CN112028325A - Method for comprehensively treating non-ferrous smelting acidic high-chlorine wastewater - Google Patents
Method for comprehensively treating non-ferrous smelting acidic high-chlorine wastewater Download PDFInfo
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal 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
- 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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Abstract
The invention provides a method for comprehensively treating non-ferrous smelting acidic high-chlorine wastewater, wherein the treated object is non-ferrous smelting acidic high-chlorine wastewater, primary dechlorination is carried out by a cuprous chloride method, primary heavy metal is removed by lime and ferric salt, secondary dechlorination is carried out by lime and sodium metaaluminate, secondary heavy metal is removed by ferric salt and sulfuric acid, and the concentration of chloride ions in the high-chlorine wastewater is reduced to be below 500 mg/L from 20000 mg/L. The produced water quality meets the 5 th part of the Shandong province local standard-drainage basin water pollutant comprehensive emission standard: peninsula watershed (DB 37/3416.5-2018). Not only solves the problem that the acid high-chlorine wastewater from nonferrous smelting is difficult to treat, but also can recover valuable elements and realize green production of changing waste into valuable.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for comprehensively treating non-ferrous smelting acidic high-chlorine wastewater.
Background
A large amount of acidic waste water is generated in the nonferrous smelting industry, and particularly, a large amount of acidic high-chlorine waste water is generated by enterprises in the hydrometallurgy industry. The content of chloride ions in the non-ferrous smelting acidic high-chlorine wastewater is up to 20000 mg/L, the heavy metal ions are higher, the wastewater is usually treated by a chemical precipitation method or a lime neutralization method, and the treated liquid has high chlorine content and contains a small amount of heavy metal ions and can not be directly recycled or discharged. The high-concentration chloride ions not only can corrode a drain pipe and a building, but also can cause serious scaling of the drain pipe together with calcium and magnesium precipitates such as gypsum, phosphate, carbonate and the like, and when a large amount of wastewater containing chloride ions and heavy metal ions with higher concentration is discharged, serious harm can be brought to the environment, people and the growth of animals and plants, so that a method for treating the nonferrous smelting acidic high-chloride wastewater is urgently needed.
Disclosure of Invention
The invention provides a method for comprehensively treating non-ferrous smelting acidic high-chlorine wastewater, which solves the problems that the acidic high-chlorine wastewater in the background technology is difficult to treat and cannot be utilized and the like.
The technical scheme of the invention is realized as follows: a method for comprehensively treating non-ferrous smelting acidic high-chlorine wastewater comprises the following steps:
1) primary dechlorination: pumping the non-ferrous smelting acidic high-chlorine wastewater into a reaction tank, adding cuprous oxide, wherein the addition amount of the cuprous oxide is added according to the molar ratio of the copper content to the chlorine content in the wastewater, namely Cu/Cl = 1.1-1.3, the reaction temperature is 40-80 ℃, the reaction time is 1-3 h, and carrying out solid-liquid separation after the reaction is finished;
2) alkaline leaching: alkaline leaching is carried out on cuprous chloride slag generated by primary dechlorination, an alkaline leaching agent is a sodium hydroxide solution, the concentration of the sodium hydroxide solution is 10-15% of the mass fraction, the leaching temperature is 60-90 ℃, the leaching time is 0.5-2 h, after the alkaline leaching is finished, solid-liquid separation is carried out, the solid is activated cuprous oxide, the activated cuprous oxide is directly recycled for primary dechlorination, the liquid is evaporated and concentrated, and sodium chloride is recovered;
3) primary heavy metal removal: pumping the wastewater generated by primary dechlorination into a stirring tank, adding lime and ferric salt, wherein the adding amount of the lime is 20 Kg/m3~100 Kg/m3The adding amount of the iron salt is 5 Kg/m3~30 Kg/m3Reacting for 0.5-2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, and carrying out secondary dechlorination on the liquid;
4) secondary dechlorination: pumping the primary heavy metal removal filtrate into a stirring tank, adding lime and sodium metaaluminate at the same time, adding the lime and the sodium metaaluminate according to the molar mass ratio of Ca to Al to Cl = (10-15): (3-4): 1, reacting for 0.5-2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, and carrying out secondary heavy metal removal on the liquid;
