CN110540317A - Method for separating and recycling acid waste water containing arsenic and nickel - Google Patents
Method for separating and recycling acid waste water containing arsenic and nickel Download PDFInfo
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- CN110540317A CN110540317A CN201910757935.7A CN201910757935A CN110540317A CN 110540317 A CN110540317 A CN 110540317A CN 201910757935 A CN201910757935 A CN 201910757935A CN 110540317 A CN110540317 A CN 110540317A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G28/00—Compounds of arsenic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention relates to a method for separating and recovering acid waste water containing arsenic and nickel, which comprises the following steps: (1) collecting, homogenizing and uniformly mixing the arsenic-nickel-containing acidic wastewater, and sending the arsenic-nickel-containing acidic wastewater into an oxidation pond for oxidation treatment, so that As3+ in the arsenic-nickel-containing acidic wastewater is oxidized into As5 +; (2) feeding the wastewater after oxidation treatment into an arsenic precipitation tank, adding ferric hydroxide and sodium carbonate, adjusting the pH value to 3.0-5.0, reacting, precipitating, and filtering to obtain filter residue and a recyclable nickel-containing filtrate; (3) sending the filter residue obtained from the arsenic precipitation tank into an arsenic washing tank, adding an alcohol solution for washing, precipitating and filtering to obtain arsenic washing liquid and reusable ferric hydroxide filter residue; (4) and (3) feeding the arsenic washing liquid obtained from the arsenic washing tank into a separation tank, heating and evaporating, recovering the obtained steam to obtain alcohol for recycling, and recycling the obtained liquid which is arsenic-containing liquid. Compared with the prior art, the method can effectively separate the acidic wastewater containing arsenic and nickel and recycle the acidic wastewater as resources.
Description
Technical Field
The invention belongs to the technical field of resource recycling of waste liquid, and relates to a method for separating and recycling acid waste water containing arsenic and nickel.
Background
In the process of refining metals, one of the most common impurity elements of arsenic influences the extraction and recovery of other metals, and the generated arsenic-containing wastewater can cause environmental pollution. At the same time, however, arsenic is also an excellent alloying additive. Nickel is mainly used for alloy addition and as a catalyst, can also be used for manufacturing currency and the like, and is a metal with high value and wide application. At present, the treatment of the acid wastewater containing arsenic and nickel mainly comprises a reverse osmosis method, a biological method, an extraction method and a precipitation method, wherein the extraction method has large investment and large occupied area, and the reverse osmosis method and the biological method have limitations on the problems of cost and operability. The precipitation method has wide application because of simple operation and good separation effect, and the precipitation method comprises a neutralization precipitation method, a ferrite method, a sulfide precipitation method, a coagulation method (also called an adsorption colloid precipitation method or a carrier coprecipitation method) and the like, soluble arsenic can form an insoluble compound with metal ions such as calcium, magnesium, iron, aluminum and the like or be adsorbed and removed, and the arsenic removal efficiency can reach 99%. Although such processes provide good arsenic removal, the resulting arsenic residues are of low purity and difficult to recover and process.
disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a recycling treatment method for separating and recycling the acid waste water containing arsenic and nickel.
The purpose of the invention can be realized by the following technical scheme:
A method for separating and recovering acid waste water containing arsenic and nickel comprises the following steps:
(1) Collecting, homogenizing and uniformly mixing the arsenic-nickel-containing acidic wastewater, and sending the arsenic-nickel-containing acidic wastewater into an oxidation pond for oxidation treatment, so that As3+ in the arsenic-nickel-containing acidic wastewater is oxidized into As5 +;
(2) feeding the wastewater after oxidation treatment into an arsenic precipitation tank, adding ferric hydroxide and sodium carbonate, adjusting the pH value to 3.0-5.0, reacting, precipitating, and filtering to obtain filter residue and a recyclable nickel-containing filtrate;
(3) Sending the filter residue obtained from the arsenic precipitation tank into an arsenic washing tank, adding an alcohol solution for washing, precipitating and filtering to obtain arsenic washing liquid and reusable ferric hydroxide filter residue;
(4) And (3) feeding the arsenic washing liquid obtained from the arsenic washing tank into a separation tank, heating and evaporating, recovering the obtained steam to obtain alcohol for recycling, and recycling the obtained liquid which is arsenic-containing liquid.
Further, in the step (1), the oxidation treatment is treatment by adding an oxidant into the oxidation pond, wherein the oxidant is one or more of hydrogen peroxide, sodium persulfate, potassium persulfate and potassium hydrogen persulfate.
