CN113336356A - Phosphogypsum leachate recycling treatment and utilization method - Google Patents
Phosphogypsum leachate recycling treatment and utilization method Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- 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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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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Abstract
The invention discloses a resource treatment and utilization method of phosphogypsum leachate, which comprises the steps of adding hydroxide into the phosphogypsum leachate to adjust the pH value to be 4-5, stirring for reaction to remove part of metal ions and impurities in the solution, and filtering to remove precipitates; adding oxalic acid into the obtained filtrate, adjusting the pH value of the solution to 6 by using hydroxide, stirring to react calcium ions with the oxalic acid to generate calcium oxalate, and filtering to remove precipitates; the obtained filtrate enters a fluidized bed induced crystallization reactor, the pH value is adjusted to 8-10 by using hydroxide solution, ammonia nitrogen wastewater and magnesium oxide are added for reaction, and high-purity magnesium ammonium phosphate crystals are obtained after filtration and drying; removing fluorine element from the obtained filtrate through membrane treatment; stirring the obtained filtrate and the traditional Chinese medicine residue adsorbing material to react so as to remove arsenic; and treating tail water of the obtained filtrate to ensure that the filtrate reaches the discharge standard.
Description
Technical Field
The invention belongs to the technical field of environmental engineering, and particularly relates to a resource treatment and utilization method of phosphogypsum leachate.
Background
The phosphogypsum leachate is formed by stacking and percolating a byproduct phosphogypsum generated in the process of producing phosphoric acid by a wet method, the source of the leachate can be mainly divided into two parts, one part is water carried by the phosphogypsum when the phosphogypsum is placed in a storage yard, and the other part is caused by natural rainfall, and the leachate is mainly characterized by strong acidity, contains phosphorus, fluoride, sulfuric acid, calcium, magnesium, heavy metals of arsenic, lead and the like, and is easy to cause serious pollution to the environment such as surface water, underground water, soil and the like. At present, the treatment of the phosphogypsum leachate mainly comprises a neutralization precipitation method, a chemical coagulation method and a closed cyclic utilization method, the chemical method is easy to generate a large amount of solid waste and generate secondary pollution, the closed cyclic utilization of the leachate can corrode pipeline equipment, and the quality of phosphoric acid is reduced due to circulating fluorine, arsenic, lead and the like.
Disclosure of Invention
The invention aims to provide a resource treatment and utilization method of phosphogypsum leachate, which realizes resource utilization of phosphorus elements in phosphogypsum; the invention also aims to simultaneously treat harmful elements such as fluorine and arsenic in the leachate so that the final water body reaches the discharge standard and is recycled.
In order to achieve the purpose, the technical scheme is as follows:
a resource treatment and utilization method of phosphogypsum leachate comprises the following steps:
1) pretreatment of phosphogypsum leachate: adding hydroxide into the phosphogypsum leachate to adjust the pH value to be 4-5, stirring for reaction to remove part of metal ions and impurities in the solution, and filtering to remove precipitates; adding oxalic acid into the obtained filtrate, adjusting the pH value of the solution to 6 by using hydroxide, stirring to react calcium ions with the oxalic acid to generate calcium oxalate, and filtering to remove precipitates;
2) resource utilization of phosphorus: the filtrate obtained in the step 1 enters a fluidized bed induced crystallization reactor, the pH value is adjusted to 8-10 by using hydroxide solution, ammonia nitrogen wastewater and magnesium oxide are added for reaction, and high-purity magnesium ammonium phosphate crystals are obtained after filtering and drying;
3) removing fluorine element: removing fluorine elements from the filtrate obtained in the step 2 through membrane treatment;
4) removing arsenic element: stirring the filtrate obtained in the step (3) and the traditional Chinese medicine residue adsorbing material for reaction to remove arsenic;
5) tail water treatment: and (4) treating tail water of the filtrate obtained in the step (4) to enable the filtrate to reach the discharge standard.