5) secondary heavy metal removal: pumping the wastewater generated by secondary dechlorination into a stirring tank, adding ferric salt and sulfuric acid, wherein the adding amount of the ferric salt is 10 Kg/m3~50 Kg/m3The addition amount of the sulfuric acid is 5 Kg/m3~20 Kg/m3Reacting for 0.5-2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, wherein the solid is used for pyrometallurgical ore blending, and the liquid can be directly discharged;
preferably, cuprous oxide is added, the firstly used cuprous oxide is activated for 2 hours by a sodium hydroxide solution with the mass concentration of 10-15%, and the subsequently used cuprous oxide is derived from cuprous oxide generated by the reaction of cuprous chloride and sodium hydroxide;
preferably, the cuprous oxide slag generated by primary dechlorination is directly added with a sodium hydroxide solution for alkaline leaching without drying, and after leaching, the alkaline slag is directly recycled without drying treatment, so that cuprous oxide is prevented from being oxidized and inactivated by air;
preferably, the lime and the ferric salt added for removing the heavy metals for the first time are added, and the ferric salt is composed of ferrous sulfate and ferric sulfate and comprises the following components in percentage by mass: adding lime and then adding ferric salt into ferric sulfate = 1-3: 1, and finally controlling the pH of the solution to = 6-8;
preferably, the sulfuric acid and the ferric salt added for secondary heavy metal removal are industrial 98% acid, and the ferric salt is composed of ferrous sulfate and ferric sulfate and comprises the following components in percentage by mass: ferric sulfate =1: 1-5, ferric salt is added firstly, then sulfuric acid is added, and finally the pH of the solution is controlled to be = 6-8.
The invention has the beneficial effects that:
1) the concentration of chloride ions in the high-chlorine wastewater is reduced from 20000 mg/L to below 500 mg/L;
2) the cuprous oxide as the dechlorinating agent can be repeatedly used, and the cuprous chloride generated after the cuprous oxide dechlorination can be directly recycled after being treated by the sodium hydroxide solution.
3) The produced water quality meets the 5 th part of the Shandong province local standard-drainage basin water pollutant comprehensive emission standard: peninsula watersheds (DB 37/3416.5-2018) can be directly discharged outwards;
4) the comprehensive utilization rate of resources is high, and sodium chloride obtained by evaporation and crystallization can be sold as a product;
5) the process is simple and easy to control, and the production cost is low.
According to the invention, through twice dechlorination and twice heavy metal ion removal, the produced water quality meets the 5 th part of the Shandong province local standard-drainage basin water pollutant comprehensive emission standard: the peninsula river basin (DB 37/3416.5-2018) not only solves the problem that the acid high-chlorine wastewater from nonferrous smelting is difficult to treat, but also can recover valuable elements and realize green production of changing waste into valuable.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
Example 1:
the elemental analysis of the nonferrous smelting acidic high-chlorine wastewater is shown in the following table 1:
TABLE 1 assay analysis results (mg/L)
| Name (R) | Cd | Cr | Cu | Pb | Hg | As | Ni | Zn | Cl- | pH |
| Waste water | 12.34 | 0.53 | 221.0 | 59.0 | 0.024 | 284.0 | 1.09 | 359.7 | 24318 | 0.62 |
Non-ferrous smelting acidic high-chlorine wastewater 10 m3Pumping into a reaction tank, adding 592 Kg of cuprous oxide activated by 15 percent by mass of sodium hydroxide solution, reacting at 60 ℃ for 2 h, and carrying out solid-liquid separation after the reaction. And (3) carrying out alkaline leaching on the generated cuprous chloride slag, wherein an alkaline leaching agent is a sodium hydroxide solution with the mass fraction of 15%, the leaching temperature is 90 ℃, leaching is carried out for 2 h, after the alkaline leaching is finished, solid-liquid separation is carried out, the solid is activated cuprous oxide, the activated cuprous oxide is directly subjected to primary dechlorination and recycling, the liquid is evaporated and crystallized, and the sodium chloride is recovered.
Pumping the wastewater generated by primary dechlorination into a stirring tank, adding 350 Kg of lime, then adding 100 Kg of ferrous sulfate and 50 Kg of ferric sulfate salt, reacting for 1 h at normal temperature, wherein the pH value of the solution is about 7, carrying out solid-liquid separation after the reaction is finished, using the solid as a pyrometallurgical ore blending, and carrying out secondary dechlorination on liquid and sampling analysis. Sample analysis is shown in table 2 below.
