CN108164065B - Sulfuric acid system acidic heavy metal wastewater treatment process - Google Patents
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/447—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by membrane distillation
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- 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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- C02F2101/20—Heavy metals or heavy metal compounds
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- 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
- C02F2101/203—Iron or iron compound
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- C02F2101/00—Nature of the contaminant
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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Abstract
The invention discloses a process for treating acidic heavy metal wastewater in a sulfuric acid system. The method comprises the following steps: (1) pretreating the wastewater, and adjusting the pH of the wastewater to be more than or equal to 1.5 by adopting sodium hydroxide; (2) conveying the wastewater to a filtering device for filtering; (3) conveying the filtered wastewater to a feed liquid tank for heating; (4) conveying the heated wastewater to a filtering device for filtering; (5) conveying the filtered wastewater to a hydrophobic microporous membrane component for membrane distillation concentration, condensing membrane-passing steam to be used as produced water, collecting and monitoring the conductivity of the produced water, and refluxing the solution to a feed liquid tank; and (5) circulating between the steps (3) to (5) until the required concentration multiple is reached, and finishing the process. The process can be used for filtering ferric hydroxide sediments generated continuously due to the cyclic concentration of the wastewater, preventing the reduction of membrane distillation performance caused by the deposition of the ferric hydroxide on the surface of a hydrophobic membrane, and improving the stability of the whole process, thereby realizing the reduction of acidic heavy metal wastewater and the improvement of heavy metal concentration.
Description
Technical Field
The invention relates to a process for treating acidic heavy metal wastewater in a sulfuric acid system, and belongs to the field of heavy metal wastewater treatment.
Background
The industries of non-ferrous metal mining, ore dressing, smelting, electroplating and the like can generate sulfuric acid system acidic wastewater which has low pH (pH is more than 1 and less than 6) and contains various heavy metals with low concentration (single metal content is less than 1 g/L). In the actual operation process of enterprises, a lime precipitation method is generally the main method for treating the wastewater, but the investment of a large amount of lime often obtains heavy metal hazardous waste sludge which brings high economic burden to the enterprises. With the continuous improvement of the environmental protection requirement of China, the treatment cost of the heavy metal hazardous waste sludge is also improved, which forces enterprises to turn to find other methods for treating the acidic heavy metal wastewater.
The wastewater is concentrated, so that the total amount of the wastewater can be effectively reduced, the concentration of heavy metal can be improved, and the treatment cost of subsequent heavy metal removal or recovery can be reduced. With the deep popularization and application of the membrane technology in the field of environmental protection, reverse osmosis is used as a mature membrane concentration technology to be applied to part of industrial wastewater treatment, such as organic salt-containing wastewater, printing and dyeing wastewater and the like in the chemical industry. In addition, reverse osmosis has also been used and studied to some extent in the field of electroplating heavy metal wastewater. However, reverse osmosis membranes are generally polyamide hydrophilic membranes, which have poor corrosion oxidation resistance and acid resistance, acidic heavy metal wastewater often contains metals with oxidation properties such as cr (vi), fe (iii), and the like, and the pH of part of wastewater is very low, which can reach about 2-3 or even lower, and reverse osmosis membranes are limited in their own properties when applied to such wastewater, and require relatively strict pretreatment at the early stage.
The membrane distillation is also a membrane concentration technology with excellent performance, wherein the membrane distillation takes a hydrophobic microporous membrane as a separation membrane, the partial pressure difference of steam is produced on two sides of the membrane by a certain means, the partial pressure difference is taken as a mass transfer driving force to drive steam perforation micropores to reach the other side of the membrane, and the steam perforation micropores are collected by a certain mode. Although the technical maturity of the current membrane distillation is inferior to reverse osmosis, the property superior to reverse osmosis in some aspects makes it promising. On one hand, the membrane distillation generally adopts an organic polymer hydrophobic membrane with excellent chemical stability as a separation membrane, such as PVDF and PTFE, which enables the membrane to have better corrosion oxidation resistance and acid resistance compared with a reverse osmosis hydrophilic membrane, and literature researches show that the PTFE hollow fiber membrane can be even used for concentrating sulfuric acid; on the other hand, the membrane distillation is a hydrophobic operation principle, only gas can permeate through membrane pores, and other nonvolatile substances in the solution are intercepted, so that the membrane distillation has better interception performance compared with reverse osmosis, and especially has extremely high interception rate on free metal ions.
