CN112871457A - Method for purifying and decontaminating phosphogypsum - Google Patents
Method for purifying and decontaminating phosphogypsum Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/002—Inorganic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/008—Organic compounds containing oxygen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/01—Organic compounds containing nitrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/005—Dispersants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
- B03D2203/06—Phosphate ores
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Abstract
The invention provides a method for purifying and decontaminating phosphogypsum, which comprises the following steps: (1) adding water into the phosphogypsum raw ore to adjust the concentration of the pulp to 25-35%; (2) adding quicklime to dissolve phosphorus and fluorine precipitates in the phosphogypsum raw ore, and adding water glass under strong stirring to disperse the generated phosphorus and fluorine precipitates and gypsum; (3) adding a decolorizing agent, wherein the decolorizing agent is a decolorizing agent containing-OH functional groups, the using amount is 100-300 g/t, and black organic matters are removed by dewatering and floating; (4) adding a gypsum selective adsorption medicament into the ore pulp obtained in the step (3), wherein the gypsum selective adsorption medicament contains-NH3 +The dosage of the reagent of the functional group is 50-150 g/t, the concentration of the operation ore pulp is controlled to be 20% -30%, and the floating product is the target product gypsum concentrate. The phosphogypsum concentrate obtained by the method has the advantages of removing organic matters, greatly improving the whiteness of gypsum and being solubleThe phosphorus and fluorine contents reach the specification of the first-grade ardealite building material product.
Description
Technical Field
The invention belongs to the technical field of industrial solid waste resource utilization, and particularly relates to a method for purifying phosphogypsum.
Background
Phosphorus is an indispensable fertilizer element in agricultural production, is mainly obtained by sulfuric acid wet leaching of apatite, but generates a large amount of phosphogypsum while obtaining phosphoric acid, so that the phosphogypsum becomes a large amount of industrial solid waste generated in the phosphate fertilizer chemical industry. The production of one ton of phosphoric acid needs 4.5-5.5 tons of phosphogypsum, and according to statistics, the accumulated phosphogypsum stacking in China reaches 56 hundred million tons, and the large amount of phosphogypsum stacking causes serious resource waste and environmental pollution.
The application of the phosphogypsum in building materials is a good method for dissolving the phosphogypsum. However, the phosphogypsum contains soluble phosphorus, fluorine, organic matters and other impurities, and the impurities can reduce the performance of the phosphogypsum as building materials and seriously hinder the phosphogypsum from being used as the building materials. For a long time, science and technology workers in China carry out a great deal of research work on impurity removal and resource utilization of phosphogypsum, and breakthrough progress is made in some fields.
The patent document with publication number CN109928367A and publication date of 2019, 6 and 25 provides a device and a method for preparing sulfur from phosphogypsum.
The patent document with publication number CN109485175A and publication number 2019, 3 and 19 provides an in-situ treatment system for leachate in a phosphogypsum yard, which invents the in-situ treatment system for the leachate in the phosphogypsum yard, and a plurality of sandstone layers are arranged along the flow direction of underground water; the sandstone layers are formed by mixing limestone, zeolite, bentonite and calcium hydroxide. The method can purify the phosphogypsum yard leachate, and reduce the content of fluoride ions, phosphate ions, total iron ions and manganese ions in the leachate underground water.
The patent document with publication number CN109231684A and publication number 2019, 1, 18, provides a treatment method and a treatment system for purifying phosphogypsum yard penetrating fluid, which researches a treatment system for the phosphogypsum yard penetrating fluid, introduces the phosphogypsum yard penetrating fluid into a multistage neutralization tank, adds quicklime or slaked lime, controls the pH value of the neutralization tank, adds a flocculating agent, then pumps the phosphogypsum yard penetrating fluid into a settling tank, and leads each index of the treated penetrating fluid to reach the first-level standard of the comprehensive sewage discharge standard (109231684A plus 1996) after multiple times of neutralization and settling.
The patent document with publication number CN108793221A and publication date of 2018, 11.13.invents a phosphogypsum purification system, the invention discloses a phosphogypsum purification system, the high-purity phosphogypsum neutralization and purification device firstly calcines the phosphogypsum, then neutralizes the phosphogypsum by lime, and finally greatly reduces the harmful impurities of the phosphogypsum through hydration, and the product performance is superior to that of natural gypsum; solves the problems of environmental pollution and low recycling rate of the existing phosphogypsum.
