CN109110981B - Method for removing thallium from waste water containing high-halogen waste acid - Google Patents
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- 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
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- 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
A method for removing thallium from waste water containing high-halogen waste acid comprises the following steps: (1) carrying out defluorination treatment; (2) oxidation treatment; (3) carrying out vulcanization treatment; the method has the advantages of simple process flow and low treatment cost, is suitable for large-scale thallium removal treatment of the high-halogen waste acid-containing wastewater, the thallium removal rate reaches more than 99.9 percent, one section of waste residue generated in the treatment process does not contain heavy metal ions and can be used for general solid waste treatment, and the thallium content in the treated wastewater stably reaches the standard.
Description
Technical Field
The invention relates to the technical field of waste acid and wastewater treatment, in particular to a method for removing thallium from waste acid and wastewater containing high halogen content.
Background
In industries of metal smelting production, metal electrolysis, acid preparation by flue gas and the like, smelting flue gas contains a large amount of SO2And some harmful metal components, most smelting plants are provided with a two-conversion and two-absorption acid making system to realize smoke dust recovery and SO2Sulfuric acid is prepared, but a large amount of strong acid waste water containing heavy metals, namely waste acid, is generated in the process.
The treatment of the waste acid water from lead smelting has been a big problem mainly because the waste acid water contains more halogen ions such as fluorine and chlorine, and thallium has Tl in the waste acid water+And Tl3+Two forms, wherein, Tl3+Has strong coordination ability and can form stable complex with halogen ions, so the high fluorine chlorine ions existThe thallium removal difficulty is increased. In addition, Tl+The hydroxide TlOH is soluble in water and is generally difficult to remove by lime precipitation.
Currently, few thallium removal processes capable of realizing large-amount wastewater treatment in the lead smelting industry are available, and the Chinese patent CN201410685634.5 discloses a thallium removal process for washing waste acid wastewater by lead-zinc smelting flue gas, which comprises the steps of firstly carrying out homogenization tank sedimentation on the waste acid wastewater, primarily removing a large amount of smoke dust and other solids, then adding sulfide for mercury removal, adjusting the pH value of the waste acid wastewater after mercury removal to 9 through acid and alkali, sequentially adding sulfide and flocculant, and removing most thallium and heavy metal ions through filter pressing; adjusting the pH value of the supernatant purified water and the primary pressure clear liquid subjected to primary treatment to 11 by acid and alkali, sequentially adding sulfide and a flocculating agent, and deeply removing thallium and heavy metal ions in the supernatant purified water and the primary pressure clear liquid by inclined plate sedimentation. However, the method is suitable for removing low-content thallium and is not suitable for treating waste acid water with high fluorine, chlorine and thallium contents.
Chinese patent CN201611071686.9, a method for removing thallium by sections for high thallium content wastewater, the method adopts two stages of wastewater pretreatment and advanced treatment, wherein the wastewater pretreatment section mainly adopts an electrochemical homogenization tank to treat pretreated wastewater with thallium content less than or equal to 0.2mg/L, pH of 9-10; in the advanced treatment stage, the pretreated wastewater is pumped to a first-stage thallium removal reaction tank and flows through an electrochemical reaction system, an aeration tank, a flocculation reaction tank and the like for a series of treatments. The method has the advantages of excessively complex process, long wastewater treatment period and high electrochemical treatment cost, and is not suitable for large-scale industrial waste acid and wastewater treatment.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides the method for removing the thallium in the high-halogen-content waste acid wastewater, which has simple process flow and low treatment cost, and is suitable for large-scale industrial waste acid wastewater treatment.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for removing thallium from waste water containing high-halogen waste acid comprises the following steps: (1) carrying out defluorination treatment; (2) oxidation treatment; (3) carrying out vulcanization treatment;
further, the oxidation treatment includes two-stage oxidation.
Further, the defluorination treatment comprises: (1) adding calcium carbonate into the waste acid water, and simultaneously controlling the pH = 1.4-1.8 in the waste water; (2) stirring and reacting for more than 30 min; (3) and (3) filtering: and carrying out first-stage filter pressing.