However, similar to other membrane technologies, membrane fouling during membrane distillation also has a large impact on membrane distillation performance. The acidic heavy metal wastewater generally contains Fe3+In an amount of up to several hundred milligrams per liter, Fe3+The membrane distillation performance is influenced by membrane pollution caused by colloid easily formed in the concentration process. Therefore, aiming at the characteristics of the wastewater, the key problems are solved, and the development of a novel treatment process based on a membrane distillation technology is necessary.
Disclosure of Invention
The invention aims to solve the problems that the acidic heavy metal wastewater of a sulfuric acid system contains corrosive oxidizing metals, has low pH value and Fe3+The concentration treatment is difficult due to high content, and a sulfuric acid system acidic heavy metal wastewater treatment process is provided to reduce the amount of acidic heavy metal wastewater and improve the concentration of heavy metal, reduce the subsequent heavy metal removal or recovery cost, obtain high-purity produced water and recycle water resources.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for treating acidic heavy metal wastewater in a sulfuric acid system comprises the following steps:
(1) pretreating the wastewater, and adjusting the pH of the wastewater to be more than or equal to 1.5 by adopting sodium hydroxide;
(2) conveying the wastewater to a filtering device for filtering;
(3) conveying the filtered wastewater to a feed liquid tank for heating;
(4) conveying the heated wastewater to a filtering device for filtering;
(5) conveying the filtered wastewater to a hydrophobic microporous membrane component for membrane distillation concentration, condensing membrane-passing steam to be used as produced water, collecting and monitoring the conductivity of the produced water, and refluxing the solution to a feed liquid tank;
and (5) circulating between the steps (3) to (5) until the required concentration multiple is reached, and finishing the process.
In the process, the pH value of the acidic heavy metal wastewater is 1-6; containing heavy metalsIncluding Fe2+、Fe3 +、Zn2+、Cr3+、Cr(VI)、Cd2+、Co2+、Mn2+、Ni2+、Cu2+、Pb2+The concentration range of each ion is 0.01-1 g/L.
In the process, the filtering pore size of the filtering equipment in the step (2) is 1-100 micrometers.
In the process, the temperature of the wastewater in the step (3) is 50-70 ℃ after the wastewater is heated.
In the process, the filtering pore size of the filtering equipment in the step (4) is 0.1-10 microns.
In the process of the invention, the maximum tolerance temperature of the filtering equipment in the step (4) is above 70 ℃.
In the process of the present invention, the hydrophobic microporous membrane module in the step (5) is a tubular membrane module.
In the process of the present invention, the hydrophobic microporous membrane in the step (5) has a minimum tolerance pH of 1 or more.
In the process of the invention, the pH of the wastewater is greater than 1 after the cyclic concentration is completed.
The invention has the beneficial effects that:
the invention provides a sulfuric acid system acidic heavy metal wastewater treatment process based on a membrane distillation technology which adopts an organic polymer hydrophobic microporous membrane as a separation membrane, fully utilizes the excellent corrosion oxidation resistance and acid resistance of the hydrophobic microporous membrane and the excellent interception performance of the membrane distillation technology, realizes the coagulation of ferric hydroxide colloid by controlling the heating temperature, and filters ferric hydroxide sediments continuously generated due to wastewater cyclic concentration through a filtering device with good temperature resistance, thereby preventing the membrane distillation performance from being reduced due to the sedimentation and aggregation of ferric hydroxide on the surface of the hydrophobic membrane, improving the overall process stability, realizing the concentration decrement and heavy metal concentration improvement of sulfuric acid system acidic heavy metal wastewater, reducing the subsequent heavy metal removal or recovery cost, obtaining high-purity produced water, and realizing the reuse of water resources.