The patent document with publication number CN107512857A and publication date of 2017, 12 and 26 provides a method and a device for preparing building gypsum by using phosphogypsum. A filter press is arranged beside a slurry pool generated by a phosphoric acid production device, a filter cake after filter pressing is an ardealite raw material, and the ardealite raw material can be directly mixed with quicklime to prepare building gypsum, so that long-term outdoor stacking aging treatment on slurry is avoided, and environmental pollution is reduced.
The patent document with publication number CN106977123A, publication number 2017, 7 and 25 provides a process method of citric acid and water washing for removing impurity fluorine in phosphogypsum, which comprises three procedures of citric acid dissolution, citric acid washing and water washing. The citric acid in the solution can have chemical action with impurities in the phosphogypsum, so that the impurities such as fluoride, phosphate and the like in the phosphogypsum are converted into water-washable soluble substances, and then the impurities are removed by a water washing process, so that the fluoride content in equipment and drying flue gas is reduced after purification, the phosphogypsum with the fluoride and phosphide removed can be utilized by a process for preparing acid and co-producing cement by the phosphogypsum, and the equipment in the production process section of sulfuric acid and cement can not be corroded due to the removal of the fluoride.
Although the invention makes great contribution in the aspects of phosphogypsum purification and resource utilization, the method still has the following defects for the current phosphogypsum purification and resource utilization: the process flow is complex and needs to be carried out at high temperature, high pressure and high acid concentration; high process cost, secondary pollution, high investment cost and low economic benefit. The existence of the problems seriously influences the industrial popularization and application of the phosphogypsum purification and resource technology.
Therefore, how to solve the problems in the impurity removal of the phosphogypsum and provide a new method for purifying and removing the impurity of the phosphogypsum becomes a technical problem to be solved urgently in the field.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for purifying phosphogypsum. The method for purifying and removing the impurities from the phosphogypsum can reduce the treatment cost of the phosphogypsum and reduce the environmental pollution generated by the treatment of the phosphogypsum, and the purified phosphogypsum is used for building materials and can realize the recycling of resources.
In order to achieve the purpose, the invention provides a method for purifying phosphogypsum, which comprises the following steps:
(1) selecting phosphogypsum raw ore as a raw material to be purified, and adding water to adjust the concentration of the pulp to be 25-35%;
(2) adding quicklime into the ore pulp obtained in the step (1) for stirring, precipitating soluble phosphorus and fluorine in the phosphogypsum raw ore, and then adding water glass in the strong stirring process to disperse the generated phosphorus and fluorine precipitate and gypsum;
(3) adding a decolorizing agent into the phosphogypsum ore pulp obtained in the step (2) for decolorizing, wherein the decolorizing agent is a decolorizing agent containing-OH functional groups, the dosage of the decolorizing agent is 100-300 g/t, and black organic matters are removed by dewatering and floating;
(4) adding a selective adsorption agent into the phosphogypsum ore pulp obtained in the step (3) to carry out adsorption treatment on gypsum, wherein the selective adsorption agent contains-NH3 +The dosage of the agent with the functional group is 50-150 g/t, the concentration of the ore pulp is controlled to be 20% -30% during adsorption treatment, and the obtained floating product is the target product gypsum concentrate.
Further, the raw phosphogypsum ore in the step (1) is the raw phosphogypsum ore produced by a wet-process phosphoric acid process, and the raw phosphogypsum ore is subjected to pressure filtration to form a filter cake which is used as a raw material to be purified.
Further, CaSO in the phosphogypsum raw ore in the step (1)4·2H2The content of O is 50-88%, the content of soluble phosphorus is more than 0.5%, and the content of soluble fluorine is more than 0.3%.
Further, in the step (2), the addition amount of the quicklime is 0.5-5% of the mass of the phosphogypsum raw ore.
Further, in the step (2), the time for adding the quicklime to carry out stirring treatment is 5min, and the stirring speed is 1800-2600 r/min.
Further, the adding amount of the water glass in the step (2) is 100-400 g/t, the stirring speed is 2300 rpm, and the stirring time is 5 minutes.
Further, the decoloring agent in the step (3) comprises pine oil.
Further, the time of the decoloring treatment in the step (3) is 5 minutes.
Further, the selective adsorbent in step (4) comprises tetradecylamine.
Further, the time of the adsorption treatment in the step (4) is 3 minutes.
