CN103204543A - Synthetic method for preparing arsenic trioxide through using arsenic-containing wastewater - Google Patents
Synthetic method for preparing arsenic trioxide through using arsenic-containing wastewater Download PDFInfo
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- CN103204543A CN103204543A CN2012105473534A CN201210547353A CN103204543A CN 103204543 A CN103204543 A CN 103204543A CN 2012105473534 A CN2012105473534 A CN 2012105473534A CN 201210547353 A CN201210547353 A CN 201210547353A CN 103204543 A CN103204543 A CN 103204543A
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Abstract
The invention discloses a synthetic method for preparing arsenic trioxide through using 3-nitro-4-hydroxyphenylarsonic acid wastewater as a raw material. The method comprises the following steps: carrying out pretreatments comprising pH value adjustment, cartridge filtration and the like of arsenic-containing wastewater, allowing the obtained pretreated wastewater to enter the feed liquid cycle tank of a membrane experiment apparatus, and intercepting high-content arsenic-containing wastewater; adjusting the pH value of the obtained high-content arsenic-containing wastewater to 10-12 by using an alkali, adding a reducing agent A to reduce pentavalent arsenic to trivalent arsenic, and carrying out a reaction at 40-80DEG C for 6-10h; allowing a tail gas generated in the reaction to go through a reaction absorption tower for absorbing the tail gas; and concentrating a reaction liquid obtained after the reaction by adopting a triple effect concentrator to a volume being 1/4 of an original volume, adjusting the pH of the obtained concentrate by using an acid, stirring for slowly cooling to 40DEG C for crystallization, and filtering to obtain arsenic trioxide powder. The synthetic method for preparing arsenic trioxide through using wastewater as a raw material has the advantages of simple flow, low raw material investment, low cost, no generation of wastes, and environmental protection.
Description
Technical field
The invention belongs to chemical field, specifically is the synthetic method that a kind of arsenic-containing waste water prepares white arsenic.
Background technology
Arsenic and compound grievous injury human health thereof are defined as first kind carcinogens by U.S. disease Disease Control and Prevention Center and the international research institution that hinders, mainly are detrimental to health by the drinking-water approach.Therefore, a plurality of countries such as China, the U.S., West Europe, Japan classify arsenic as one of water pollutant of preferential control.In recent years, along with the fast development of industries such as mining, metallurgy, pottery, crystal glass, leather, agricultural chemicals, the arsenic-containing waste water amount increases day by day, and arsenic increases with pollution day by day to the discharging of environment.
Handling the arsenic-containing waste water main method has in chemical method, extraction process, embrane method, ion exchange method, absorption method, the lime and method such as molysite coagulant sedimentation.Extraction process, ion exchange method, absorption method are mainly for the treatment of the lower concentration arsenic-containing waste water, but processing cost is higher, and industrial application is less.Wherein in the lime and the molysite coagulant sedimentation handle and can not reclaim valuable metal, produce a large amount of arsenic-containing waste residues and need security landfill, be the hidden danger that has secondary pollution,
Arsenic in the waste water is to exist with organoarsenic and two kinds of forms of inorganic arsenic, emphasis of the present invention is handled inorganic arsenic, owing to contain arsenic concentration height, qualified discharge processing costs height, country forbids strictly its direct discharging, containing the arsenic contamination thing must could discharge behind the governance for reaching standard, and the strictness monitoring is carried out in its source.
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Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing arsenic-containing waste water to prepare white arsenic, make arsenic in the waste water effectively be reclaimed and utilize.
