydrochloric acid and the liquid-solid ratio of white arsenic are 6L: 1kg, mechanical stirring, temperature of reaction are 30 ℃, and the reaction times is 0.5 hour, the elemental arsenic throw out is collected from the mixture of reaction, through washing, filter, oven dry, can obtain elemental arsenic and contain As and reach 99.9%, carry arsenic rate 〉=98%.
Embodiment 4: press processing step, get arsenic sulfide fine ore 50g, add sulphuric acid soln and (contain H
2SO
4About 90%) 200ml, its liquid-solid ratio is 4L: 1kg, 270 ℃ of temperature of reaction, mechanical stirring was reacted 0.5 hour, and sulphur is with sulfurous gas (SO
2) the gas form volatilization, the white arsenic throw out is collected from the mixture of reaction, through washing, filtration, can obtain the white arsenic solid and contain As
2O
3Reach 99.9%; Get SnCl
2Consumption is stoichiometric 1.3 times, HCl concentration is 6N/L, the mixed aqueous solution of tin protochloride and hydrochloric acid and the liquid-solid ratio of white arsenic are 4L: 1kg, mechanical stirring, temperature of reaction are 40 ℃, and the reaction times is 0.5 hour, the elemental arsenic throw out is collected from the mixture of reaction, through washing, filter, oven dry, can obtain elemental arsenic and contain As and reach 99.8%, carry arsenic rate 〉=98%.
Embodiment 5: press processing step, get arsenic sulfide fine ore 50g, add sulphuric acid soln (being oleum) 100ml, its liquid-solid ratio is 2L: 1kg, and temperature of reaction is 140 ℃, mechanical stirring, reacted 1 hour, sulphur is collected the white arsenic throw out with the volatilization of sulfurous gas form from the mixture of reaction, through washing, filtration, can obtain the white arsenic solid and contain As
2O
3Reach 99.9%; Get SnCl
2Consumption is stoichiometric 1.3 times, HCl concentration is 12N/L, the mixed aqueous solution of tin protochloride and hydrochloric acid and the liquid-solid ratio of white arsenic are 3L: 1kg, mechanical stirring, temperature of reaction are 30 ℃, and the reaction times is 1 hour, the elemental arsenic throw out is collected from the mixture of reaction, through washing, filter, oven dry, can obtain elemental arsenic and contain As and reach 99.9%, carry arsenic rate 〉=98%.
Embodiment 6: get the white arsenic that is made by the inventive method and (contain As
2O
3Be 99.9%) solid 40g, SnSO
4Consumption is stoichiometric 1.5 times, H in the reducing solution
2SO
4Concentration be 8N/L, the liquid-solid ratio of stannous sulfate and vitriolic mixed aqueous solution and white arsenic is 4L: 1kg, mechanical stirring, temperature of reaction is 70 ℃, reaction times is 1 hour, the elemental arsenic throw out is collected from the mixture of reaction, through washing, filtration, oven dry, can obtain elemental arsenic and contain As and reach 99.8%, carry arsenic rate 〉=98%.
Claims (7)
1. a method of wet-extraction for arsenic is characterized in that adopting sulfuric acid (H
2SO
4) the molten arsenic sulfide (As that soaks of solution
2S
2Or As
2S
3), vitriolic concentration 〉=70%, the liquid-solid ratio of sulfuric acid and arsenic sulfide material is (1.5-6) L: 1kg, the temperature of sulfuric acid and the reaction of arsenic sulfide is 40 ℃-280 ℃, mechanical stirring, reaction times is 0.5-5 hours, after arsenic sulfide decomposes, generate the white arsenic solid, sulphur is along with the rising of reaction control temperature, respectively with the suspension elemental sulfur, molten elemental sulfur or sulfur dioxide gas form are separated from arsenic sulfide, the white arsenic throw out that reaction generates is collected from the mixture of reaction, through washing, filter, obtain the white arsenic solid, the white arsenic solid that obtains is further reduced with containing Ya Xi (Sn (II)) ionic acidic solution, the consumption of stannous ion surpasses its chemical reaction metering, the concentration of acid is (1-12) N/L in the acidic solution, contain the acidic solution of stannous ion and the liquid-solid ratio of white arsenic and be (1.5-6) L: 1kg, mechanical stirring, temperature of reaction is 10 ℃-95 ℃, and the reaction times is 0.5-1.5 hours, after the reaction, from reaction mixture, collect elemental arsenic, through washing, filter, oven dry gets final product.
