CN115893885A - Phosphogypsum immersion cleaning agent and phosphogypsum harmless treatment method - Google Patents
Phosphogypsum immersion cleaning agent and phosphogypsum harmless treatment method Download PDFInfo
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Abstract
The invention discloses an immersion cleaning agent of phosphogypsum and a harmless treatment method of the phosphogypsum. The method for the innocent treatment of the phosphogypsum comprises the following steps: s 1 Uniformly mixing fresh dry-discharged phosphogypsum with water to prepare phosphogypsum slurry; s 2 Leaching the phosphogypsum slurry with a leaching agent, and concentrating and dehydrating after the leaching is finished to obtain leached phosphogypsum; s 3 Screening and rubbing the washed phosphogypsum; s 4 Dehydrating the phosphogypsum concentrated slurry after friction washing to obtain washed phosphogypsum; s 5 Oxidizing the washed phosphogypsum by using an oxidant to obtain the whitened phosphogypsum; s 6 And performing acid-base neutralization treatment on the whitening phosphogypsum by using quick lime to obtain harmless high-purity high-whiteness regenerated gypsum. The method only effectively removes soluble fluorine, phosphorus, organic matters and other impurities in the phosphogypsum, can also deeply remove eutectic phosphorus in the phosphogypsum, and increases regenerated stonesThe whiteness of the paste.
Description
Technical Field
The invention belongs to the technical field of phosphogypsum innocent treatment and resource utilization, and particularly relates to a phosphogypsum pickling agent and a phosphogypsum innocent treatment method.
Background
Phosphogypsum is industrial solid waste residue produced when phosphorite is treated by sulfuric acid in the wet-process phosphoric acid production process, and about 4.5-5 tons of phosphogypsum are produced per 1 ton of phosphoric acid produced. The main component of the phosphogypsum is calcium sulfate dihydrate (CaSO) 4 ·2H 2 O), which belongs to general solid waste class ii, is generally acidic (PH = 1.9-5.3), and contains impurities such as undecomposed phosphate ore, fluoride, organic matter, and residual phosphoric acid. Worldwide, the stockpiling of phosphogypsum is over 60 hundred million tons, and the annual rate of the stockpiling of the phosphogypsum is still continuously increased by about 2 hundred million tons, but the global comprehensive utilization rate of the phosphogypsum is only about 25 percent.
China is the first country of producing the large phosphate fertilizer in the world and is also the first country of producing the phosphogypsum by-product. 85% of phosphorus chemical enterprises in China are mainly distributed in Yangtze river basin, and the key points are in Sichuan province, yunnan province, hubei province, anhui province and Guizhou province. In 2021, the stockpiling amount of the national phosphogypsum reaches 5 hundred million tons, 5000 million tons of the newly added phosphogypsum are added every year, and the phosphogypsum becomes the second major industrial solid waste in China. The stacking of the phosphogypsum not only occupies a large amount of land, but also causes persistent pollution to the environment such as soil, underground water, surface water flow and the like due to soluble fluorine, phosphorus, acidic substances, organic substances and the like in a stack body. Therefore, the harmless treatment and resource comprehensive utilization of the phosphogypsum are not slow.
Calcium sulfate dihydrate (CaSO) in phosphogypsum 4 ·2H 2 O) is an important regenerated gypsum resource, but contains various harmful impurities such as phosphorus, fluorine, organic matters and the like, and the material characteristics of the gypsum building material are seriously influenced.
The phosphorus impurities in the phosphogypsum are mainly divided into soluble phosphorus, eutectic phosphorus and insoluble phosphorus. Soluble phosphorus is mainly in the form of H 3 PO 4 、H 2 PO 4 - 、HPO 4 2- 、PO 4 3- Four major classes, of which the most influential on gypsum performance is H 3 PO 4 The presence of calcium sulfate in an acidic environment will inhibit the growth of calcium sulfate. This occurs when the gypsum is hydratedSome soluble phosphorus will react with Ca 2+ Insoluble calcium phosphate is generated by reaction and covers the surface of the phosphogypsum to prevent gypsum from being dissolved and hydrated continuously, so that the setting and hardening time of the phosphogypsum is prolonged, crystals of the phosphogypsum are coarsened, the structure is loose, and the strength is reduced. Eutectic phosphorus is H in wet-process phosphoric acid production 2 PO 4 - 、HPO 4 2- In place of SO 4 2- Enters into crystal lattices of calcium sulfate dihydrate to form eutectic, and in the hydration process of phosphogypsum, the eutectic phosphorus is dissolved out from the crystal lattices and reacts with Ca 2+ Formation of insoluble Ca 3 (PO 4 ) 2 And the crystal growth inhibitor is covered on the surface of the phosphorus building gypsum powder, so that the crystallization supersaturation degree of the dihydrate gypsum is obviously reduced, the hydration rate is reduced, the initial setting time and the final setting time are prolonged, the structure is coarsened, the lapping quantity among crystals is reduced, the flexural strength and the compressive strength of a hardened body are reduced, and the eutectic phosphorus is difficult to remove by a common process method. Ca is the main component of insoluble phosphorus 3 (PO 4 ) 2 The gypsum powder has the advantages of high melting point, stable chemical property, no participation in hydration reaction in the hydration process of the gypsum powder of the phosphorus building, and inertia.