The treatment method provided by the invention can be used for CaSO4·2H2The phosphogypsum resource with the O content of 50-88 percent, the soluble phosphorus content of more than 0.5 percent and the soluble fluorine content of more than 0.3 percent has good purifying and impurity removing effects. The principle of the invention is as follows: firstly, adding quicklime to precipitate soluble phosphorus and fluorine according to the concentration of the soluble phosphorus and the fluorine in the phosphogypsum, and then adding a decolorizing agent to remove the soluble phosphorus and the fluorine by utilizing the surface property difference of organic matters, slime, micro-fine grain phosphorus-fluorine-containing minerals and gypsum; finally, adding a selective adsorption agent to float out gypsum, wherein the coarse-grained phosphorus and fluorine-containing minerals and other coarse-grained impurities become tailings, and finally purifying the phosphogypsum impurities.
Compared with other treatment methods, the method has the biggest difference that the tail water generated after the treatment by the method does not contain soluble phosphorus and soluble fluorine, can be directly recycled, does not generate discharged wastewater, can obtain high-quality gypsum concentrate with whiteness of more than 60 and purity of more than 98 percent, greatly reduces the treatment flow, saves the cost and improves the quality.
The method removes organic matters in the phosphogypsum concentrate, greatly improves the whiteness of gypsum, and ensures that the content of soluble phosphorus and soluble fluorine reaches the specification of the first-grade products in the phosphogypsum building materials. The content of eutectic phosphorus and fluorine in phosphogypsum is also reduced. The method has the advantages of simple process flow, no high temperature, high pressure and high acid concentration in the process flow, cyclic use of the wastewater, no secondary pollution and low production cost. The method can effectively solve some engineering problems in the existing phosphogypsum purification and impurity removal process, and provides a new way for efficiently utilizing phosphogypsum resources.
Compared with the prior art, the invention has the following beneficial effects:
(1) the phosphogypsum purification and impurity removal method provided by the invention has the advantages of simple process flow and low production cost, and high-grade concentrate can be obtained without carrying out multiple concentration and scavenging treatment on ore pulp;
(2) the method for purifying and removing the impurities from the phosphogypsum has the advantages that organic matters in the obtained phosphogypsum concentrate are removed, the whiteness of gypsum is greatly improved, and the content of soluble phosphorus and soluble fluorine reaches the specification of a first-grade product in a phosphogypsum building material.
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FIG. 1 is a process flow diagram of the purification and impurity removal of phosphogypsum adopted by the method of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is described in detail below with reference to the following embodiments, and it should be noted that the following embodiments are only for explaining and illustrating the present invention and are not intended to limit the present invention. The invention is not limited to the embodiments described above, but rather, may be modified within the scope of the invention.
Example 1
Phosphogypsum raw ore CaSO4·2H282.0% of O, 1.72% of total phosphorus, 0.7% of total fluorine and 0.6% of soluble phosphorus. The soluble fluorine content is 0.5%, and the whiteness of the raw ore is 31.0. Firstly, preparing phosphogypsum into ore pulp, wherein the concentration of the ore pulp is 30%, strongly stirring, then adding quicklime with the mass fraction of 1.5% of the phosphogypsum into a flotation machine, continuously stirring for 5 minutes, adding 50g/t of dispersing agent, then adding 300g/t of decolorizing agent pine oil, stirring and aerating to remove organic matters, slime and micro-fine phosphorus and fluorine minerals in the phosphogypsum to obtain a tail 1, then adding 80g/t of selective adsorbent tetradecylamine to obtain gypsum concentrate, and taking the coarse phosphorus, fluorine and silicon-containing minerals as a tail 2. CaSO in gypsum concentrate treated by the method4·2H2The purity of O reaches 98.5, and the whiteness reaches 63.5. The detailed process is shown in figure 1, and the test indexes are shown in table 1.
