CN115180787A - Method for stabilizing thallium-containing sludge - Google Patents
Method for stabilizing thallium-containing sludge Download PDFInfo
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- CN115180787A CN115180787A CN202210964379.2A CN202210964379A CN115180787A CN 115180787 A CN115180787 A CN 115180787A CN 202210964379 A CN202210964379 A CN 202210964379A CN 115180787 A CN115180787 A CN 115180787A
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/06—Treatment of sludge; Devices therefor by oxidation
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/008—Sludge treatment by fixation or solidification
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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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Abstract
The invention belongs to the technical field of solid waste treatment, and discloses a method for stably treating thallium-containing sludge. The method comprises the following steps: (1) Adding an oxidant into the thallium-containing sludge, and stirring and reacting until the oxidation is complete; (2) Adding a curing agent into the mixed solution treated in the step (1), adding alkali to adjust the pH value to 10-14, carrying out a fixed reaction at the temperature of 120-140 ℃, and carrying out solid-liquid separation on the material after the reaction is finished to obtain a fixed liquid and a cured product; the curing agent is K 3 PO 4 、Na 2 SiO 3 One or a combination of both. The solidifying agent used by the method is cheap and easy to obtain, the process operation is convenient, the stabilizing effect on thallium and the rest heavy metals is good, and the method has important practical significance in the field of hazardous waste treatment and disposal.
Description
Technical Field
The invention belongs to the technical field of solid waste treatment, and particularly relates to a method for stabilizing thallium-containing sludge.
Background
Thallium is a rare metal and is often associated with metals such as lead and zinc in sulphide minerals. With the increase of the exploitation amount of lead and zinc mineral resources, the originally dispersed thallium is gradually enriched after the smelting process. Most thallium is enriched into flue gas in the smelting process, and enters waste acid wastewater after the flue gas is purified, so that the total thallium concentration is relatively high. In order to remove the concentration of thallium and other heavy metals in the contaminated acid, the sulfide precipitation method can effectively remove a large amount of heavy metals in a mode of adding a vulcanizing agent into the contaminated acid-containing wastewater to generate insoluble sulfide precipitation, and is widely applied to thallium-containing wastewater treatment.
However, at the same time, the industrial application of the sulfide precipitation method is also accompanied with the mass production of thallium-containing sludge, and the sludge produced by the method has thallium which is mainly present as monovalent ions and is easy to dissolve in water, and the direct stacking brings serious thallium pollution. At present, the method for stabilizing thallium-containing solid waste comprises the following steps: CN107486464A a disposal method for thallium-containing solid waste, which utilizes polyacrylate emulsion, ethylene vinyl acetate copolymer emulsion, cement to mix to prepare thermosetting encapsulating material; and (4) carrying out mixed curing on the solidified material and the thallium-containing solid waste to finish the disposal of the thallium-containing solid waste. The method only realizes the wrapping curing of thallium-containing solid waste, does not consider the problem of migration of monovalent thallium, has insufficient stability of cured products, large capacity increase and large occupied space for stockpiling. CN110203995A discloses a thallium pollution advanced curing agent and a preparation method and application thereof, wherein a silicon-aluminum mineral, a calcium-magnesium adjuvant and a fluxing agent are uniformly mixed, and an active aluminum silicate material is obtained after roasting; and adding water and an oxidant into the active aluminum silicate material, uniformly mixing, and drying and crushing the obtained slurry to obtain the thallium-polluted deep curing agent. The thallium pollution deep curing agent prepared by the method is applied to thallium pollution treatment, and can be stably combined with thallium and a thallium compound to form an insoluble substance, so that the effect of efficiently, permanently and stably curing pollution source thallium is achieved. However, the components and the preparation method of the curing agent are complex and the cost is high.
In view of the shortcomings of the prior art for stabilizing thallium-containing sludge, a method for stabilizing thallium-containing sludge is needed to solve or at least alleviate the above technical shortcomings.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a method for stabilizing thallium-containing sludge. The solidifying agent used by the method is cheap and easy to obtain, the process is convenient to operate, and the stabilizing effect on thallium and the rest heavy metals is good.