According to the scheme, the hydroxide in the step 1 is a 30 wt% sodium hydroxide solution.
According to the scheme, the reaction process of the stage of removing the metal ions and impurities in the step 1 is stirring reaction at normal temperature for 10-20 min; the reaction process of the calcium removal stage is stirring reaction at normal temperature for 20-30 min.
According to the scheme, the hydroxide is a sodium hydroxide solution with the mass fraction of 30 wt% in the step 2); the ammonia nitrogen concentration in the ammonia nitrogen wastewater is 3000-3100 mg/L; controlling the reaction system to have N: mg: the molar ratio of P is 1.1:1.2: 1.
According to the scheme, the ammonia nitrogen wastewater in the step 2 is ammonia nitrogen circulating wastewater for intermittently preparing the semi-water gas.
According to the scheme, in the step 2, the reaction is carried out for 20-40min in a fluidized bed induced crystallization reactor at normal temperature.
According to the scheme, the stirring reaction time of the step 4 is 1.5-2.5 h; the preparation process of the traditional Chinese medicine residue adsorbing material is as follows:
adding Chinese medicinal residue into FeCl3Stirring, filtering and drying the solution for later use.
The invention has the following beneficial effects:
the method for utilizing the defluorination and heavy phosphorus removal resources of the phosphogypsum leachate takes the leachate of a phosphogypsum storage yard as a raw material to carry out chemical reaction, fully utilizes the phosphorus in the leachate, simultaneously removes arsenic and fluorine elements harmful to the environment in the leachate, and reduces the pollution to surface water, underground water and soil environment.
The invention implements the concept of 'treating waste by waste', realizes the resource utilization of valuable element phosphorus by the reaction of ammonia nitrogen wastewater and phosphogypsum percolate, simultaneously reduces the discharge of solid waste by applying the traditional Chinese medicine residue of waste gas in the arsenic removal process, and has great environmental protection benefit.
The method has the advantages of simple process, low cost, high utilization rate of phosphorus and high removal rate of pollution elements, and provides a practical and reliable treatment process for the industry.
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FIG. 1: the invention relates to a phosphogypsum leachate recycling treatment and utilization process flow chart.
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
The resource treatment and utilization method of the phosphogypsum leachate is shown in the attached figure 1:
1) pretreatment of phosphogypsum leachate: adding hydroxide into the phosphogypsum leachate in a neutralization regulating tank to regulate the pH value to be 4-5, stirring for reaction to remove partial metal ions and impurities in the solution, and filtering to remove precipitates; adding oxalic acid into the obtained filtrate in a sedimentation tank, adjusting the pH value of the solution to 5-6 by using hydroxide, stirring for reaction to enable calcium ions to react with the oxalic acid to generate calcium oxalate, and filtering to remove sediment;
2) resource utilization of phosphorus: the filtrate obtained in the step 1 enters a fluidized bed induced crystallization reactor, the pH value is adjusted to 8-10 by using hydroxide solution, ammonia nitrogen wastewater and magnesium oxide are added for reaction, and high-purity magnesium ammonium phosphate crystals are obtained after filtering and drying; the hydroxide is a sodium hydroxide solution with the mass fraction of 30 wt%; the ammonia nitrogen concentration in the ammonia nitrogen wastewater is 3000-3100 mg/L; controlling the reaction system to have N: mg: the molar ratio of P is 1.1:1.2: 1.
3) Removing fluorine element: removing fluorine elements from the filtrate obtained in the step 2 through membrane treatment; the membrane treatment process adopts a filtration design with a DTRO disc tube type reverse osmosis membrane as a core, percolate passes through a gap between a membrane stack and a shell and then enters a bottom diversion disc through a diversion channel, the treated liquid rapidly flows through a filtration membrane at the shortest distance, then is reversed to the other membrane surface by 180 degrees and then flows into the next filtration membrane, so that tangential flow filtration from the periphery of the diversion disc to the center of the circle, then to the periphery and then to the center of the circle is formed on the surface of the membrane, and the effect of efficient defluorination and desalination is achieved.