Further, the first oxidation in the two-stage oxidation comprises: (1) adding ferrite and hydrogen peroxide into the clear liquid subjected to the first-stage filter pressing, wherein the solid-to-liquid ratio of the ferrite to the hydrogen peroxide is 1: 1-4, and simultaneously controlling the oxidation-reduction potential in the wastewater to be more than 500 mv; (2) stirring and reacting for more than 10 min; (3) adding lime to adjust the pH of the wastewater to be more than =11.5, and continuously reacting for more than 30 min; (3) and (3) filtering: and carrying out two-stage filter pressing.
Further, the secondary oxidation in the two-stage oxidation comprises: (1) adding dilute acid into the clear liquid after the second-stage filter pressing to adjust the pH = 1.5-3 of the wastewater; (2) adding ferrous salt and hydrogen peroxide, wherein the solid-to-liquid ratio of the ferrous salt to the hydrogen peroxide is 1: 1-4, and simultaneously controlling the oxidation-reduction potential to be more than 600 mv; (3) reacting for more than 30min, adding lime to adjust the pH of the wastewater to be 6-8, and continuing to react for more than 10 min; (4) and (3) filter pressing: carrying out three-stage filter pressing;
further, the vulcanization treatment includes: (1) adding alkali into the clear liquid obtained after the three-stage filter pressing to adjust the pH of the wastewater to be more than 11; (2) then adding sodium sulfide and an auxiliary thallium removal agent, and simultaneously controlling the oxidation-reduction potential to be below-300 mv; (3) reacting for more than 30 min; (4) and (3) filtering: and carrying out four-stage filter pressing.
Further, the solid-to-liquid ratio of the ferrous salt to the hydrogen peroxide in the first-stage oxidation is 1: 2.
Further, the filtration is carried out by adopting a membrane filter press.
Furthermore, the oxidation-reduction potential in the first-stage oxidation is 500 mv-600 mv.
Furthermore, the oxidation-reduction potential in the secondary oxidation is 600 mv-700 mv.
The technical scheme of the invention is mainly based on the principle that: the invention relates to a method for removing thallium from waste water containing high-halogen waste acid, which adopts a combined method of neutralization precipitation and sulfidization precipitation to remove thallium from the waste water containing high-halogen waste acid, wherein thallium is in the waste acidThe presence of Tl in the wastewater+And Tl3+Two forms, wherein, Tl3+Has strong coordination ability and can form stable coordination compound with halogen ions, so the thallium removal difficulty is increased due to the existence of high halogen in waste acid, therefore, the invention firstly carries out defluorination treatment on high halogen, reduces the interference of halogen ions to thallium removal, and then adopts two-stage oxidation to control the numerical value of oxidation-reduction potential, so that most thallium is converted into Tl (OH)3And removing the precipitate, removing residual thallium by a vulcanization method, and adding sodium sulfide and an auxiliary thallium removal agent to ensure that the thallium content in the treated wastewater stably reaches the standard.
Compared with the prior art, the invention has the advantages that: the method has the advantages of simple process flow and low treatment cost, is suitable for large-scale industrial high-halogen-content waste acid wastewater thallium removal treatment, the thallium removal rate reaches more than 99.9 percent, one section of waste residue generated in the treatment process does not contain heavy metal ions, the waste residue can be used as common solid waste for treatment, and the thallium content in the treated wastewater stably reaches the standard.