TABLE 1 purification index of phosphogypsum
Example 2:
phosphogypsum raw ore CaSO4·2H2O contains83.6%, total phosphorus content 1.63%, total fluorine content 0.68%, soluble phosphorus content 0.51%. The soluble fluorine content is 0.34%, and the whiteness of the raw ore is 30.4. Firstly, preparing phosphogypsum into ore pulp, wherein the concentration of the ore pulp is 25%, strongly stirring, then adding quicklime with the mass fraction of 1.25% of the phosphogypsum into a flotation machine, continuously stirring for 4 minutes, adding a dispersing agent for 60g/t, then adding a decolorizing agent, namely, pine oil for 250g/t, stirring and aerating to remove organic matters, slime and micro-fine phosphorus and fluorine minerals in the phosphogypsum to obtain a tail 1, then adding a selective adsorbent, namely, tetradecylamine, for 100g/t to obtain gypsum concentrate, wherein the coarse phosphorus, fluorine and silicon-containing minerals become a tailing 2. CaSO in gypsum concentrate treated by the method4·2H2The purity of O reaches 98.8, and the whiteness reaches 64.4. The detailed process is shown in figure 1, and the test indexes are shown in table 2.
TABLE 2 purification index of phosphogypsum
Example 3:
phosphogypsum raw ore CaSO4·2H278.0% of O, 1.95% of total phosphorus and 0.87% of soluble phosphorus. The soluble fluorine content is 0.55 percent, and the whiteness of the raw ore is 30.0. Firstly, preparing phosphogypsum into ore pulp with the concentration of 32 percent, strongly stirring, then adding quicklime with the mass fraction of 2.0 percent of the phosphogypsum into a flotation machine, continuously stirring for 5 minutes, and adding 80g/t of water glass dispersant. Adding 280g/t of decolorizing agent pine oil, stirring and aerating to remove organic matters, slime and micro-fine phosphorus and fluorine minerals in the phosphogypsum, wherein the removed product is tail 1, then adding 70g/t of selective adsorbent decatetramine to obtain gypsum concentrate, and obtaining tailing 2 from coarse phosphorus and fluorine minerals and silicon-containing minerals. CaSO in gypsum concentrate treated by the method4·2H2The purity of O reaches 97.6, and the whiteness reaches 63.1. The detailed process is shown in figure 1, and the test indexes are shown in table 3.
TABLE 3 purification index of phosphogypsum
Example 4:
phosphogypsum raw ore CaSO4·2H2The content of O is 88.3 percent, the content of total phosphorus is 1.58 percent, and the content of soluble phosphorus is 0.51 percent. The soluble fluorine content is 0.32%, and the whiteness of the raw ore is 36.2. Firstly, preparing the phosphogypsum into ore pulp with the concentration of 30 percent, strongly stirring, then adding quicklime with the mass fraction of 1.0 percent of the phosphogypsum into a flotation machine, continuously stirring for 7 minutes, and adding 40g/t of dispersing agent. Then adding 200g/t of decolorizing agent pine oil, stirring and aerating to remove organic matters, slime and micro-fine phosphorus and fluorine minerals in the phosphogypsum, wherein the removed product is tail 1, then adding 120g/t of selective adsorbent decatetramine to obtain gypsum concentrate, and obtaining tailing 2 from coarse phosphorus and fluorine minerals and silicon-containing minerals. CaSO in gypsum concentrate treated by the method4·2H2The purity of O reaches 98.6, and the whiteness reaches 61.3. The detailed process is shown in figure 1, and the test indexes are shown in table 4.
TABLE 4 purification index of phosphogypsum
Example 5:
phosphogypsum raw ore CaSO4·2H284.6 percent of O, 1.64 percent of total phosphorus, 0.67 percent of total fluorine and 0.72 percent of soluble phosphorus. The soluble fluorine content is 0.54 percent, and the whiteness of the raw ore is 33.6. Firstly, preparing phosphogypsum into ore pulp with the concentration of 28 percent, strongly stirring, then adding quicklime with the mass fraction of 1.8 percent of the phosphogypsum into a flotation machine, continuously stirring for 8 minutes, and adding 60g/t of water glass dispersant. Then adding 200g/t of decolorizing agent pine oil, stirring and aerating to remove organic matters, slime and micro-fine phosphorus and fluorine minerals in the phosphogypsum to obtain a tail 1, then adding 120g/t of selective adsorbent tetradecylamine to obtain gypsum concentrate, and using coarse phosphorus and fluorine minerals and silicon-containing minerals as tailings 2. CaSO in gypsum concentrate treated by the method4·2H2The purity of O reaches 98.7, and the whiteness reaches 62.2. The detailed process is shown in figure 1, and the test indexes are shown in table 5.