TABLE 2 assay results (mg/L)
| Name (R) | Cd | Cr | Cu | Pb | Hg | As | Ni | Zn | Cl- | pH |
| Waste water | 1.01 | 0.15 | 1.23 | 2.25 | ＜0.005 | 2.75 | 0.59 | 9.98 | 1526 | 6.85 |
Pumping the primary heavy metal removal filtrate into a stirring tank, adding 24.5 Kg of lime and 42 Kg of sodium metaaluminate at the same time, reacting for 1 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, and carrying out secondary heavy metal removal on the liquid. Pumping the wastewater generated by secondary dechlorination into a stirring tank, adding ferric salt and sulfuric acid, adding 150 Kg of ferric salt, adding sulfuric acid to adjust the pH =7, reacting for 2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, sampling and analyzing the liquid, wherein the analysis is shown in the following table 3 and can be directly discharged.
TABLE 3 assay analysis results (mg/L)
| Name (R) | Cd | Cr | Cu | Pb | Hg | As | Ni | Zn | Cl- | pH |
| Efflux standard | ＜0.05 | ＜1.0 | ＜0.5 | ＜0.5 | ＜0.005 | ＜0.3 | ＜1.0 | ＜5.0 | —— | 6~9 |
| Waste water | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.005 | ＜0.01 | ＜0.01 | 0.052 | 452 | 7.35 |
Example 2:
case 1 acidic high-chlorine wastewater from nonferrous smelting 10 m3Pumping into a reaction tank, adding cuprous oxide obtained in the case 1, reacting at 60 ℃ for 1.5 h, and carrying out solid-liquid separation after the reaction is finished. And (3) carrying out alkaline leaching on the generated cuprous chloride slag, wherein an alkaline leaching agent is a sodium hydroxide solution with the mass fraction of 13%, the leaching temperature is 80 ℃, the leaching time is 2 h, after the alkaline leaching is finished, the solid-liquid separation is carried out, the solid is activated cuprous oxide, the activated cuprous oxide is directly subjected to primary dechlorination and recycling, the liquid is evaporated and crystallized, and the sodium chloride is recovered.
And pumping the wastewater generated by primary dechlorination into a stirring tank, adding 300 Kg of lime, then adding 90 Kg of ferrous sulfate and 60 Kg of ferric sulfate salt, reacting for 1 h at normal temperature, wherein the pH value of the solution is about 7, carrying out solid-liquid separation after the reaction is finished, using the solid as a pyrometallurgical ore blending, and carrying out secondary dechlorination on the liquid and sampling analysis. Sample analysis is shown in table 4 below.
TABLE 4 assay analysis results (mg/L)
| Name (R) | Cd | Cr | Cu | Pb | Hg | As | Ni | Zn | Cl- | pH |
| Waste water | 0.19 | 0.112 | 2.57 | 1.15 | ＜0.005 | 2.17 | 0.38 | 6.24 | 1324 | 7.01 |
Pumping the primary heavy metal removal filtrate into a stirring tank, adding 22.5 Kg of lime and 40 Kg of sodium metaaluminate at the same time, reacting for 1 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, and carrying out secondary heavy metal removal on the liquid. Pumping the wastewater generated by secondary dechlorination into a stirring tank, adding ferric salt and sulfuric acid, adding 130 Kg of ferric salt, adding sulfuric acid to adjust the pH =7, reacting for 2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, sampling and analyzing the liquid, wherein the analysis is shown in the following table 5 and can be directly discharged.