4) Removing arsenic element: stirring the filtrate obtained in the step (3) and the traditional Chinese medicine residue adsorbing material for reaction to remove arsenic; chinese medicine residue adsorption materialThe preparation process of the material is as follows: adding Chinese medicinal residue into FeCl3Stirring and filtering the solution, and drying the Chinese medicine residue for later use; the stirring time is 12 hours, the stirring temperature is 40 ℃, the drying temperature is 80 ℃, and the drying time is 5 hours.
5) Tail water treatment: and (4) treating tail water of the filtrate obtained in the step (4) to enable the filtrate to reach the discharge standard.
The main component of the phosphogypsum leachate used in the embodiment of the invention is phosphorus (expressed as H)3PO4、H2PO4 -、HPO4 2-Type existing), Ca2+、SO4 2-While less soluble Ca may be present in the leachate3(PO4)2Or eutectic phosphorus and fluorine (mainly soluble NaF and insoluble CaF)2、Na2SiF6Two types of fluorides), alkali metal salt (the alkali metal compound in phosphorite reacts with sulfuric acid to form new sulfate compound), part of special elements (such As metalloid element As and radioactive element radium, etc.) and insoluble particulate matters.
Example 1
1) Adding a proper amount of 30% sodium hydroxide solution into the phosphogypsum leachate to remove part of impurities, adjusting the pH value of the solution to 4-5, stirring and reacting for 10-20min at normal temperature, filtering after the reaction is finished, and keeping the filtrate.
2) Adding oxalic acid into the obtained filtrate, wherein the adding amount is that the molar ratio of the oxalic acid to the calcium is 1.3: 1, stirring and reacting at normal temperature, adjusting the pH value of the solution to 5-6 by using a sodium hydroxide solution, stirring and reacting for 20-30min, and filtering after the reaction is finished to obtain calcium oxalate and filtrate.
3) Adding ammonia nitrogen wastewater and magnesium oxide into the obtained filtrate in a fluidized bed induced crystallization reactor, wherein the adding amount is controlled to be N: mg: and (3) adjusting the pH value to 8-10 by using a 30% sodium hydroxide solution, stirring and reacting for 20-40min at normal temperature, and drying a precipitate after the reaction is finished to obtain magnesium ammonium phosphate.
4) And (3) passing the obtained filtrate through a set DTRO membrane reactor to obtain clear water after reaction.
5) Adding the modified Chinese medicinal residue into the above clear water, stirring for 2 hr, and filtering the solution.
6) And (4) treating tail water of the filtered solution, and finally flowing the solution to a water return pool for recycling.
Claims (7)
1. A resource treatment and utilization method of phosphogypsum leachate is characterized by comprising the following steps:
1) pretreatment of phosphogypsum leachate: adding hydroxide into the phosphogypsum leachate to adjust the pH value to be 4-5, stirring for reaction to remove part of metal ions and impurities in the solution, and filtering to remove precipitates; adding oxalic acid into the obtained filtrate, adjusting the pH value of the solution to 6 by using hydroxide, stirring to react calcium ions with the oxalic acid to generate calcium oxalate, and filtering to remove precipitates;
2) resource utilization of phosphorus: the filtrate obtained in the step 1 enters a fluidized bed induced crystallization reactor, the pH value is adjusted to 8-10 by using hydroxide solution, ammonia nitrogen wastewater and magnesium oxide are added for reaction, and high-purity magnesium ammonium phosphate crystals are obtained after filtering and drying;
3) removing fluorine element: removing fluorine elements from the filtrate obtained in the step 2 through membrane treatment;
4) removing arsenic element: stirring the filtrate obtained in the step (3) and the traditional Chinese medicine residue adsorbing material for reaction to remove arsenic;
5) tail water treatment: and (4) treating tail water of the filtrate obtained in the step (4) to enable the filtrate to reach the discharge standard.