The technical solution used in the present invention is:
A kind of is the method for feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, may further comprise the steps: waste water enters film experimental installation feed liquid circulation tank after overregulating pre-treatment such as pH value, security personnel's filtration; Experimental installation is the periodical operation system, trapped fluid all returns the feed liquid circulation tank, by pump discharge valve and recycle valve control circular flow and feed pressure, film sees through liquid and discharges system with flexible pipe, in the feed liquid circulation tank, constantly replenish pretreated filtrate, the feed liquid circulation tank is full of all the time, till the experiment feed liquid adds, hold back the high-content arsenic-containing waste water, adopt nanofiltration as typical membrane sepn process, the molecular weight cut-off scope of nanofiltration is 150～1000Dalton, separate small-molecule substance from waste liquid, remove sodium-chlor and solvent simultaneously, the described arsenic-containing waste water of holding back by membrane separation technique is waste water A, waste water A is the film trapped fluid, concentration 15000～45000 mg/L; It is 10～12 that described waste water A is regulated PH with alkali, add reductive agent A pentavalent arsenic is reduced to trivalent arsenic, temperature of reaction control is at 40～80 ℃, 6～10 hours reaction times, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, after reaction finishes, reaction solution adopts the triple effect thickener that it is concentrated, concentrated solution is concentrated into 1/4 of cumulative volume, and concentrated solution is regulated pH value with acid, stirs to slowly cool to 40 ℃ of crystallizations filtrations, obtain filter cake A and filtrate A, described filtrate A recycles, described filter cake A, by dry the white arsenic dry product.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that the waste water of described 3-nitro-4-phenol-arsonic acid is from the waste water that produces in 3-nitro-4-phenol-arsonic acid production process; Comprise inorganic arsine and organoarsenic in the described waste water, organic arsine and inorganic arsenic total content are 1000～6000mg/L; Described inorganic arsine comprises trivalent arsenic and pentavalent arsenic, and the concentration of trivalent arsenic and pentavalent arsenic is 5000～15000 mg/L in the described waste water; The described original pH value of waste water that contains inorganic arsenic is 0.5～2.5.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described waste water must carry out pre-treatment earlier the original waste water pH value is adjusted to 5～8, the control of the pH value of feed liquid is 7～8; Described waste water must filter to guarantee that water filtration precision and protective membrane filtering element are not subjected to the damage of large particulate matter through security personnel, and the process membrane flux described in the membrane sepn process is 18～20LMH; Concentration rate control is 2.8～3.3 in the membrane sepn process; Feed temperature described in the membrane sepn treating processes is 40～50 ℃ and is advisable.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that the arsenic in the described arsenic-containing waste water is to exist with the pentavalent arsenic form more than 98%.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described reductive agent A is hydrazine hydrate, formic acid, sodium bisulfite or S-WAT, sulfurous gas.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that the ratio of the amount of substance of arsenic content in the described arsenic-containing waste water and reductive agent A is 1:3～5.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described alkali is oxyhydroxide and oxide compound and the aqueous solution thereof of the oxyhydroxide of metal and oxide compound, alkaline-earth metal, is preferably yellow soda ash or sodium hydroxide or its solution.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described concentrated solution regulates pH value with acid, described acid is preferably sulphuric acid soln, described concentrated solution is regulated pH value and is preferably 2.5～3.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described filtrate A recycles, turn back to waste water A through sorbent treatment and prepare white arsenic, described sorbent material is for being the various acticarbons of raw material or metal, nonmetal oxide class sorbent material with the carbonaceous, and described sorbent material is preferably silica gel, activated alumina, gac, molecular sieve.
Described a kind of be the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that reaction solution adopts the triple effect thickener that it is concentrated.
Table 1 membrane separation technique is held back the operating parameters of high-content arsenic-containing waste water:
| The experiment lot number | 01 | 02 | 03 | 04 | 05 | 06 |
| Feed liquid PH | 5 | 7 | 8 | 8 | 7 | 6 |
| Feeding liquid arsenic content mg/l | 7918 | 8946 | 8910 | 11183 | 12808 | 9958 |
| Feeding liquid sodium-chlor % | 13.6 | 12.5 | 14.9 | 15.4 | 16.2 | 15.1 |
| See through liquid arsenic content mg/l | 541 | 405 | 313 | 480 | 552 | 982 |
| See through liquid sodium-chlor % | 14.4 | 13.2 | 15.4 | 15.7 | 16.4 | 15.5 |
| Concentrated solution arsenic content mg/l | 25338 | 29523 | 27622 | 31311 | 33302 | 30869 |
| Process arsenic yield % | 95.2 | 96.8 | 97.6 | 97.2 | 97.3 | 93.1 |
| Process membrane flux LMH | 39.5 | 20.6 | 18.4 | 18.8 | 20.3 | 26.4 |
| Process feed temperature ℃ | 42-52 | 47-50 | 45-48 | 41-48 | 45-47 | 42-49 |
| Concentration rate doubly | 3.2 | 3.3 | 3.1 | 2.8 | 2.6 | 3.1 |
| Membrane flux recovery rate % | 95 | 94 | 89 | 99 | 110 | 95 |
The invention provides a kind of product (white arsenic) that can carry out reaction treatment and system to the waste water that wherein contains inorganic arsenic, then can reduce pollutant emission, turn waste into wealth, realize that business economic benefit and social benefit develop simultaneously.Synthetic method flow process of the present invention is simple, and raw material drops into low, and cost is low, does not produce refuse, environmental friendliness.
Description of drawings
Fig. 1 is the infared spectrum of product white arsenic of the present invention.