The purpose of the invention is realized by the following technical scheme:
a method for stabilizing thallium-containing sludge comprises the following steps:
(1) Adding an oxidant into the thallium-containing sludge, and stirring and reacting until the oxidation is complete;
(2) Adding a curing agent into the mixed solution treated in the step (1), adding alkali to adjust the pH value to 10-14, carrying out a fixation reaction at the temperature of 120-140 ℃, and carrying out solid-liquid separation on the material after the reaction is finished to obtain a fixed liquid and a cured product; the curing agent is K 3 PO 4 、Na 2 SiO 3 Or a combination of both.
Further, the thallium-containing sludge in the step (1) is heavy metal sulfide sludge precipitated by adding sulfides in the treatment of smelting acidic wastewater or residual bottom slag after thallium is recovered from the thallium-containing sludge.
Further, the thallium-containing sludge in the step (1) contains the following heavy metal components in percentage by mass: 0.01 to 5 percent of thallium, 5 to 15 percent of lead, 3 to 10 percent of cadmium and 1 to 5 percent of zinc.
Further, the oxidizing agent in the step (1) is preferably a hydrogen peroxide solution having a mass concentration of 1% to 30%.
Further, the oxidant is added in the step (1) in a dropwise manner, and the adding amount of the oxidant is controlled to be 1-5.
Further, the stirring reaction in the step (1) is carried out at normal temperature at a stirring speed of 300-800 rpm for 30-60 min.
Further preferably, the curing agent in the step (2) is K 3 PO 4 And Na 2 SiO 3 Combinations of (a) and (b).
Further, the adding amount of the curing agent in the step (2) is 1-20% of the mass of the thallium-containing sludge.
Further, the time of the fixed reaction in the step (2) is 12-24 h.
Furthermore, the solidified product thallium in the step (2) has low leaching toxicity, can be directly sent to a landfill site for landfill, has very little heavy metal content in the fixed liquid, and can directly enter a wastewater treatment system.
The main principle of the invention comprises:
①Tl + + oxidizing agent → Tl 3+
Common valence states of thallium are monovalent and trivalent, wherein monovalent thallium has extremely high mobility and few insoluble compounds, and conversely trivalent thallium has very low mobility and compounds that precipitate poorly.
②Zn/Cd/PbS+PO 4 3- +OH - → Zn/Cd/Pb-apatite ↓
Zn/Cd/PbS+Na 2 SiO 3 → silicate mineral/SiO 2 ↓
As trivalent thallium is easily reduced to transportable monovalent thallium in the natural environment, secondary thallium wrapping is realized by means of insoluble minerals of other heavy metals in the residue, wherein the solubility of apatite is as low as 10 -50 . In addition, the silicate mineral is wrapped on the solid surface, so that the structure of the cured product is further stabilized.
Compared with the prior art, the invention has the beneficial effects that:
(1) The oxidant used in the invention is hydrogen peroxide, so that new impurities are prevented from being introduced in the treatment process, secondary pollution is avoided, the process operation is convenient, and the reaction condition is mild.
(2) The method provided by the invention realizes fixation by utilizing different properties of heavy metal compounds in sludge, firstly, high-mobility monovalent thallium is oxidized into a trivalent thallium compound with insoluble precipitation, then, other heavy metal insoluble precipitation is utilized to wrap the thallium compound, secondary wrapping is realized, a highly stable solid precipitate can be formed after treatment, and the volume of the sludge cannot be increased.
(3) The method provided by the invention has wide application range, is especially suitable for high-concentration thallium-containing sludge, has the advantages of economy, environmental protection, short process flow and the like, has wide actual industrial application prospect, and has important practical significance in the field of hazardous waste treatment and disposal.