2. a kind of method of wet-extraction for arsenic according to claim 1 is characterized in that sulfuric acid is oleum.
3. according to claim 1 or 2 described a kind of method of wet-extraction for arsenic, the consumption that it is characterized in that stannous ion is 1.2-2 times of its chemical reaction metering.
4. according to claim 1 or 2 described a kind of method of wet-extraction for arsenic, it is characterized in that containing Ya Xi (Sn (II)) ionic acidic solution is tin protochloride (SnCl
2) and the mixed aqueous solution of hydrochloric acid (HCl).
5. a kind of method of wet-extraction for arsenic according to claim 3, it is characterized in that containing Ya Xi (Sn (II)) ionic acidic solution is tin protochloride (SnCl
2) and the mixed aqueous solution of hydrochloric acid (HCl).
6. according to claim 1 or 2 described a kind of method of wet-extraction for arsenic, it is characterized in that containing Ya Xi (Sn (II)) ionic acidic solution is stannous sulfate (SnSO
4) and sulfuric acid (H
2SO
4) mixed aqueous solution.
7. a kind of method of wet-extraction for arsenic according to claim 3, it is characterized in that containing Ya Xi (Sn (II)) ionic acidic solution is stannous sulfate (SnSO
4) and sulfuric acid (H
2SO
4) mixed aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94110976 CN1120018A (en) | 1994-05-07 | 1994-05-07 | Method of wet-extraction for arsenic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94110976 CN1120018A (en) | 1994-05-07 | 1994-05-07 | Method of wet-extraction for arsenic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1120018A true CN1120018A (en) | 1996-04-10 |
Family
ID=5034890
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94110976 Pending CN1120018A (en) | 1994-05-07 | 1994-05-07 | Method of wet-extraction for arsenic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1120018A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100355918C (en) * | 2006-08-24 | 2007-12-19 | 浙江大学 | Preparation method and use of single, compound arsenic with bio-effect |
| CN100406595C (en) * | 2006-08-24 | 2008-07-30 | 浙江大学 | Preparation method and use of bioactive sing-compound arsenic |
| CN101587072B (en) * | 2009-06-09 | 2010-12-29 | 扬州高能新材料有限公司 | Method of detecting Se in high-purity arsenic trioxide |
| CN101619398B (en) * | 2009-07-27 | 2011-07-27 | 昭通天元实业有限责任公司 | Method for extracting arsenic from pyrite cinder |
| CN111233034A (en) * | 2020-03-24 | 2020-06-05 | 中南大学 | Method for preparing yolk crystal by hydrothermal method |
| CN115354342A (en) * | 2022-10-20 | 2022-11-18 | 矿冶科技集团有限公司 | Method for preparing simple substance arsenic by diaphragm electrolysis |
-
1994
- 1994-05-07 CN CN 94110976 patent/CN1120018A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100355918C (en) * | 2006-08-24 | 2007-12-19 | 浙江大学 | Preparation method and use of single, compound arsenic with bio-effect |
| CN100406595C (en) * | 2006-08-24 | 2008-07-30 | 浙江大学 | Preparation method and use of bioactive sing-compound arsenic |
| CN101587072B (en) * | 2009-06-09 | 2010-12-29 | 扬州高能新材料有限公司 | Method of detecting Se in high-purity arsenic trioxide |
| CN101619398B (en) * | 2009-07-27 | 2011-07-27 | 昭通天元实业有限责任公司 | Method for extracting arsenic from pyrite cinder |
| CN111233034A (en) * | 2020-03-24 | 2020-06-05 | 中南大学 | Method for preparing yolk crystal by hydrothermal method |
| CN115354342A (en) * | 2022-10-20 | 2022-11-18 | 矿冶科技集团有限公司 | Method for preparing simple substance arsenic by diaphragm electrolysis |
| CN115354342B (en) * | 2022-10-20 | 2023-02-07 | 矿冶科技集团有限公司 | Method for preparing simple substance arsenic by diaphragm electrolysis |
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