Furthermore, the dosage of the oxidant is 1 to 10 times of the molar concentration of As3+ in the nickel arsenic-containing acidic wastewater.
Further, in the step (2), the mass ratio of the addition amount of the ferric hydroxide to the addition amount of the sodium carbonate is 10: 0.1-10.
further, the reaction settling time is 30-180 min.
further, the mass concentration of the alcohol solution is 50-95%.
Further, in the step (3), the washing time is 30-180min, and the settling time is 30-180 min.
Further, in the step (4), the temperature for heating and evaporating is 78-99 ℃.
The adding of the ferric hydroxide can play a role in regulating the pH value when the pH value of the acid wastewater containing arsenic and nickel is lower than 2.7, the adding amount is greatly reduced compared with the adding of sodium carbonate directly, and the ferric hydroxide plays a role in adsorbing arsenic ions in the acid wastewater containing arsenic and nickel when the pH value is higher than 2.7; the sodium carbonate is added when the pH value of the acidic wastewater containing nickel arsenic is adjusted to be more than 2.7, and the pH value is further adjusted to be 3.0-5.0. After the ferric hydroxide is used for adsorbing arsenic ions in the acid wastewater containing arsenic and nickel, solid-liquid separation is carried out, and the nickel-containing recovery liquid can be recovered. The alcohol solution is adopted, so that arsenic adsorbed by the ferric hydroxide can be eluted, and the ferric hydroxide can be recycled; the alcohol and the water can be separated through the different boiling points of the alcohol and the water, and the arsenic is left in the water for recycling.
According to the invention, the medicament obtained by compounding ferric hydroxide and sodium carbonate is adopted to settle arsenic, so that relatively pure nickel-containing wastewater is obtained; washing the ferric hydroxide by adopting an alcohol solution so that the ferric hydroxide can be recycled; the pure arsenic-containing liquid is obtained on the basis of separating the alcohol by heating, so that the alcohol can be recycled.
Compared with the prior art, the invention has the following advantages:
(1) The method can effectively separate the acidic wastewater containing arsenic and nickel and recycle the acidic wastewater.
(2) The ferric hydroxide and the alcohol used in the invention can be recycled, thus reducing the investment of cost.
(3) the method does not produce arsenic-containing waste residues, is harmless to the environment, and solves the problem that the arsenic-containing waste residues are difficult to treat.
(4) The process facility can change the treatment capacity according to the production requirement, has simple process and convenient operation, can fully recover the acid wastewater containing arsenic and nickel, and generates economic effect.
drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
In the following examples, unless otherwise specified, the starting materials or the treatment techniques are all conventional and commercially available materials or conventional treatment techniques in the art.
Example 1
The situation of the acid wastewater containing nickel arsenic produced by a certain plant is as follows: 40 cubic meters per day, the pH was 1.75, the As3+ concentration was 9.7g/L, the As5+ concentration was 4.7g/L, and the Ni2+ concentration was 17 g/L.
The method for recycling the acidic wastewater containing nickel and arsenic as shown in figure 1 comprises the following specific steps:
Step 1: collecting the acid wastewater containing arsenic and nickel, and uniformly mixing the acid wastewater in a homogenizing pool to keep the water quality stable.
Step 2: and (2) feeding the wastewater in the homogenizing tank into an oxidation tank, opening a dosing tank, automatically controlling hydrogen peroxide with the weight concentration of 27.5-50% through an automatic control valve, and reserving the hydrogen peroxide from the dosing tank to the oxidation tank for oxidation, so that As3+ in the wastewater is oxidized into As5+, the using amount of the hydrogen peroxide is 2.7 times of the molar concentration of As3+, and the flow rate is controlled to be 0.3m 3/h. The time of the oxidation reaction after the dosing is finished is 60 min.
And step 3: and (2) feeding the wastewater oxidized by the oxidation pond into an arsenic precipitation pond, adding ferric hydroxide and sodium carbonate according to the mass ratio of 10:3, adjusting the pH to be about 3.0-5.0, reacting for 60min, precipitating for 120min, and performing pressure filtration by using a plate-and-frame filter press to obtain filtrate and filter residue, wherein the concentration of nickel in the filtrate is 16.4g/L, and the concentration of As5+ is 0.1 g/L.
And 4, step 4: and (3) sending filter residues obtained in the arsenic precipitation tank into an arsenic washing tank, wherein the arsenic washing tank contains 50-95% of alcohol solution by mass concentration, and washing for 60 min. Settling for 60min, and press-filtering with plate-and-frame filter press to obtain reusable ferric hydroxide filter residue and arsenic washing solution;
and 5: and (3) feeding the arsenic washing liquid obtained from the arsenic precipitation tank into a separation tank, heating to 78-99 ℃ (78 ℃, 85 ℃ or 99 ℃ or any other temperature value in the range), recovering the obtained steam after evaporation to obtain alcohol for recycling, wherein the obtained liquid is arsenic-containing liquid with arsenic concentration of 40g/L, and recycling.
