CN103964601A - Method for treating arsenic-containing industrial wastewater - Google Patents
Method for treating arsenic-containing industrial wastewater Download PDFInfo
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- CN103964601A CN103964601A CN201310047867.8A CN201310047867A CN103964601A CN 103964601 A CN103964601 A CN 103964601A CN 201310047867 A CN201310047867 A CN 201310047867A CN 103964601 A CN103964601 A CN 103964601A
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Abstract
The invention belongs to the wet metallurgy and environmental protection technical fields, and particularly, discloses a method for treating arsenic in arsenic-containing industrial wastewater. Under a condition of high temperature, an iron solution is slowly added into the arsenic-containing industrial wastewater, arsenic in the wastewater forms a stable scorodite crystal (FeAsO4.2H2O), and thus arsenic in the wastewater is removed. The method is simple in process, can obtain the stable arsenic-containing solid waste, and reduces secondary pollution caused to the environment.
Description
Technical field
The invention belongs to hydrometallurgy and environmental technology field, specifically a kind of method of adsorptive treatment of arsenic-containing industrial wasterwater.
Background technology
Arsenic is a kind of poisonous element, mainly exist with the form of sulfide and association in other metals as: in the mineral that gold, copper, lead, nickel, cobalt, zinc etc. form, the arsenic-containing waste water of a large amount of high density that can generation in nonferrous smelting and sulfuric acid industry flue gas acid preparing process.Arsenic in these waste water must be got rid of with stable compound, and waste water could discharge.Therefore in, non-ferrous metal metallurgy research field, the removal of arsenic and technique for fixing are the focuses of research always.
At present, the treatment technology of arsenic-containing waste water mainly contains: scorodite method, lime method, lime-iron salt method.Lime-iron salt method by adding molysite in arsenic-containing waste water, make in arsenic-containing waste water arsenic with the form Precipitation of arsenic iron co-precipitation, the method suitable treatment containing lower concentration containing arsenic arsenic waste water, have advantages of that cost is low, technique simple, arsenic removal efficiency is high, but conventionally need to use in the method molysite more than iron arsenic mol ratio 4:1, exist waste residue amount large, be unfavorable for the shortcoming of ultimate disposal or the processing of waste residue.When arsenic in waste water content is very high, iron level is lower simultaneously, it is the method for generally taking now that arsenic is removed with the form of crystal form scorodite.Have arsenic content high (>30%) using this as solid arsenic carrier, need that iron amount is little, crystallization degree is high, easily clarification, filters and separates, compared with other contain arsenic carrier, has good stability, the advantages such as lower storage expense.At present, for the existing many reports of synthetic method of scorodite, still, mostly severe reaction conditions, needs the strict degree of supersaturation of controlling.For example: generate scorodite at the lower heating of High Temperature High Pressure (150 DEG C) arsenic ferrous solution; Normal pressure (95 DEG C) is lower generates scorodite, slow oxidation ferrous iron (chemical oxidation or microbiological oxidation) generation scorodite by slowly improving arsenic ferrous solution pH, first generate amorphous ferric arsenate transforms to scorodite under hot conditions again.These scorodite methods are arsenic ferrous solution and are pre-mixed.
Therefore the new treatment process of, exploring, study arsenic in the arsenic-containing waste water of easy, easy handling is the problem that must face.
Summary of the invention
The object of the invention is to provide a kind of method of adsorptive treatment of arsenic-containing industrial wasterwater.
For achieving the above object, the present invention adopts technical scheme to be:
A method for adsorptive treatment of arsenic-containing industrial wasterwater under hot conditions, slowly adds ferrous solution in waste water containing arsenic, and the arsenic in waste water is formed to stable scorodite crystal (FeAsO
42H
2, and then remove the arsenic in waste water O).
Further, under 70-95 DEG C, the condition of pH0.8-2.0, in waste water containing arsenic, slowly drip ferric iron solution or ferric iron and ferrous iron mixing solutions, reaction 5-8 hour, forms stable scorodite crystal (FeAsO by the arsenic in waste water
42H
2o), then solid-liquid separation obtains the precipitation of scorodite; And then remove the arsenic in waste water.