Detailed Description
The following further describes embodiments of the present invention, but the embodiments of the present invention are not limited thereto.
The wastewater treatment process comprises the following steps: (1) taking out and quantifying the heavy metal ions (including Fe)2+、Fe3+、Zn2+、Cr3+、Cr(VI)、Cd2+、Co2+、Mn2+、Ni2+、Cu2+、Pb2+) Adding sodium hydroxide into the sulfuric acid system heavy metal wastewater to adjust and control the pH of the wastewater to be more than or equal to 1.5; (2) conveying the wastewater to a filtering device for filtering to remove suspended particulate matters, flocculent precipitates and the like in the wastewater; (3) conveying the filtered wastewater to a wastewater feed liquid tank, and heating to 50-70 ℃; (4) conveying the heated wastewater to a filtering device with good high temperature resistance for filtering; (5) conveying the filtered wastewater to a hydrophobic microporous membrane component for membrane distillation concentration, condensing membrane-passing steam to be used as produced water, collecting and monitoring the conductivity of the produced water, and refluxing the solution to a feed liquid tank; and then circulating among the steps (3) to (5) until the required concentration multiple is reached, and finishing the process.
Example 1
The process of the invention is used for treating zinc (Zn)2+) Copper (Cu)2+) Nickel (Ni)2+) Chromium (VI), iron (Fe)3+) The pH value of the electroplating wastewater is 1.2 by using a sulfuric acid system of plasma metal ions (the content is shown in the table 1); the membrane distillation operation mode is air gap type membrane distillation (circulating condensed water on the other side of the cooling partition plate is used for cooling and collecting membrane steam), the membrane component is a tubular membrane component made of PTFE material, the average membrane pore size of the hydrophobic microporous membrane is 0.08 micrometer, and the membrane wall thickness is 0.44 micrometer. The method comprises the following specific steps: (1) adjusting the pH value of the wastewater to 1.5 by using sodium hydroxide; (2) then, carrying out solid-liquid separation on the wastewater after the pH is adjusted by adopting filter cloth with the aperture of 50 microns; (3) heating the supernatant in a square feed liquid tank made of PP material; (4) the heated wastewater flows through a PP cotton filter with the filter aperture of about 1 micron to filter out ferric hydroxide sediment formed after heating; (5) and the wastewater from which the ferric hydroxide sediment is filtered enters a membrane distillation system to operate a membrane distillation concentration process. The operating conditions were: the average temperature of the inlet and the outlet of the feed liquid membrane module is 60 ℃, and the temperature of circulating condensed water isThe membrane module was backwashed for 30 minutes at 20 ℃ with the water conductivity set at 150. mu.S/cm.
The membrane distillation process was stopped when the concentration factor reached 10 times, at which time the pH of the concentrated wastewater was 1.2. In the operation process of membrane distillation, the conductivity of the membrane distillation produced water is always maintained below 60 mu S/cm, the water quality of the produced water is good in reusability, the content and the retention rate of each heavy metal before and after concentration are shown in Table 1, wherein Fe3+The increase in the content of (A) is much smaller than that of other metals, about 85% Fe3+The iron hydroxide sediment formed after the cyclic concentration and heating is filtered out in a PP cotton filter.
