CN104496095B - A kind of copper powder displacement is removed and reclaims the method for antimony in water body - Google Patents
A kind of copper powder displacement is removed and reclaims the method for antimony in water body Download PDFInfo
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- CN104496095B CN104496095B CN201410784112.0A CN201410784112A CN104496095B CN 104496095 B CN104496095 B CN 104496095B CN 201410784112 A CN201410784112 A CN 201410784112A CN 104496095 B CN104496095 B CN 104496095B
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- copper powder
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention provides the displacement of a kind of copper powder remove and reclaim the method for antimony in water body, comprise the following steps: the pH of stibium-containing wastewater is adjusted to 0 ~ 3 with hydrochloric acid by (1), under nitrogen protection, add copper powder, closed reactor, with the speed stirring reaction of 100 ~ 600r/min, temperature of reaction is 10 ~ 80 DEG C, and time swap is 10 ~ 120min; In described stibium-containing wastewater, Sb (III) content is 0.1 ~ 30g/L; The quality consumption of described copper powder counts 2.5 ~ 100g/L with the volume of described waste water; (2) after having replaced, reaction system is filtered, reclaim filter residue, and filtrate is through the crystal of fast low temperature recrystallization gained; The inventive method technique is simple, and non-secondary pollution, economic environmental protection, achieves resource reproducible utilization.
Description
(1) technical field
The present invention relates to the displacement of a kind of copper powder remove and reclaim the method for antimony in water body, belong to heavy metal water-treatment technology field.
(2) technical background
Antimony is a kind of toxic element, and continuous contact brings injury can to heart and liver, and can cause stibialism when sucking the antimony of high-content, Long Term Contact has carinogenicity.After antimony is absorbed by the body, combine with the sulfydryl in human body internal protein, inhibit the activity of sulfydryl enzyme, or destroy the balance of cell intermediate ion, thus destroy the metabolic capacity of human body protein and sugar.Can acute poisoning be caused if wrongly taken into antimony compounds, produce headache, feel sick, a series of abnormal symptom such as cough, when serious, the phenomenons such as renal shutdown, arrhythmia, spasm can be caused, even may cause death.Relative to the acute poisoning of antimony, chronic poisoning is more common, after the antimony of Long Term Contact low levels and antimony compounds, will cause chronic poisoning, the general symptom such as occur weak, stomachache, uncomfortable in chest, body is empty, causes chronic conjunctivitis, the diseases such as chronic pharyngitis.
The antimony toxicity size order of different valence state is as follows: SbH
3>Sb>Sb
2s
3>Sb
2s
5>Sb
2o
3>Sb
2o
5.Antimony is successively classified as top-priority pollutent by European Union, EPA, the Japanese environmental sanitation Room etc.The World Health Organization is the experimental result of 0.43mg/ (kgd) according to causing a disease containing antimony amount in home mouse experiment, and the antimony content in regulation tap water must not higher than 5 μ g/L.Strict environmental standard has all been formulated to antimony in countries in the world.In China " water environment quality standard " (GB3838-2002) and " Drinking Water hygienic practice " (Ministry of Health, calendar year 2001), all the limit value of regulation antimony is 5 μ g/L.In addition, " water supply engineering planning specification " (GB50282-98) specifies that antimony content in water factory's water outlet is lower than 10 μ g/L, and in drinking water source, antimony is not higher than 50 μ g/L.
Along with the quickening of process of industrialization, the antimony pollution that industrial production is brought constantly expands, and in polluted river, antimony content raises gradually.Human factor has become the major cause of water body antimony pollution, mainly comprises: (1) is containing the domestic refuse of antimony; (2) discharge in the extraction industry smelting process of antimony-containing mineral containing the antimony three wastes; (3) gasoline and coal etc. are containing the burning of antimony fossil oil.How effectively to administer antimony pollution in water body and become the instant problem of reason.At present, the methods such as the precipitator method, absorption method, ion exchange method, biological process and electrochemical process are mainly contained about the purifying treatment of antimony in water body.Although these methods can remove the antimony ion of water body middle and high concentration to a certain extent, the antimony removed exists with other solid waste form, easily causes secondary pollution, and not obvious to the removal effect of lower concentration antimony in water body.
Therefore, study new and effective removal and reclaim antimony in water body, the reproducible utilization realizing resource is significant.
(3) summary of the invention
The object of the invention is the deficiency of antimony pollution in water body being administered for prior art, provide the displacement of a kind of copper powder remove and reclaim the method for antimony in water body, by adding appropriate copper powder in the hydrochloric acid system of certain temperature, effectively can remove and reclaiming the antimony in water body.