Described waste water containing arsenic be after dissolving containing arsenic waste solution or pyrometallurgical smelting flue dust of producing containing arsenic waste solution, sulfuric acid industry of producing of copper, lead, zinc, nickel, uranium, gold and the non-ferrous metal hydrometallurgy such as silver-colored containing arsenic waste solution; Wherein arsenic content is more than 1g/L.
Describedly in waste water containing arsenic, add ferric iron solution, wherein the mol ratio of ferric iron and arsenic is: 0.8-2:1;
Or describedly in waste water containing arsenic, add ferric iron and ferrous iron mixing solutions, wherein the mol ratio of ferric iron and arsenic is: 0.8-2:1, the mol ratio of ferrous iron and arsenic is: 0-1:1.
Adopt hydrochloric acid, it is 0.8-2.0 that waste water containing arsenic is adjusted to pH by sulfuric acid, nitric acid, calcium oxide or sodium hydroxide.
Described ferrous solution is one or more the combination in ferric sulfate, iron(ic) chloride, iron nitrate, polymerization iron, ferrous sulfate, iron protochloride and Iron nitrate; And ferrous solution was added dropwise to complete in 2-6 hour.
The advantage that the present invention has is:
The present invention is by under high temperature (70-95 DEG C) condition, in arsenic containing solution, slowly add ferric iron or ferric iron and ferrous iron mixing solutions, form stable scorodite crystal and remove the arsenic in waste water in the Fe/As mol ratio compared with low and in certain pH value condition, technique of the present invention is simple, easy handling, waste residue generation is little, stable, causes the risk of secondary pollution little to environment.
Processing method easy handling of the present invention, wide accommodation, reduces processing cost, reduces waste residue output, obtains stablizing waste residue, prevents the secondary pollution of arsenic, and avoids arsenic dispersion and pollution on stream.The present invention is guaranteeing that arsenic-containing waste water reaches under the prerequisite of wastewater discharge standard after treatment, the minimizing that realizes waste residue of maximum possible, stabilization, innoxious processing.
Brief description of the drawings
Fig. 1 is the XRD figure of the scorodite that obtains of the embodiment of the present invention;
Fig. 2 is the SEM figure of the scorodite that obtains of the embodiment of the present invention.
Embodiment:
The method of the waste water arsenic removal relating in the present invention is described by specific embodiment below, and can form limitation of the present invention.
As one embodiment of the present invention, comprise following process: regulate between the pH0.8-2.0 of arsenic solution, and be heated to preset temperature (70-95 DEG C), be the mixing ferrous solution that 0.8-2, ferrous iron arsenic mol ratio are 0-1 according to the content configuration ferric iron arsenic mol ratio of arsenic in waste water, and regulate pH0.8-2.0, in arsenic solution, slowly drip and mix ferrous solution, control time for adding is 2-6 hour, dropwises follow-up continuation of insurance temperature more than 2 hours.After reacting completely, cool to room temperature, solid-liquid separation, the scorodite that obtains crystallization precipitates.
Embodiment 1:
By Na
3asO
4.12H
2o is dissolved in 100ml distilled water, is made into the solution containing As:10g/L, adds the vitriol oil to regulate and control pH1.1 under room temperature; Under mechanical stirring condition, (200rpm) is heated to 95 DEG C; Separately by Fe
2(SO
4)
3.xH
2o and Fe SO
4.7H
2o is dissolved in 100ml distilled water simultaneously, is made into containing Fe (III): the mixing ferrous solution of 7.5g/L, Fe (II): 3.75g/L.With the speed of 0.4ml/min, mixing ferrous solution is joined in the middle of arsenic solution with peristaltic pump, within approximately 4 hours, drip off, drip off rear continuation keep 95 DEG C 4 hours, reaction finishes rear cool to room temperature, solid-liquid separation, obtain the precipitation of stable scorodite crystal, the X-ray diffraction analysis of this precipitation and scanning electron microscope analysis picture are respectively as depicted in figs. 1 and 2.