Example 2
The situation of the acid wastewater containing nickel arsenic produced by a certain plant is as follows: 7 cubic meters per day, pH was 1.24, As3+ concentration was 17g/L, As5+ concentration was 7g/L, and Ni2+ concentration was 27 g/L.
The method for recycling the acidic wastewater containing nickel and arsenic as shown in figure 1 comprises the following specific steps:
Step 1: collecting the acid wastewater containing arsenic and nickel, and uniformly mixing the acid wastewater in a homogenizing pool to keep the water quality stable.
Step 2: and (2) feeding the wastewater in the homogenizing tank into an oxidation tank, opening a dosing tank, automatically controlling hydrogen peroxide with the weight concentration of 27.5-50% through an automatic control valve, and reserving the hydrogen peroxide from the dosing tank to the oxidation tank for oxidation, so that As3+ in the wastewater is oxidized into As5+, the using amount of the hydrogen peroxide is 4 times of the molar concentration of As3+, and the flow rate is controlled to be 0.3m 3/h. The time of the oxidation reaction after the dosing is finished is 60 min.
And step 3: sending the wastewater oxidized by the oxidation tank into an arsenic precipitation tank, and adding ferric hydroxide and sodium carbonate according to the mass ratio of 10: and 3, adjusting the pH value to about 3.0-5.0, reacting for 60min, settling for 120min, and performing pressure filtration by using a plate-and-frame filter press to obtain filtrate and filter residue, wherein the concentration of nickel in the filtrate is 25.9g/L, and the concentration of As5+ is 0.13 g/L.
and 4, step 4: and (3) sending filter residues obtained in the arsenic precipitation tank into an arsenic washing tank, wherein the arsenic washing tank contains 50-95% of alcohol solution by mass concentration, and washing for 60 min. Settling for 60min, and press-filtering with plate-and-frame filter press to obtain reusable ferric hydroxide filter residue and arsenic washing solution;
And 5: and (3) feeding the arsenic washing liquid obtained from the arsenic precipitation tank into a separation tank, heating to 78-99 ℃, recovering the obtained steam after evaporation to obtain alcohol for recycling, wherein the obtained liquid is arsenic-containing liquid, and the concentration of arsenic contained in the liquid is 43g/L for recycling.
Example 3
The situation of the acid wastewater containing nickel arsenic produced by a certain plant is as follows: 20 cubic meters per day, the pH was 1.14, the As3+ concentration was 9.7g/L, the As5+ concentration was 2.7g/L, and the Ni2+ concentration was 10 g/L.
The method for recycling the acidic wastewater containing nickel and arsenic as shown in figure 1 comprises the following specific steps:
Step 1: collecting the acid wastewater containing arsenic and nickel, and uniformly mixing the acid wastewater in a homogenizing pool to keep the water quality stable.
Step 2: and (2) feeding the wastewater in the homogenizing tank into an oxidation tank, opening a dosing tank, automatically controlling hydrogen peroxide with the weight concentration of 27.5-50% through an automatic control valve, and reserving the hydrogen peroxide from the dosing tank to the oxidation tank for oxidation, so that As3+ in the wastewater is oxidized into As5+, the using amount of the hydrogen peroxide is 3 times of the molar concentration of As3+, and the flow rate is controlled to be 0.5m 3/h. The time of the oxidation reaction after the dosing is finished is 60 min.
And step 3: sending the wastewater oxidized by the oxidation tank into an arsenic precipitation tank, and adding ferric hydroxide and sodium carbonate according to the mass ratio of 10: and 3, adjusting the pH value to 3.0-5.0, reacting for 60min, settling for 120min, and performing pressure filtration by using a plate-and-frame filter press to obtain filtrate and filter residue, wherein the concentration of nickel in the filtrate is 9.7g/L, and the concentration of As5+ is 0.07 g/L.
And 4, step 4: and (3) sending filter residues obtained in the arsenic precipitation tank into an arsenic washing tank, wherein the arsenic washing tank contains 50-95% of alcohol solution by mass concentration, and washing for 60 min. Settling for 60min, and press-filtering with plate-and-frame filter press to obtain reusable ferric hydroxide filter residue and arsenic washing solution;
And 5: and (3) feeding the arsenic washing liquid obtained from the arsenic precipitation tank into a separation tank, heating to 78-99 ℃, recovering the obtained steam after evaporation to obtain alcohol for recycling, wherein the obtained liquid is arsenic-containing liquid, and the concentration of arsenic is 20g/L for recycling.
example 4-example 6
Compared with example 1, the same is mostly true except that sodium persulfate, potassium persulfate or oxone are used instead as the oxidizing agent in this example, respectively.