TABLE 5 purification index of phosphogypsum
From the test results in tables 1-5, it can be seen that by using the novel method for purifying and removing the impurities from the phosphogypsum, the content of soluble phosphorus and fluorine, the total content of phosphorus and fluorine and the content of organic matters in the phosphogypsum can be effectively reduced, the whiteness and the purity of the phosphogypsum are improved, and better process indexes are obtained.
Claims (10)
1. The method for purifying and decontaminating the phosphogypsum is characterized by comprising the following steps of:
(1) selecting phosphogypsum raw ore as a raw material to be purified, and adding water to adjust the concentration of the pulp to be 25-35%;
(2) adding quicklime into the ore pulp obtained in the step (1) for stirring, precipitating soluble phosphorus and fluorine in the phosphogypsum raw ore, and then adding water glass in the strong stirring process to disperse the generated phosphorus and fluorine precipitate and gypsum;
(3) adding a decolorizing agent into the phosphogypsum ore pulp obtained in the step (2) for decolorizing, wherein the decolorizing agent is a decolorizing agent containing-OH functional groups, the dosage of the decolorizing agent is 100-300 g/t, and black organic matters are removed by dewatering and floating;
(4) adding a selective adsorption agent into the phosphogypsum ore pulp obtained in the step (3) to carry out adsorption treatment on gypsum, wherein the selective adsorption agent contains-NH3 +The dosage of the agent with the functional group is 50-150 g/t, the concentration of the ore pulp is controlled to be 20% -30% during adsorption treatment, and the obtained floating product is the target product gypsum concentrate.
2. The method according to claim 1, characterized in that the raw phosphogypsum ore in the step (1) is the raw phosphogypsum ore produced by a wet-process phosphoric acid process, and the raw phosphogypsum ore is used as the raw material to be purified after being subjected to pressure filtration to form a filter cake.
3. The method of claim 2, wherein the first and second light sources are selected from the group consisting of,characterized in that the CaSO in the phosphogypsum raw ore in the step (1)4·2H2The content of O is 50-88%, the content of soluble phosphorus is more than 0.5%, and the content of soluble fluorine is more than 0.3%.
4. The method according to claim 1, characterized in that the addition amount of the quicklime in the step (2) is 0.5-5% of the mass of the raw phosphogypsum ore.
5. The method as claimed in claim 1, wherein the quicklime is added in the step (2) for stirring treatment for 5min, and the stirring speed is 1800-2600 rpm.
6. The method according to claim 1, wherein the amount of the water glass added in the step (2) is 100-400 g/t, the stirring speed is 2300 rpm, and the stirring time is 5 minutes.
7. The method of claim 1, wherein the decolorizing agent in step (3) is pine oil.
8. The method as claimed in claim 1, wherein the time of the decoloring treatment in the step (3) is 5 minutes, and the black organic matter is floated up to be separated from the gypsum by aeration stirring.
9. The method of claim 1, wherein the selective adsorbent agent in step (4) is tetradecylamine.
10. The method according to claim 1, wherein the adsorption treatment in the step (4) is performed for 3 minutes, and then the gypsum adsorbed with the medicinal agent is floated hydrophobically by aeration stirring for 3 minutes.
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Cited By (5)
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| CN115124265A (en) * | 2022-02-21 | 2022-09-30 | 上海胜义环境科技有限公司 | Phosphogypsum purification and purification method capable of realizing full utilization |
| CN115180646A (en) * | 2022-08-22 | 2022-10-14 | 清华大学 | Method for purifying calcium sulfate dihydrate from by-product gypsum |
| CN115400881A (en) * | 2022-08-26 | 2022-11-29 | 广东邦普循环科技有限公司 | Method for purifying and whitening phosphogypsum |
| CN116425187A (en) * | 2023-04-20 | 2023-07-14 | 湖南科技大学 | Method for improving whiteness of phosphogypsum |
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| CN115124265A (en) * | 2022-02-21 | 2022-09-30 | 上海胜义环境科技有限公司 | Phosphogypsum purification and purification method capable of realizing full utilization |
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| CN115180646A (en) * | 2022-08-22 | 2022-10-14 | 清华大学 | Method for purifying calcium sulfate dihydrate from by-product gypsum |
| CN115400881A (en) * | 2022-08-26 | 2022-11-29 | 广东邦普循环科技有限公司 | Method for purifying and whitening phosphogypsum |
| CN116425187A (en) * | 2023-04-20 | 2023-07-14 | 湖南科技大学 | Method for improving whiteness of phosphogypsum |
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