Drawings
FIG. 1 shows the different concentrations of K in example 1 3 PO 4 A thallium leaching concentration change diagram of the fixed product;
FIG. 2 shows the concentrations of K in example 1 3 PO 4 Phase diagram of the solidified product after fixation;
FIG. 3 shows the different Na concentrations in example 2 2 SiO 3 A thallium leaching concentration change diagram of the fixed product;
FIG. 4 shows the different Na concentrations in example 2 2 SiO 3 Phase diagram of the fixed cured product.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
In this example, thallium-containing sludge of a lead-zinc ore smelting plant is taken as an example (containing thallium content of 3.5%, lead content of 6.9%, cadmium content of 5.4%, and zinc content of 1.7%) and compared with different K dosages 3 PO 4 The influence of the curing agent on Tl leaching toxicity in the high-concentration thallium-containing sludge is that the thallium leaching toxicity of the original thallium-containing sludge is as high as 760mg/L, and the specific process is as follows:
(1) 30g of thallium-containing sludge is weighed into a reaction kettle, 30ml of hydrogen peroxide (30%) is continuously dripped into the reaction kettle through a peristaltic pump, the mixture is fully stirred (400 rpm) and uniformly mixed, and after the dripping of the oxidant is finished, the mixture is fully stirred and reacts for 30min to ensure complete oxidation.
(2) Adding K into the mixed solution treated in the step (1) 3 PO 4 The addition amounts were 0.636g, 1.908g, 3.18g, 4.452g, 6.36g, respectively, while adding NaOH solution to adjust the pH to 14, and heating to 140 ℃ to perform a fixation reaction for 18h.And carrying out solid-liquid separation on the materials after the reaction is finished to obtain the fixed liquid and the fixed product.
According to the standard of sulfuric acid-nitric acid method (HJ/T299-2007) of solid waste leaching toxicity leaching method, a Tl toxicity leaching test is carried out by adopting a turnover type oscillator. The leaching toxicity of thallium-containing sludge thallium is as high as 760mg/L, and after the hydrothermal curing reaction of the embodiment, different K 3 PO 4 The leaching concentration of thallium is respectively reduced to 3.52mg/L, 4.23mg/L, 2.41mg/L, 1.68mg/L and 0.632mg/L under the adding amount condition, as shown in figure 1, and the leaching toxicity of other heavy metal elements is lower than the detection limit. It can be seen that with K 3 PO 4 The more the added amount is gradually increased, the better the thallium fixation effect is. The fixation rate of thallium obtained by analyzing and calculating the element content of the solidified product can reach 97.6 percent, and the fixation effect is obvious. Phase analysis of the cured product, as shown in FIG. 2, can be seen with K 3 PO 4 The more the amount of apatite mineral is increased, the better the crystallinity of apatite mineral.
Example 2
In this example, thallium-containing sludge (containing 3.5% thallium, 6.9% lead, 5.4% cadmium, and 1.7% zinc as heavy metal components) in a certain lead-zinc ore smelter is compared with different Na dosages 2 SiO 3 The influence of the curing agent on Tl leaching toxicity in the high-concentration thallium-containing sludge is that the thallium leaching toxicity of the original thallium-containing sludge is as high as 760mg/L, and the specific process is as follows:
(1) 30g of thallium-containing sludge is weighed into a reaction kettle, 30ml of hydrogen peroxide (30%) is continuously dripped into the reaction kettle through a peristaltic pump, the mixture is fully stirred (400 rpm) and uniformly mixed, and after the dripping of the oxidant is finished, the mixture is fully stirred and reacts for 30min to ensure complete oxidation.
(2) Adding Na into the mixed solution treated in the step (1) 2 SiO 3 The addition amounts were 0.366g, 0.732g, 1.098g, and 1.83g, respectively, while adding NaOH solution to adjust pH to 14, and heating to 140 ℃ to perform immobilization reaction for 18h. And carrying out solid-liquid separation on the materials after the reaction is finished to obtain the fixed liquid and the fixed product.
According to the standard of 'solid waste leaching toxicity leaching sulfuric acid-nitric acid method' (HJ/T299-2007), tl toxicity is carried out by adopting a turnover type oscillatorAnd (4) performing a sexual leaching test. The leaching toxicity of thallium-containing sludge is as high as 760mg/L, the leaching concentrations of thallium are respectively reduced to 14.32mg/L, 10.78mg/L, 6.62mg/L and 2.32mg/L after the hydrothermal curing reaction in the embodiment, and as shown in FIG. 3, the leaching toxicity of other heavy metal elements is lower than the detection limit. It can be seen that along with Na 2 SiO 3 The more the added amount is gradually increased, the better the thallium fixation effect is. The fixation rate of thallium obtained by analyzing and calculating the element content of the solidified product can reach 96.3%, and the fixation effect is obvious. Phase analysis of the cured product was carried out, as can be seen from FIG. 4, along with Na 2 SiO 3 The more the silicate mineral crystallinity is better when the adding amount is gradually increased.