Embodiment 2:
By Na
3asO
4.12H
2o is dissolved in 100ml distilled water, is made into the solution containing As:50g/L, under room temperature, adds the vitriol oil to be adjusted to pH0.8; Under mechanical stirring condition, (200rpm) is heated to 70 DEG C; Separately by Fe
2(SO
4)
3.xH
2o and Fe SO
4.7H
2o is dissolved in 100ml distilled water simultaneously, is made into containing Fe (III): the mixing ferrous solution of 28g/L, Fe (II): 14g/L.With the speed of 0.3ml/min, mixing ferrous solution is joined in the middle of arsenic solution with peristaltic pump, within approximately 6 hours, drips off, drip off rear continuation keep 95 DEG C 2 hours, reaction finishes rear cool to room temperature, solid-liquid separation obtains the precipitation of stable scorodite crystal.
Embodiment 3:
By Na
3asO
4.12H
2o is dissolved in 100ml distilled water, is made into the solution containing As:1g/L, under room temperature, adds the vitriol oil to be adjusted to pH2.0; Under mechanical stirring condition, (200rpm) is heated to 90 DEG C; Separately by Fe
2(SO
4)
3.xH
2o and Fe SO
4.7H
2o is dissolved in 100ml distilled water simultaneously, is made into containing Fe (III): the mixing ferrous solution of 0.75g/L, Fe (II): 0.4g/L.With the speed of 0.8ml/min, mixing ferrous solution is joined in the middle of arsenic solution with peristaltic pump, within approximately 2 hours, drips off, drip off rear continuation keep 95 DEG C 6 hours, reaction finishes rear cool to room temperature, solid-liquid separation obtains the precipitation of stable scorodite crystal.
Embodiment 4:
By Na
3asO
4.12H
2o is dissolved in 100ml distilled water, is made into the solution containing As:10g/L, under room temperature, adds the vitriol oil to be adjusted to pH1.5; Under mechanical stirring condition, (200rpm) is heated to 95 DEG C; Separately by Fe
2(SO
4)
3.xH
2o and Fe SO
4.7H
2o is dissolved in 100ml distilled water simultaneously, is made into containing Fe (III): the mixing ferrous solution of 7.5g/L, Fe (II): 1.5g/L.With the speed of 0.5ml/min, mixing ferrous solution is joined in the middle of arsenic solution with peristaltic pump, within approximately 3.5 hours, drips off, drip off rear continuation keep 95 DEG C 5 hours, reaction finishes rear cool to room temperature, solid-liquid separation obtains the precipitation of stable scorodite crystal.
Embodiment 5:
By Na
3asO
4.12H
2o is dissolved in 100ml distilled water, is made into the solution containing As:10g/L, under room temperature, adds the vitriol oil to be adjusted to pH1.5; Under mechanical stirring condition, (200rpm) is heated to 90 DEG C; Separately by Fe
2(SO
4)
3.xH
2o and Fe SO
4.7H
2o is dissolved in 100ml distilled water simultaneously, is made into containing Fe (III): the mixing ferrous solution of 8g/L, Fe (II): 4g/L.With the speed of 0.5ml/min, mixing ferrous solution is joined in the middle of arsenic solution with peristaltic pump, within approximately 3.5 hours, drips off, drip off rear continuation keep 95 DEG C 5 hours, reaction finishes rear cool to room temperature, solid-liquid separation obtains the precipitation of stable scorodite crystal.
Embodiment 6:
By Na
3asO
4.12H
2o is dissolved in 100ml distilled water, is made into the solution containing As:10g/L, under room temperature, adds the vitriol oil to be adjusted to pH1.5; Under mechanical stirring condition, (200rpm) is heated to 95 DEG C; Separately by Fe
2(SO
4)
3.xH
2o is dissolved in 100ml distilled water, is made into containing Fe (III): the solution of 7.5g/L.With the speed of 0.5ml/min, ferrous solution is joined in the middle of arsenic solution with peristaltic pump, within approximately 3.5 hours, drips off, drip off rear continuation keep 95 DEG C 5 hours, reaction finishes rear cool to room temperature, solid-liquid separation obtains the precipitation of stable scorodite crystal.
Respectively the As content before and after dirty acid treatment in embodiment 1-6 is measured, its measurement result is as shown in table 1.