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FIG. 1 is a process flow diagram of the method for removing thallium from waste water containing high halogen content;
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention relates to a method for removing thallium from waste water containing high-halogen waste acid, which comprises the following steps: waste acid and waste water from lead smelting in certain place in Hunan provinceThe main component Tl in the wastewater is 17.36mg/L, F2.87.87 g/L, Cl 5.32.32 g/L, H2SO435.6g/L, and is treated by adopting the method for removing thallium from the high-halogen-content waste acid wastewater of the invention shown in figure 1, (1) defluorination treatment: slowly adding calcium carbonate into the waste acid water, detecting the pH value, controlling the pH value in the waste water to be 1.83 at the end point, stirring and reacting for 30min, and performing first-stage filter pressing by using a diaphragm filter press to obtain first-stage filter pressing clear liquid and first-stage slag with the water content of 26.7%; (2) primary oxidation: adding ferrous sulfate heptahydrate and hydrogen peroxide into the first-stage filter pressing clear liquid, wherein the solid-to-liquid ratio of the ferrous sulfate heptahydrate to the hydrogen peroxide is respectively 0:1, 1:1 and 1:2 (as shown in the proportion of the ferrous sulfate heptahydrate to the hydrogen peroxide in the table 1), controlling the oxidation-reduction potential to be 580mv, after reacting for 10min, adding lime to adjust the pH of the wastewater to be =11.58, and after reacting for 30min, performing second-stage filter pressing by using a membrane filter press to obtain second-stage filter pressing clear liquid and second-stage slag; (3) secondary oxidation: firstly, adjusting the pH =2.38 of the second-stage filter pressing clear liquid by using dilute acid, then adding ferrous sulfate heptahydrate and hydrogen peroxide, wherein the solid-to-liquid ratio of the ferrous sulfate heptahydrate to the hydrogen peroxide is 1:2, controlling the oxidation-reduction potential to be 650mv, fully oxidizing thallium into trivalent thallium, after reacting for 30min, then adding lime to adjust the pH =7.32, and after reacting for 10min, performing three-stage filter pressing by using a membrane filter press to obtain three-stage filter pressing clear liquid and three-stage slag; (4) adjusting the pH of the three-stage filter pressing clear liquid to be =11.89 by lime, adding sodium sulfide and auxiliary thallium removal agent portland cement, controlling the oxidation-reduction potential to be 300mv, enabling residual thallium to generate a thallium sulfide precipitate, reacting for 30min, and then carrying out four-stage filter pressing by using a membrane filter press to obtain four-stage filter pressing clear liquid and four-stage slag. Taking two-stage filter pressing filtration to measure the thallium content, and calculating the thallium removal rate. The results of the experiment are shown in table 1.
TABLE 1 comparison of the proportioning and consumption of ferrous sulfate heptahydrate and hydrogen peroxide solution in the first-stage oxidation
As can be seen from Table 1, thallium removal is not facilitated by adding no or more ferrous sulfate heptahydrate in the first-stage oxidation treatment, and when the solid-to-liquid ratio of ferrous sulfate heptahydrate to hydrogen peroxide is 1:2, the thallium removal effect in the two-stage filter-pressing clear liquid is the best, and the removal rate is 98.72%.
Further, taking four stages of filter-pressing clear liquid obtained under the experimental condition that the solid-to-liquid ratio of the ferrous sulfate heptahydrate to the hydrogen peroxide is 1:2, measuring to obtain that the thallium content is 1.565 mu g/L, and calculating the thallium removal rate to be 99.99%.
Example 2:
the invention relates to a method for removing thallium from waste water containing high-halogen waste acid, which comprises the following steps: the waste acid water from lead smelting in some place in Hunan province contains main component Tl 5.81mg/L, F3.22.22 g/L, Cl 4.85.85 g/L, H2SO443.8g/L, and is treated by adopting the method for removing thallium from the waste water containing high-halogen acid of the invention shown in figure 1, (1) defluorination treatment: slowly adding calcium carbonate into the waste acid water, detecting the pH value, controlling the pH value in the waste water to be 1.38 at the end point, stirring and reacting for 30min, and performing first-stage filter pressing by using a diaphragm filter press to obtain first-stage filter pressing filtration and first-stage slag with the water content of 24.3%; (2) primary oxidation: adding ferrous sulfate heptahydrate and hydrogen peroxide into the first-stage filter pressing clear liquid, wherein the solid-to-liquid ratio of the ferrous sulfate heptahydrate to the hydrogen peroxide is 1:2, controlling the oxidation-reduction potential to be 592mv, reacting for 10min, then adding lime to adjust the pH of the wastewater to be =11.83, reacting for 30min, and then carrying out second-stage filter pressing by using a diaphragm filter press to obtain second-stage filter pressing filter liquid and second-stage slag; (3) secondary oxidation: firstly, adjusting the pH =2.38 of the second-stage filter pressing clear liquid by using dilute acid, then adding ferrous sulfate heptahydrate and hydrogen peroxide, wherein the solid-to-liquid ratio of the ferrous sulfate heptahydrate to the hydrogen peroxide is 1:2, controlling the oxidation-reduction potential to 665mv to fully oxidize thallium into trivalent thallium, after reacting for 30min, adding lime to adjust the pH =6.7, and after reacting for 10min, performing three-stage filter pressing by using a membrane filter press to obtain three-stage filter pressing clear liquid and three-stage slag; (4) adjusting the pH =11.82 of the three-stage filter-pressing clear liquid by lime, adding sodium sulfide and an auxiliary thallium removal agent, controlling the oxidation-reduction potential to be-345 v, enabling residual thallium to generate a thallium sulfide precipitate, reacting for 30min, and then carrying out four-stage filter pressing by using a diaphragm filter press to obtain four-stage filter-pressing clear liquid and four-stage slag. The four stages of filter-pressed clear liquid are taken, the thallium content is measured to be 2.767 mug/L, and the calculated thallium removal rate is 99.95 percent.