Example 7
Compared to example 1, most of them are the same except that in this example: the dosage of the oxidant is 1 time of the molar concentration of As3+ in the nickel arsenic-containing acidic wastewater.
Example 8
Compared to example 1, most of them are the same except that in this example: the dosage of the oxidant is 10 times of the molar concentration of As3+ in the nickel arsenic-containing acidic wastewater.
example 9
Compared to example 1, most of them are the same except that in this example: the mass ratio of the addition amount of the ferric hydroxide to the sodium carbonate is 10: 0.1.
example 10
compared to example 1, most of them are the same except that in this example: the mass ratio of the addition amount of the ferric hydroxide to the sodium carbonate is 10: 10.
In the above embodiments, the reaction settling time may be arbitrarily selected within 30-180min, for example, 30min or 180min, or any intermediate value within the range, according to the ion concentration in the wastewater, the type and the addition amount of the reaction settling reagent added, and the like. Similarly, the washing settling time in step 4 can be arbitrarily selected within 30-180 min.
In the above examples, unless otherwise specified, raw materials, reagents or processing techniques are all conventional in the art and commercially available raw materials or conventional techniques.
the embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (8)
1. The method for separating and recovering the acidic waste water containing arsenic and nickel is characterized by comprising the following steps of:
(1) Collecting, homogenizing and uniformly mixing the arsenic-nickel-containing acidic wastewater, and sending the arsenic-nickel-containing acidic wastewater into an oxidation pond for oxidation treatment, so that As3+ in the arsenic-nickel-containing acidic wastewater is oxidized into As5 +;
(2) Feeding the wastewater after oxidation treatment into an arsenic precipitation tank, adding ferric hydroxide and sodium carbonate, adjusting the pH value to 3.0-5.0, reacting, precipitating, and filtering to obtain filter residue and a recyclable nickel-containing filtrate;
(3) Sending the filter residue obtained from the arsenic precipitation tank into an arsenic washing tank, adding an alcohol solution for washing, precipitating and filtering to obtain arsenic washing liquid and reusable ferric hydroxide filter residue;
(4) And (3) feeding the arsenic washing liquid obtained from the arsenic washing tank into a separation tank, heating and evaporating, recovering the obtained steam to obtain alcohol for recycling, and recycling the obtained liquid which is arsenic-containing liquid.
2. the method for separating and recovering the acid waste water containing arsenic and nickel as claimed in claim 1, wherein in the step (1), the oxidation treatment is a treatment of adding an oxidant into an oxidation pond, and the oxidant is one or more of hydrogen peroxide, sodium persulfate, potassium persulfate or potassium hydrogen persulfate.
3. The method for separating and recovering the acidic wastewater containing nickel arsenic As claimed in claim 2, wherein the amount of the oxidant added is 1-10 times of the molar concentration of As3 +.
4. The method for separating and recovering the acidic wastewater containing nickel arsenic according to claim 1, wherein in the step (2), the mass ratio of the addition amount of the ferric hydroxide to the addition amount of the sodium carbonate is 10: 0.1-10.
5. The method for separating and recovering the acidic waste water containing nickel arsenic according to claim 1, wherein the reaction settling time is 30-180 min.
6. The method for separating and recovering the acidic wastewater containing nickel arsenic according to claim 1, wherein the mass concentration of the alcohol solution is 50-95%.
7. The method for separating and recovering the acidic waste water containing nickel arsenic according to claim 1, wherein in the step (3), the washing time is 30-180min, and the settling time is 30-180 min.
8. The method for separating and recovering the acid waste water containing nickel arsenic according to claim 1, wherein the temperature for heating and evaporating in the step (4) is 78-99 ℃.
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Citations (8)
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2019
- 2019-08-16 CN CN201910757935.7A patent/CN110540317A/en active Pending
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| CN102815818A (en) * | 2012-08-07 | 2012-12-12 | 华南理工大学 | Method of removing arsenic from printed circuit board acid etching exhausted liquid |
| CN103626338A (en) * | 2013-12-12 | 2014-03-12 | 南京大学 | Method for treating high-concentration alkaline arsenic mining and metallurgy wastewater by coprecipitation-ion exchange compound technology |
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