As testing method: As concentration adopts atomic fluorescence spectrophotometer-hydride generator method to measure, and after 10 samples of every mensuration, atomic fluorescence spectrophotometer (AFS-2202E) is carried out to single-point verification.
As content before and after table 1 wastewater treatment
As can be seen from the above table: after application the present invention processes, the arsenic overwhelming majority in waste water removes with scorodite form precipitation, and clearance is all in 95% left and right.
By GB/15085.3.2007 and US EPA(TCLP) the scorodite precipitation that obtains after respectively arsenic containing solution in embodiment 1-6 being processed of Hazardous wastes Leaching testing method in stability measure, its measurement result is as shown in table 2.
The stability of table 2 scorodite
As can be seen from the above table: the precipitation obtaining after application the present invention processes can be by the Hazardous wastes Leaching standard of GB/5085.3.2007 and US EPA.
As can be seen from the above results: the present invention by lower Fe/As mol ratio, 70-95 DEG C and under pH0.8-2 condition by slowly drip ferric iron and ferrous mixing solutions in arsenic solution, generate good stability scorodite crystal and remove the arsenic in solution, obtain stablely containing arsenic solid waste, can reduce the secondary pollution that it causes environment.
Claims (6)
1. a method for adsorptive treatment of arsenic-containing industrial wasterwater, is characterized in that: under hot conditions, in waste water containing arsenic, slowly add ferrous solution, the arsenic in waste water is formed to stable scorodite crystal (FeAsO
42H
2, and then remove the arsenic in waste water O).
2. by the method for adsorptive treatment of arsenic-containing industrial wasterwater claimed in claim 1, it is characterized in that: under 70-95 DEG C, the condition of pH0.8-2.0, in waste water containing arsenic, slowly drip ferric iron solution or ferric iron and ferrous iron mixing solutions, reaction 5-8 hour, forms stable scorodite crystal (FeAsO by the arsenic in waste water
42H
2o), then solid-liquid separation obtains the precipitation of scorodite; And then remove the arsenic in waste water.
3. the method for pressing adsorptive treatment of arsenic-containing industrial wasterwater claimed in claim 1, is characterized in that: described waste water containing arsenic is the arsenic waste solution that contains after arsenic waste solution or the dissolving of pyrometallurgical smelting flue dust that contains containing arsenic waste solution, sulfuric acid industry generation of non-ferrous metal hydrometallurgy generation.
4. by the method for adsorptive treatment of arsenic-containing industrial wasterwater claimed in claim 1, it is characterized in that: describedly in waste water containing arsenic, add ferric iron solution, wherein the mol ratio of ferric iron and arsenic is: 0.8-2:1;
Or describedly in waste water containing arsenic, add ferric iron and ferrous iron mixing solutions, wherein the mol ratio of ferric iron and arsenic is: 0.8-2:1, the mol ratio of ferrous iron and arsenic is: 0-1:1.
5. by the method for adsorptive treatment of arsenic-containing industrial wasterwater claimed in claim 1, it is characterized in that: adopt hydrochloric acid, it is 0.8-2.0 that waste water containing arsenic is adjusted to pH by sulfuric acid, nitric acid, calcium oxide or sodium hydroxide.
6. by the method for adsorptive treatment of arsenic-containing industrial wasterwater claimed in claim 1, it is characterized in that: described ferrous solution is one or more the combination in ferric sulfate, iron(ic) chloride, iron nitrate, polymerization iron, ferrous sulfate, iron protochloride and Iron nitrate; And ferrous solution was added dropwise to complete in 2-6 hour.
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| CN104525555A (en) * | 2014-12-29 | 2015-04-22 | 中国电建集团中南勘测设计研究院有限公司 | Stabilizing treatment method and equipment for arsenic slag |
| CN104609573A (en) * | 2015-02-03 | 2015-05-13 | 中国科学院过程工程研究所 | Method for treating acid waste water containing arsenic |
| CN105060431A (en) * | 2015-07-31 | 2015-11-18 | 中南大学 | Treatment method for high arsenic contaminated acid wastewater |
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