TABLE 5 assay results (mg/L)
| Name (R) | Cd | Cr | Cu | Pb | Hg | As | Ni | Zn | Cl- | pH |
| Efflux standard | ＜0.05 | ＜1.0 | ＜0.5 | ＜0.5 | ＜0.005 | ＜0.3 | ＜1.0 | ＜5.0 | —— | 6~9 |
| Waste water | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.01 | ＜0.005 | ＜0.01 | ＜0.01 | 0.034 | 402 | 6.81 |
Claims (5)
1. A method for comprehensively treating non-ferrous smelting acidic high-chlorine wastewater is characterized by comprising the following steps:
1) primary dechlorination: pumping the non-ferrous smelting acidic high-chlorine wastewater into a reaction tank, adding cuprous oxide, wherein the addition amount of the cuprous oxide is added according to the molar ratio of the copper content to the chlorine content in the wastewater, namely Cu/Cl = 1.1-1.3, the reaction temperature is 40-80 ℃, the reaction time is 1-3 h, and carrying out solid-liquid separation after the reaction is finished;
2) alkaline leaching: alkaline leaching is carried out on cuprous chloride slag generated by primary dechlorination, an alkaline leaching agent is a sodium hydroxide solution, the concentration of the sodium hydroxide solution is 10-15% of the mass fraction, the leaching temperature is 60-90 ℃, the leaching time is 0.5-2 h, after the alkaline leaching is finished, solid-liquid separation is carried out, the solid is activated cuprous oxide, the activated cuprous oxide is directly recycled for primary dechlorination, the liquid is evaporated and concentrated, and sodium chloride is recovered;
3) primary heavy metal removal: pumping the wastewater generated by primary dechlorination into a stirring tank, adding lime and ferric salt, wherein the adding amount of the lime is 20Kg/m3~100 Kg/m3The adding amount of the iron salt is 5 Kg/m3~30 Kg/m3Reacting for 0.5-2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, and carrying out secondary dechlorination on the liquid;
4) secondary dechlorination: pumping the primary heavy metal removal filtrate into a stirring tank, adding lime and sodium metaaluminate at the same time, adding the lime and the sodium metaaluminate according to the molar mass ratio of Ca to Al to Cl = (10-15): (3-4): 1, reacting for 0.5-2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, using the solid as pyrometallurgical ore blending, and carrying out secondary heavy metal removal on the liquid;
5) secondary heavy metal removal: pumping the wastewater generated by secondary dechlorination into a stirring tank, adding ferric salt and sulfuric acid, wherein the adding amount of the ferric salt is 10 Kg/m3~50 Kg/m3The addition amount of the sulfuric acid is 5 Kg/m3~20 Kg/m3And reacting for 0.5-2 h at normal temperature, carrying out solid-liquid separation after the reaction is finished, wherein the solid is used for pyrometallurgical ore blending, and the liquid can be directly discharged.
2. The method for comprehensively treating the non-ferrous smelting acidic high-chlorine wastewater as claimed in claim 1, wherein cuprous oxide is added, the first-used cuprous oxide must be activated for 2 hours by a sodium hydroxide solution with a mass concentration of 10% -15%, and the subsequent-used cuprous oxide is derived from cuprous oxide generated by the reaction of cuprous chloride and sodium hydroxide.
3. The method for comprehensively treating the non-ferrous smelting acidic high-chlorine wastewater according to claim 1 or 2, characterized in that the cuprous oxide is prevented from being deactivated by air oxidation by directly adding sodium hydroxide solution to alkaline leaching the cuprous chloride slag generated by primary dechlorination without drying, and directly recycling the alkaline slag without drying after leaching.
4. The method for comprehensively treating the acidic high-chlorine wastewater from nonferrous smelting according to claim 1 or 2, wherein the lime and iron salt added for removing the heavy metals at one time are composed of ferrous sulfate and ferric sulfate, and the weight ratio of the ferrous sulfate to the ferric sulfate is as follows: and (4) ferric sulfate = 1-3: 1, adding lime firstly, then adding ferric salt, and finally controlling the pH of the solution to be = 6-8.
5. The method for comprehensively treating the acidic high-chlorine wastewater from nonferrous smelting according to claim 1 or 2, characterized in that the sulfuric acid and the ferric salt added for the secondary heavy metal removal are sulfuric acid and ferric salt, the sulfuric acid is industrial 98% acid, the ferric salt is composed of ferrous sulfate and ferric sulfate, and the weight ratio of the components is ferrous sulfate: ferric sulfate =1: 1-5, ferric salt is added firstly, then sulfuric acid is added, and finally the pH of the solution is controlled to be = 6-8.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115845790A (en) * | 2022-11-02 | 2023-03-28 | 江苏理工学院 | Cuprous oxide/carbon nitride oxide composite material and preparation method and application thereof |
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