Embodiment
Embodiment 1:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is 15000mg/L, the waste water of PH=7, regulate PH to 12.0 with alkali, stirred 30 minutes, slowly add reductive agent hydrazine hydrate 100kg under the whipped state, temperature control is at 60 ℃, reacted 6 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, sampling detects pentavalent arsenic content and is down to 0.2% by original 1.5%, and after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated, concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 2.5, stir, slowly cool to 40 ℃ of crystallizations, filter, filtrate is recycled, filter cake is white arsenic 90kg, detection level 94.5%.
Embodiment 2:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is the waste water of 45000mg/L, PH=8, regulate PH to 10.0 with alkali, stirred 30 minutes, slowly add reductive agent hydrazine hydrate 200kg under the whipped state, temperature control is at 80 ℃, reacted 10 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, and sampling detects pentavalent arsenic content and is down to 0.3% by original 4.5%, after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated.Concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 3.0, stirs, slowly cools to 40 ℃ of crystallizations, filters, and filtrate is recycled, and filter cake is white arsenic 282kg, detection level 98.2%.
Embodiment 3:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is the waste water of 15000mg/L, PH=7, regulate PH to 12.0 with alkali, stirred 30 minutes, slowly add reductive agent formic acid 100kg under the whipped state, temperature control is at 60 ℃, reacted 6 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, and sampling detects pentavalent arsenic content and is down to 0.2% by original 1.5%, after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated.Concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 2.5, stirs, slowly cools to 40 ℃ of crystallizations, filters, and filtrate is recycled, and filter cake is white arsenic 87kg, detection level 98.6%.
Embodiment 4:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is the waste water of 45000mg/L, PH=8, regulate PH to 10.0 with alkali, stirred 30 minutes, slowly add reductive agent formic acid 200kg under the whipped state, temperature control is at 80 ℃, reacted 10 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, and sampling detects pentavalent arsenic content and is down to 0.3% by original 4.5%, after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated.Concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 3.0, stirs, slowly cools to 40 ℃ of crystallizations, filters, and filtrate is recycled, and filter cake is white arsenic 287kg, detection level 96.5%.
Embodiment 5:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is the waste water of 15000mg/L, PH=7, regulate PH to 12.0 with alkali, stirred 30 minutes, slowly add reductive agent sodium bisulfite 210kg under the whipped state, temperature control is at 60 ℃, reacted 6 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, and sampling detects pentavalent arsenic content and is down to 0.05% by original 1.5%, after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated.Concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 2.5, stirs, slowly cools to 40 ℃ of crystallizations, filters, and filtrate is recycled, and filter cake is white arsenic 98kg, detection level 97.3%.
Embodiment 6:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is the waste water of 45000mg/L, PH=8, regulate PH to 10.0 with alkali, stirred 30 minutes, slowly add reductive agent sodium bisulfite 378kg under the whipped state, temperature control is at 80 ℃, reacted 10 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, and sampling detects pentavalent arsenic content and is down to 0.08% by original 4.5%, after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated.Concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 3.0, stirs, slowly cools to 40 ℃ of crystallizations, filters, and filtrate is recycled, and filter cake is white arsenic 303kg, detection level 96.2%.
Embodiment 7:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is the waste water of 15000mg/L, PH=8, regulate PH to 12.0 with alkali, stirred 30 minutes, slowly add reductive agent S-WAT 153kg under the whipped state, temperature control is at 80 ℃, reacted 10 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, and sampling detects pentavalent arsenic content and is down to 0.2% by original 1.5%, after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated.Concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 3.0, stirs, slowly cools to 40 ℃ of crystallizations, filters, and filtrate is recycled, and filter cake is white arsenic 80kg, detection level 98.4%.
Embodiment 8:
Get the arsenic-containing waste water that 5000L holds back by membrane separation technique, arsenic content is the waste water of 45000mg/L, PH=8, regulate PH to 12.0 with alkali, stirred 30 minutes, slowly add reductive agent sulfurous gas 192kg under the whipped state, temperature control is at 80 ℃, reacted 10 hours, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, and sampling detects pentavalent arsenic content and is down to 0.4% by original 1.5%, after reaction finished, reaction solution adopted the triple effect thickener that it is concentrated.Concentrated solution is concentrated into the 1/4 usefulness acid of cumulative volume and regulates PH to 3.0, stirs, slowly cools to 40 ℃ of crystallizations, filters, and filtrate is recycled, and filter cake is white arsenic 230kg, detection level 94.3%.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all is included within protection scope of the present invention.