Example 3
In this embodiment, taking thallium-containing sludge from a lead-zinc ore smeltery as an example (containing 3.5% of thallium, 6.9% of lead, 5.4% of cadmium, and 1.7% of zinc as heavy metal components), comparing the influence of different curing agents on the Tl leaching toxicity in high-concentration thallium-containing sludge, the leaching toxicity of thallium-containing sludge in the prior art is as high as 760mg/L, and the specific process is as follows:
(1) 30g of thallium-containing sludge is weighed in a reaction kettle, 30ml of hydrogen peroxide (30%) is continuously dripped by a peristaltic pump, the mixture is fully stirred (400 rpm) and uniformly mixed, and after the dripping of the oxidant is finished, the mixture is fully stirred and reacts for 30min to ensure complete oxidation.
(2) Respectively adding 2.0gK into the mixed solution treated in the step (1) 3 PO 4 、2.0gNa 2 SiO 3 And 1.0gK 3 PO 4 +1.0gNa 2 SiO 3 Adding NaOH solution to adjust the pH value to 14, and heating to 140 ℃ to carry out a fixation reaction for 18h. And (4) performing solid-liquid separation on the reacted material to obtain a fixed liquid and a fixed product.
According to the standard of sulfuric acid-nitric acid method (HJ/T299-2007) of solid waste leaching toxicity leaching method, a Tl toxicity leaching test is carried out by adopting a turnover type oscillator. After hydrothermal curing reaction, the leaching concentration of thallium is respectively reduced to 2.12mg/L, 2.08mg/L and 1.32mg/L, and the leaching toxicity of other heavy metal elements is lower than the detection limit.
From the above results, it can be seen that K is equal to the amount of the curing agent 3 PO 4 +Na 2 SiO 3 In comparison with K alone 3 PO 4 And Na 2 SiO 3 The fixation effect on thallium in the high-concentration thallium-containing sludge is better. Under the requirement of the same fixing effect, the dosage of the curing agent can be obviously reduced.
Example 4
In this embodiment, taking the circulating bottom slag remaining after thallium is recovered from thallium-containing sludge in a lead-zinc ore smelting plant as an example (containing 0.07% of thallium, 11.2% of lead, 4.7% of cadmium, and 1.1% of zinc), comparing the influence of different curing agents on Tl leaching toxicity in low-concentration thallium-containing sludge, the leaching toxicity of thallium-containing sludge is 34mg/L, and the specific process is as follows:
(1) 30g of thallium-containing sludge is weighed in a reaction kettle, 30ml of hydrogen peroxide (30%) is continuously dripped by a peristaltic pump, the mixture is fully stirred (400 rpm) and uniformly mixed, and after the dripping of the oxidant is finished, the mixture is fully stirred and reacts for 30min to ensure complete oxidation.
(2) Respectively adding 0.72gK into the mixed solution treated in the step (1) 3 PO 4 、0.72gNa 2 SiO 3 And 0.36gK 3 PO 4 +0.36gNa 2 SiO 3 Adding NaOH solution to adjust the pH value to 14, and heating to 140 ℃ to carry out a fixation reaction for 18h. And (4) performing solid-liquid separation on the reacted material to obtain a fixed liquid and a fixed product.
According to the standard of sulfuric acid-nitric acid method (HJ/T299-2007) of solid waste leaching toxicity leaching method, a Tl toxicity leaching test is carried out by adopting a turnover type oscillator. After hydrothermal curing reaction, the leaching concentration of thallium is respectively reduced to 0.1255mg/L, 0.1524mg/L and 0.0829mg/L, and the leaching toxicity of other heavy metal elements is lower than the detection limit.