For achieving the above object, the present invention adopts following technical scheme:
Copper powder displacement is removed and is reclaimed a method for antimony in water body, said method comprising the steps of:
(1) with hydrochloric acid, the pH of stibium-containing wastewater is adjusted to 0 ~ 3, under nitrogen protection, adds copper powder, closed reactor, with the speed stirring reaction of 100 ~ 600r/min, temperature of reaction is 10 ~ 80 DEG C, and time swap is 10 ~ 120min; In described stibium-containing wastewater, Sb (III) content is 0.1 ~ 30g/L; The quality consumption of described copper powder counts 2.5 ~ 100g/L with the volume of described waste water;
(2) after having replaced, reaction system is filtered, reclaim filter residue, and filtrate is through the crystal of fast low temperature recrystallization gained.
Copper powder displacement of the present invention is removed and reclaims the method for antimony in water body, and in described step (1), the quality consumption of preferred described copper powder counts 5 ~ 50g/L with the volume of described waste water.
In described step (2), the drying of gained residue washing is black solid afterwards, and main component is Cu
2sb; Gained filtrate can obtain white crystal through fast low temperature recrystallization, is CuCl; Copper powder displacement is removed in water body and can be prepared CuCl and Cu while antimony
2sb, reaches the object of resource regeneration.
Water body of the present invention is commercial metal Metallurgical Waste Water, surface water or sanitary sewage.
Copper powder of the present invention is recommended to be 60 ~ 400 orders, preferably 200 ~ 400 orders.
The invention has the beneficial effects as follows: the invention solves in water body poor to high density antimony sewage treatment capacity in antimony pollution governance process, and easily cause the chronic illness of secondary pollution.Adopt the method for copper powder displacement, in efficient removal water body while antimony, do not produce poisonous stibine gas, and important industrial chemicals CuCl and functional materials Cu can be prepared
2sb.Preparation technology of the present invention is simple, easy to operate, efficiency is high, be easy to realization, and non-secondary pollution, economic environmental protection, achieves resource reproducible utilization.
(4) accompanying drawing explanation
Fig. 1: 200mLSb (III) content is the waste water of 5g/L, adopts hydrochloric acid that pH value of solution is adjusted to 0, adds 3g copper powder, pass into closed reactor after nitrogen, stirring velocity is 400r/min, and time swap is 60min, the removal efficiency of antimony and the relation curve of temperature of reaction in water body.
(5) embodiment
Below by specific embodiment, the present invention is further detailed, but protection scope of the present invention is not limited in this.
Embodiment 1
1) getting 200mLSb (III) content is that point silver-colored slag leach liquor of 5g/L is in reactor, adopt hydrochloric acid that pH value of solution is adjusted to 0, add 3g copper powder (60 order), pass into closed reactor after nitrogen, stirring velocity is 400r/min, temperature of reaction is 40 DEG C, and time swap is 10 ~ 120min.
Displacement efficiency is adopted to assess the displacement removal effect of copper powder to antimony in water body.
The experimental result of the different time swap of table 1
| Time/min | Displacement efficiency/% |
| 10 | 16.8 |
| 30 | 45.8 |
| 60 | 92.9 |
| 90 | 98.9 |
| 120 | 99.5 |
Embodiment 2
1) getting 200mLSb (III) content is that the surface water of 0.1g/L is in reactor, adopt hydrochloric acid that pH value of solution is adjusted to 0, add 1g copper powder (400 order), pass into closed reactor after nitrogen, stirring velocity is 400r/min, temperature of reaction is 40 DEG C, and time swap is 10 ~ 120min.
Displacement efficiency is adopted to assess the displacement removal effect of copper powder to antimony in water body.
The experimental result of the different time swap of table 2
| Time/min | Displacement efficiency/% |
| 10 | 25.8 |
| 30 | 64.5 |
| 60 | 92.9 |
| 90 | 96.8 |
| 120 | 98.7 |
Embodiment 3
1) getting 200mLSb (III) content is that point silver-colored slag leach liquor of 5g/L is in reactor, adopt hydrochloric acid that pH value of solution is adjusted to 0, add 3g copper powder (200 order), pass into closed reactor after nitrogen, stirring velocity is 400r/min, temperature of reaction is 10 ~ 80 DEG C, and time swap is 60min.
Displacement efficiency is adopted to assess the displacement removal effect of copper powder to antimony in water body.
The experimental result of table 3 difference displacement temperature
| Temperature/DEG C | Displacement efficiency/% |
| 10 | 28.3 |
| 25 | 55.8 |
| 40 | 92.9 |
| 60 | 98.2 |
| 80 | 99.7 |
Embodiment 4
1) getting 200mLSb (III) content is that point silver-colored slag leach liquor of 5g/L is in reactor, adopt hydrochloric acid that pH value of solution is adjusted to 0, add 3g copper powder (200 order), pass into closed reactor after nitrogen, stirring velocity is 100 ~ 600r/min, temperature of reaction is 40 DEG C, and time swap is 60min.
Displacement efficiency is adopted to assess the displacement removal effect of copper powder to antimony in water body.