Claims (10)
1. one kind is the method for feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, may further comprise the steps: waste water enters film experimental installation feed liquid circulation tank after overregulating pre-treatment such as pH value, security personnel's filtration; Experimental installation is the periodical operation system, trapped fluid all returns the feed liquid circulation tank, by pump discharge valve and recycle valve control circular flow and feed pressure, film sees through liquid and discharges system with flexible pipe, in the feed liquid circulation tank, constantly replenish pretreated filtrate, the feed liquid circulation tank is full of all the time, till the experiment feed liquid adds, hold back the high-content arsenic-containing waste water, adopt nanofiltration as typical membrane sepn process, the molecular weight cut-off scope of nanofiltration is 150～1000Dalton, separate small-molecule substance from waste liquid, remove sodium-chlor and solvent simultaneously, the described arsenic-containing waste water of holding back by membrane separation technique is waste water A, waste water A is the film trapped fluid, concentration 15000～45000 mg/L; It is 10～12 that described waste water A is regulated PH with alkali, add reductive agent A pentavalent arsenic is reduced to trivalent arsenic, temperature of reaction control is at 40～80 ℃, 6～10 hours reaction times, the tail gas that produces during reaction absorbs tail gas through the reaction absorption tower, after reaction finishes, reaction solution adopts the triple effect thickener that it is concentrated, concentrated solution is concentrated into 1/4 of cumulative volume, and concentrated solution is regulated pH value with acid, stirs to slowly cool to 40 ℃ of crystallizations filtrations, obtain filter cake A and filtrate A, described filtrate A recycles, described filter cake A, by dry the white arsenic dry product.
2. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that the waste water of described 3-nitro-4-phenol-arsonic acid is from the waste water that produces in 3-nitro-4-phenol-arsonic acid production process; Comprise inorganic arsine and organoarsenic in the described waste water, organic arsine and inorganic arsenic total content are 1000～6000mg/L; Described inorganic arsine comprises trivalent arsenic and pentavalent arsenic, and the concentration of trivalent arsenic and pentavalent arsenic is 5000～15000 mg/L in the described waste water; The described original pH value of waste water that contains inorganic arsenic is 0.5～2.5.
3. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described waste water must carry out pre-treatment earlier the original waste water pH value is adjusted to 5～8, and the pH value control of feed liquid is 7～8; Described waste water must filter to guarantee that water filtration precision and protective membrane filtering element are not subjected to the damage of large particulate matter through security personnel, and the process membrane flux described in the membrane sepn process is 18～20LMH; Concentration rate control is 2.8～3.3 in the membrane sepn process; Feed temperature described in the membrane sepn treating processes is 40～50 ℃ and is advisable.
4. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that the arsenic in the described arsenic-containing waste water is to exist with the pentavalent arsenic form more than 98%.
5. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described reductive agent A is hydrazine hydrate, formic acid, sodium bisulfite or S-WAT, sulfurous gas.
6. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that the ratio of the amount of substance of arsenic content in the described arsenic-containing waste water and reductive agent A is 1:3～5.
7. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described alkali is oxyhydroxide and oxide compound and the aqueous solution thereof of the oxyhydroxide of metal and oxide compound, alkaline-earth metal, is preferably yellow soda ash or sodium hydroxide or its solution.
8. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described concentrated solution acid adjusting pH value, described acid is preferably sulphuric acid soln, and described concentrated solution is regulated pH value and is preferably 2.5～3.
9. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that described filtrate A recycles, turn back to waste water A through sorbent treatment and prepare white arsenic, described sorbent material is for being the various acticarbons of raw material or metal, nonmetal oxide class sorbent material with the carbonaceous, and described sorbent material is preferably silica gel, activated alumina, gac, molecular sieve.
10. a kind of according to claim 1 is the synthetic method of feedstock production white arsenic with 3-nitro-4-phenol-arsonic acid waste water, it is characterized in that reaction solution adopts the triple effect thickener that it is concentrated.
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| RU2574449C2 (en) * | 2013-11-13 | 2016-02-10 | Александр Михайлович Ченцов | Method of removing arsenic (v) compounds from technological solutions |
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| CN102345143A (en) * | 2011-10-09 | 2012-02-08 | 中南大学 | Method for separating copper, arsenic and nickel and purifying copper electrolyte |
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| CN102345143A (en) * | 2011-10-09 | 2012-02-08 | 中南大学 | Method for separating copper, arsenic and nickel and purifying copper electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2574449C2 (en) * | 2013-11-13 | 2016-02-10 | Александр Михайлович Ченцов | Method of removing arsenic (v) compounds from technological solutions |
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