From the above results, it can be seen that K is equal to the amount of the curing agent 3 PO 4 +Na 2 SiO 3 In comparison with K alone 3 PO 4 And Na 2 SiO 3 The fixation effect on thallium in the low-concentration thallium-containing sludge is better. Under the requirement of the same fixing effect, the dosage of the curing agent can be obviously reduced.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for stabilizing thallium-containing sludge is characterized by comprising the following steps:
(1) Adding an oxidant into the thallium-containing sludge, and stirring and reacting until the oxidation is complete;
(2) Adding a curing agent into the mixed solution treated in the step (1), adding alkali to adjust the pH value to 10-14, carrying out a fixed reaction at the temperature of 120-140 ℃, and carrying out solid-liquid separation on the material after the reaction is finished to obtain a fixed liquid and a cured product; the curing agent is K 3 PO 4 、Na 2 SiO 3 Or a combination of both.
2. The method for stabilizing thallium-containing sludge according to claim 1, wherein the thallium-containing sludge in step (1) is heavy metal sulfide sludge precipitated by adding sulfide to the smelting acidic wastewater or bottom slag left after thallium is recovered from the thallium-containing sludge.
3. The method for stabilizing thallium-containing sludge according to claim 2, wherein the thallium-containing sludge contains the following heavy metal components in percentage by mass: 0.01 to 5 percent of thallium, 5 to 15 percent of lead, 3 to 10 percent of cadmium and 1 to 5 percent of zinc.
4. The method for stabilizing thallium-containing sludge according to claim 1, wherein the oxidizing agent in step (1) is a hydrogen peroxide solution with a mass concentration of 1% to 30%.
5. The method for stabilizing thallium-containing sludge according to claim 4, wherein the oxidant is added dropwise, and the addition amount of the oxidant is controlled to be 1-5.
6. The method for stabilizing thallium-containing sludge according to claim 1, wherein the stirring reaction in step (1) is performed at normal temperature, at a stirring speed of 300-800 rpm, and for a reaction time of 30-60 min.
7. The method of claim 1, wherein the curing agent is K 3 PO 4 And Na 2 SiO 3 Combinations of (a) and (b).
8. The method for stabilizing thallium-containing sludge according to claim 1, wherein the addition amount of the curing agent is 1-20% of the thallium-containing sludge.
9. The method for stabilizing thallium-containing sludge according to claim 1, wherein the time for the fixation reaction in step (2) is 12-24 h.
10. The method for stabilizing thallium-containing sludge according to claim 1, wherein the solidified product in the step (2) is sent to a landfill, and the liquid after fixation is sent to a wastewater treatment system.
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| CN202210964379.2A CN115180787B (en) | 2022-08-11 | 2022-08-11 | Method for stabilizing thallium-containing sludge |
| ZA2023/01187A ZA202301187B (en) | 2022-08-11 | 2023-01-30 | Method for stabilizing thallium-containing sludge |
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Citations (5)
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| JP2008036470A (en) * | 2006-08-01 | 2008-02-21 | Dowa Holdings Co Ltd | Thallium-containing iron/arsenic compound and its production method, and treatment method of aqueous arsenic/thallium-containing solution |
| CN204198537U (en) * | 2014-10-27 | 2015-03-11 | 湖南净源环境工程有限公司 | Waste water containing thallium Strong oxdiative coagulation and sedimentation integrated device |
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| CN107285581A (en) * | 2017-07-25 | 2017-10-24 | 云南大地绿坤环保科技有限公司 | A kind of processing method of multivalent state dreg containing arsenic |
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2022
- 2022-08-11 CN CN202210964379.2A patent/CN115180787B/en active Active
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- 2023-01-30 ZA ZA2023/01187A patent/ZA202301187B/en unknown
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| JP2008036470A (en) * | 2006-08-01 | 2008-02-21 | Dowa Holdings Co Ltd | Thallium-containing iron/arsenic compound and its production method, and treatment method of aqueous arsenic/thallium-containing solution |
| CN204198537U (en) * | 2014-10-27 | 2015-03-11 | 湖南净源环境工程有限公司 | Waste water containing thallium Strong oxdiative coagulation and sedimentation integrated device |
| CN104528985A (en) * | 2014-12-09 | 2015-04-22 | 湖南沐坤环保股份有限公司 | Method for removing metal thallium in wastewater |
| CN105293775A (en) * | 2015-11-19 | 2016-02-03 | 湖南力泓新材料科技股份有限公司 | Method adopting combined technology of pre-oxidation and coagulating sedimentation to process wastewater containing thallium and ammonia-nitrogen |
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| ZA202301187B (en) | 2023-05-31 |
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