2. The resource treatment and utilization method of phosphogypsum leachate according to claim 1, characterized in that the hydroxide in step 1 is 30 wt% sodium hydroxide solution.
3. The resource treatment and utilization method of phosphogypsum leachate according to claim 1, which is characterized in that the reaction process of the stage of removing metal ions and impurities in the step 1 is stirring reaction at normal temperature for 10-20 min; the reaction process of the calcium removal stage is stirring reaction at normal temperature for 20-30 min.
4. The resource treatment and utilization method of phosphogypsum leachate according to claim 1, characterized in that in step 2), the hydroxide is a sodium hydroxide solution with the mass fraction of 30 wt%; the ammonia nitrogen concentration in the ammonia nitrogen wastewater is 3000-3100 mg/L; controlling the reaction system to have N: mg: the molar ratio of P is 1.1:1.2: 1.
5. The resource treatment and utilization method of phosphogypsum leachate according to claim 1, characterized in that the ammonia nitrogen wastewater in the step 2 is ammonia nitrogen circulating wastewater for intermittently preparing semi-water gas.
6. The resource treatment and utilization method of phosphogypsum leachate as claimed in claim 1, wherein in the step 2, the reaction is carried out for 20-40min at normal temperature in a fluidized bed induced crystallization reactor.
7. The resource treatment and utilization method of phosphogypsum leachate according to claim 1, characterized in that the stirring reaction time of the step 4 is 1.5-2.5 h; the preparation process of the traditional Chinese medicine residue adsorbing material is as follows: adding Chinese medicinal residue into FeCl3Stirring, filtering and drying the solution for later use.
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Cited By (5)
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| CN113788558A (en) * | 2021-09-08 | 2021-12-14 | 武汉工程大学 | Method for removing fluorine in phosphogypsum leachate by using reverse osmosis membrane |
| CN114920417A (en) * | 2022-06-28 | 2022-08-19 | 中化云龙有限公司 | Equipment and method for deep purification treatment of phosphogypsum slag warehouse leachate |
| CN115155317A (en) * | 2022-07-12 | 2022-10-11 | 杭州匠容道环境科技有限公司 | Treatment process for recycling phosphoric acid by using phosphogypsum |
| CN115611401A (en) * | 2022-12-16 | 2023-01-17 | 淄博包钢灵芝稀土高科技股份有限公司 | Recycling separation and purification method for alkaline high-content fluorine and phosphorus wastewater from rare earth ore hydrometallurgy |
| CN116444060A (en) * | 2023-03-09 | 2023-07-18 | 湖北省协诚交通环保有限公司 | Phosphogypsum percolate recycling treatment and utilization method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113788558A (en) * | 2021-09-08 | 2021-12-14 | 武汉工程大学 | Method for removing fluorine in phosphogypsum leachate by using reverse osmosis membrane |
| CN114920417A (en) * | 2022-06-28 | 2022-08-19 | 中化云龙有限公司 | Equipment and method for deep purification treatment of phosphogypsum slag warehouse leachate |
| CN114920417B (en) * | 2022-06-28 | 2024-03-05 | 中化云龙有限公司 | Equipment and method for deep purification treatment of phosphogypsum slag warehouse percolate |
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| CN115611401A (en) * | 2022-12-16 | 2023-01-17 | 淄博包钢灵芝稀土高科技股份有限公司 | Recycling separation and purification method for alkaline high-content fluorine and phosphorus wastewater from rare earth ore hydrometallurgy |
| CN116444060A (en) * | 2023-03-09 | 2023-07-18 | 湖北省协诚交通环保有限公司 | Phosphogypsum percolate recycling treatment and utilization method |
| CN116444060B (en) * | 2023-03-09 | 2024-03-19 | 湖北省协诚交通环保有限公司 | Phosphogypsum percolate recycling treatment and utilization method |
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