It should be noted that, those skilled in the art may also choose to use other chemical agents to adjust the pH, such as calcium hypochlorite, sodium hydroxide, etc., and other ferrous salts, such as ferrous chloride, as needed; ferrous carbonate, and the like, and the auxiliary thallium removal agent can also be common portland cement containing one or more of tricalcium silicate, dicalcium silicate, tricalcium aluminate or tetracalcium aluminoferrite.
The above description of the specific embodiments of the present invention is not intended to limit the present invention, and those skilled in the art can make various modifications and changes to the composition ratio of the components according to the technical principle and principle of the present invention, and also fall within the scope of the claims of the present invention, as long as the technical principle and principle of the present invention are not departed from.
Claims (5)
1. A method for removing thallium from waste water containing high-halogen acid comprises the steps of (1) defluorination treatment, (2) oxidation treatment and (3) vulcanization treatment, and is characterized in that,
the defluorination treatment comprises the following steps: adding calcium carbonate into the waste acid water, controlling the pH = 1.4-1.8 in the waste water, stirring and reacting for more than 30min, and then carrying out first-stage filter pressing;
the oxidation treatment comprises two-stage oxidation, wherein the first-stage oxidation in the two-stage oxidation comprises the following steps: adding ferrous salt and hydrogen peroxide into the clear liquid after the first-stage filter pressing, wherein the solid-to-liquid ratio g of the ferrous salt to the hydrogen peroxide is as follows: 1: 1-4 mL, controlling the oxidation-reduction potential in the wastewater to be more than 500mV, stirring and reacting for more than 10min, adding lime to adjust the pH of the wastewater to be more than =11.5, continuously reacting for more than 30min, and then carrying out two-stage filter pressing;
the secondary oxidation in the two-stage oxidation comprises the following steps: adding dilute acid into the clear liquid obtained after the second-stage filter pressing to adjust the pH = 1.5-3, and then adding ferrite and hydrogen peroxide, wherein the solid-to-liquid ratio g of the ferrite to the hydrogen peroxide is as follows: the mL is 1: 1-4, the oxidation-reduction potential is controlled to be more than 600mV, the reaction is carried out for more than 30min, lime is added to adjust the pH = 6-8 of the wastewater, the reaction is continued for more than 10min, and then three-stage filter pressing is carried out;
the vulcanization treatment comprises the following steps: adding alkali into the clear liquid obtained after three-stage filter pressing to adjust the pH of the wastewater to be more than =11, adding sodium sulfide and an auxiliary thallium removal agent, controlling the oxidation-reduction potential to be less than-300 mV, reacting for more than 30min, and then carrying out four-stage filter pressing.
2. The method for removing thallium from waste water containing high halogen content acid as claimed in claim 1, characterized in that: the solid-liquid ratio g: mL of the ferrous salt and the hydrogen peroxide in the first-stage oxidation is 1: 2.
3. The method for removing thallium from waste water containing high halogen content acid as claimed in claim 1, characterized in that: the oxidation-reduction potential in the first-stage oxidation is 500 mV-600 mV.
4. The method for removing thallium from waste water containing high halogen content acid as claimed in claim 1, characterized in that: the oxidation-reduction potential in the secondary oxidation is 600 mV-700 mV.
5. The method for removing the thallium from the waste water containing high halogen content acid as claimed in any one of claims 1-4, characterized by that: and the filter pressing is carried out by adopting a diaphragm filter press.
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| CN114735857B (en) * | 2022-05-13 | 2023-08-25 | 甘肃厂坝有色金属有限责任公司 | Lead-zinc smelting industrial waste acid and sewage treatment process |
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Inventor after: Fu Gaoming Inventor after: Fu Linlin Inventor after: Huang Anping Inventor after: Chen Guolan Inventor after: Bai Chengqing Inventor before: Fu Gaoming Inventor before: Fu Linlin Inventor before: Chen Guolan Inventor before: Bai Chengqing |