The displacement experimental result of the different stirring velocity of table 4
| Stirring velocity/(r/min) | Displacement efficiency/% |
| 100 | 90.2 |
| 200 | 92.8 |
| 400 | 92.9 |
| 500 | 93.6 |
| 600 | 93.9 |
Embodiment 5
1) getting 200mLSb (III) content is that point silver-colored slag leach liquor of 5g/L is in reactor, adopt hydrochloric acid that pH value of solution is adjusted to 0 ~ 3, add 3g copper powder (200 order), pass into closed reactor after nitrogen, stirring velocity is 400r/min, temperature of reaction is 40 DEG C, and time swap is 60min.
Displacement efficiency is adopted to assess the displacement removal effect of copper powder to antimony in water body.
The displacement experimental result of the different pH of table 5
| pH | Displacement efficiency/% |
| 0 | 92.9 |
| 1 | 91.8 |
| 2 | 86.7 |
| 3 | 80.4 |
Embodiment 6
1) getting 200mLSb (III) content is that point silver-colored slag leach liquor of 0.1 ~ 30g/L is in reactor, adopt hydrochloric acid that pH value of solution is adjusted to 0, add 20g copper powder (200 order), pass into closed reactor after nitrogen, stirring velocity is 400r/min, temperature of reaction is 40 DEG C, and time swap is 60min.
Displacement efficiency is adopted to assess the displacement removal effect of copper powder to antimony in water body.
The displacement experimental result of the different Sb concentration of table 6
| Sb (III) concentration/gL -1 | Displacement efficiency/% |
| 0.1 | 98.9 |
| 5.0 | 92.9 |
| 10.0 | 92.1 |
| 20.0 | 91.4 |
| 30.0 | 90.8 |
Embodiment 7
1) getting 200mLSb (III) content is that the waste water of 5g/L is in reactor, adopt hydrochloric acid that pH value of solution is adjusted to 0, add 1 ~ 20g copper powder (200 order), pass into closed reactor after nitrogen, stirring velocity is 400r/min, temperature of reaction is 40 DEG C, and time swap is 60min.
Displacement efficiency is adopted to assess the displacement removal effect of copper powder to antimony in water body.
The displacement experimental result of the different copper powder add-on of table 7
| Copper powder quality/g | Displacement efficiency/% |
| 1.0 | 87.9 |
| 3.0 | 92.9 |
| 10.0 | 94.7 |
| 15.0 | 96.3 |
| 20.0 | 98.9 |
Claims (5)
1. copper powder displacement is removed and is reclaimed a method for antimony in water body, it is characterized in that, said method comprising the steps of:
(1) with hydrochloric acid, the pH of stibium-containing wastewater is adjusted to 0 ~ 3, under nitrogen protection, adds copper powder, closed reactor, with the speed stirring reaction of 100 ~ 600r/min, temperature of reaction is 10 ~ 80 DEG C, and time swap is 10 ~ 120min; In described stibium-containing wastewater, Sb (III) content is 0.1 ~ 30g/L; The quality consumption of described copper powder counts 2.5 ~ 100g/L with the volume of described waste water;
(2) after having replaced, reaction system is filtered, reclaim filter residue, and filtrate is through the crystal of fast low temperature recrystallization gained.
2. copper powder displacement as claimed in claim 1 is removed and reclaims the method for antimony in water body, and it is characterized in that, the quality consumption of described copper powder counts 5 ~ 50g/L with the volume of described waste water.
3. copper powder displacement as claimed in claim 1 is removed and reclaims the method for antimony in water body, and it is characterized in that, described water body is commercial metal Metallurgical Waste Water, surface water or sanitary sewage.
4. the copper powder displacement as described in any one of claims 1 to 3 is removed and reclaims the method for antimony in water body, and it is characterized in that, described copper powder is 60 ~ 400 orders.
5. copper powder displacement as claimed in claim 4 is removed and reclaims the method for antimony in water body, and it is characterized in that, described copper powder is 200 ~ 400 orders.
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| CN105671363B (en) * | 2016-01-11 | 2017-09-26 | 浙江工业大学 | A kind of antimony-containing alloy material and its application |
| CN105826542B (en) * | 2016-01-11 | 2019-09-03 | 浙江工业大学 | A kind of copper-antimony alloy-antimony nucleocapsid structure material and its application |
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| JPS58146490A (en) * | 1982-02-26 | 1983-09-01 | Mitsubishi Metal Corp | Removing method of antimony in acidic solution of sulfuric acid |
| CN101798629A (en) * | 2009-12-16 | 2010-08-11 | 株洲冶炼集团股份有限公司 | Method for separating valuable metals from lead anode mud |
| CN102925703B (en) * | 2012-11-22 | 2014-04-30 | 湖南稀土金属材料研究院 | Method for recycling valuable metals from lead anode slime |
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