TABLE 1 content and rejection rate of each heavy metal in electroplating wastewater before and after membrane distillation concentration
| Metal ion | Zn2+ | Cu2+ | Ni2+ | Cr(VI) | Fe3+ |
| Content before concentration (mg/L) | 72 | 120 | 65 | 86 | 206 |
| Content after concentration (mg/L) | 701 | 1142 | 633 | 863 | 362 |
| Retention rate | ＞99％ | ＞99％ | ＞99％ | ＞99％ |
Example 2
The process of the invention is adopted to treat cadmium (Cd)2+) Cobalt (Co)2+) Copper (Cu)2+) Iron (Fe)3+) Waste water from sulfuric acid system smelting of plasma metal ions, in which Fe3+The content exceeds 5g/L, and the pH value of the wastewater is 2.6; the membrane distillation operation mode is direct contact membrane distillation (membrane steam is collected by directly condensing cooling circulating pure water on the cold side of the membrane), the membrane component is a tubular membrane component made of PTFE material, the average membrane pore size of a hydrophobic microporous membrane is 0.12 micrometer, and the wall thickness of the membrane is 0.3 micrometer. The method comprises the following specific steps: (1) carrying out solid-liquid separation on the wastewater by adopting filter cloth with the aperture of 10 microns; (2) heating the supernatant in a square feed liquid tank made of PP material; (3) the heated wastewater flows through a PP cotton filter with the filter aperture of about 1 micron to filter out ferric hydroxide sediment formed after heating; (5) and the wastewater from which the ferric hydroxide sediment is filtered enters a membrane distillation system to operate a membrane distillation concentration process. The operating conditions were: the average temperature of the inlet and the outlet of the feed liquid membrane module is 60 ℃, the temperature of circulating condensed water is 20 ℃, and the membrane module is backwashed for 30 minutes when the conductivity of produced water is set to be 150 mu S/cm.
The membrane distillation process was stopped when the concentration factor reached 10 times, at which time the pH of the concentrated wastewater was 2.3. During the operation of membrane distillation, the conductivity of the membrane distillation produced water is always maintained at 100 muS/cm or less, the contents and retention rates of each heavy metal before and after concentration are shown in Table 2, wherein Fe in the solution3+The content of Fe is reduced from 5.26g/L to 650mg/L and is more than 95 percent3+Filtered off during this process.
TABLE 2 content and retention rate of heavy metals in the smelting wastewater before and after membrane distillation concentration
| Metal ion | Cd2+ | Co2+ | Cu2+ | Fe3+ |
| Content before concentration (mg/L) | 120 | 63 | 230 | 5260 |
| Content after concentration (mg/L) | 1030 | 585 | 2010 | 650 |
| Retention rate | ＞85％ | ＞90％ | ＞85％ |
Claims (4)
1. A process for treating the acidic heavy metal sewage containing corrosive oxidizing metal, low pH value and Fe in sulfuric acid system3+The content is high, and the method is characterized in that the pH value of the acidic heavy metal wastewater is 1-6; containing heavy metals including Fe2+、Fe3+、Zn2+、Cr3+、Cr(VI)、Cd2+、Co2+、Mn2+、Ni2+、Cu2+、Pb2+The concentration range of each ion is 0.01-10 g/L, wherein Fe3+Is higher than 206 mg/L;
the process comprises the following steps:
(1) pretreating the wastewater, and adjusting the pH of the wastewater to 1.5-2.6 by using sodium hydroxide;
(2) conveying the wastewater to a filtering device for filtering;
(3) conveying the filtered wastewater to a material liquid tank for heating, wherein the temperature of the heated wastewater is 50-70 ℃;
(4) conveying the heated wastewater to a filtering device for filtering;
(5) conveying the filtered wastewater to a hydrophobic microporous membrane component for membrane distillation concentration, condensing membrane-passing steam to be used as produced water, collecting and monitoring the conductivity of the produced water, refluxing the solution to a material liquid tank, and backwashing the membrane component when the conductivity of the produced water is set to be 150 muS/cm; the hydrophobic microporous membrane component is a tubular membrane component, and the lowest tolerance pH of the hydrophobic microporous membrane is below 1;
and (5) circulating the steps (3) to (5) until the required concentration multiple is reached, ending the process, and finishing the circulating concentration until the pH value of the wastewater is more than 1.
2. The process for treating the acidic heavy metal wastewater in the sulfuric acid system according to claim 1, which comprises the following steps: and (3) filtering pore size of the filtering equipment in the step (2) is 1-100 microns.
3. The process for treating the acidic heavy metal wastewater in the sulfuric acid system according to claim 1, which comprises the following steps: and (4) filtering pore size of the filtering equipment in the step (4) is 0.1-10 microns.
4. The process for treating the acidic heavy metal wastewater in the sulfuric acid system according to claim 1, which comprises the following steps: the highest tolerance temperature of the filtering equipment in the step (4) is above 70 ℃.
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