The fluorine impurities in the phosphogypsum are mainly divided into soluble fluorine and insoluble fluorine. Soluble fluorine is one of the main forms affecting the performance of phosphogypsum, mainly as soluble fluorine F - The calcium sulfate dihydrate is in the form of particles, and can slowly release a certain acidity in the gypsum product, when the mass fraction exceeds 0.3%, the calcium sulfate dihydrate crystals can be coarsened, the intermolecular force among the crystals is weakened, the structure is loose, and the strength of the phosphogypsum product is reduced. Insoluble fluorine CaF 2 、Na 2 SiF 6 The two forms exist, do not participate in hydration reaction, and have small influence on the gelling performance.
At present, the methods for the innocent treatment of the phosphogypsum mainly comprise a water washing method, a flotation method, an acid washing method, a calcining method and the like, wherein some of the methods cannot thoroughly remove soluble impurity impurities and can not remove eutectic phosphorus in the soluble impurity impurities, and the treated phosphogypsum has low whiteness, so that the recycling of the phosphogypsum is influenced; in addition, some methods have large investment, high operation cost and large practical application difficulty. How to carry out efficient impurity removal on phosphogypsum with low cost to produce high-quality regenerated gypsum and improve the level of resource utilization of the phosphogypsum becomes a technical problem to be solved urgently.
Disclosure of Invention
Based on the prior art, the invention provides a phosphogypsum pickling agent and a phosphogypsum harmless treatment method, which organically combines the phosphogypsum pickling, oxidation, neutralization and other harmless treatment methods, effectively removes soluble fluorine, phosphorus, organic matters and other impurities in the phosphogypsum, can also deeply remove eutectic phosphorus in the phosphogypsum, and simultaneously increases the whiteness of the phosphogypsum.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
the pickling agent for the phosphogypsum comprises the following components in percentage by mass:
40 to 55 percent of inorganic acid
40 to 55 percent of organic acid
2 to 5 percent of organic extractant.
Further, the inorganic acid is at least one selected from sulfuric acid and nitric acid.
Further, the mass fraction of the sulfuric acid is 20-30%, and the mass fraction of the nitric acid is 25-35%.
Further, the organic acid is at least one selected from citric acid and acetic acid.
Further, the organic extractant is selected from at least one of butyl acetate and n-butanol.
A method for harmlessly treating phosphogypsum comprises the following steps:
S 1 uniformly mixing fresh dry-discharged phosphogypsum with water to prepare phosphogypsum slurry;
S 2 carrying out leaching treatment on the phosphogypsum slurry by using the leaching agent of any one of claims 1 to 5, and concentrating and dehydrating after the leaching is finished to obtain leached phosphogypsum;
S 3 screening and rubbing the washed phosphogypsum;
S 4 dehydrating the phosphogypsum concentrated slurry after friction washing to obtain washed phosphogypsum;
S 5 oxidizing the washed phosphogypsum by using an oxidant to obtain the whitened phosphogypsum;
S 6 and performing acid-base neutralization treatment on the whitening phosphogypsum by using quick lime to obtain harmless high-purity high-whiteness regenerated gypsum.
Further, the water content of the fresh dry-discharge phosphogypsum is 10-20%, and the water content of the phosphogypsum slurry is 40-70%.
Further, the dosage of the immersion cleaning agent is 6-35kg/t of fresh dry-discharge phosphogypsum, and the immersion cleaning time is 30-60min.
Further, the water content of the washed phosphogypsum is less than 40%, and the water content of the washed phosphogypsum is 20-30%.
Further, the oxidant is hydrogen peroxide, the mass fraction of the hydrogen peroxide is 15% -30%, the dosage of the hydrogen peroxide is 5-15kg/t, and the time of oxidation treatment is 20-60min.
Further, step S 6 Adjusting pH to 6.5-8.0 with calx, and neutralizing for 10-20min.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the leaching agent can effectively remove the eutectic phosphorus in the phosphogypsum, and can react with fluoride to generate a complex which is easy to dissolve in water, so that the complex can be removed by subsequent water washing.
2. The immersion cleaning agent disclosed by the invention is simple in components, low in price, easy to obtain and low in cost, does not introduce new harmful impurities, does not influence subsequent resource utilization of phosphogypsum, and is suitable for popularization and application.
3. The main pollutants, impurities, fluorine, phosphorus and organic matters in the phosphogypsum are separated and removed through the water washing of the pickling agent and the vibrating screen, the phosphogypsum is oxidized and subjected to acid-base neutralization treatment, and finally, the harmless, high-purity and high-whiteness regenerated gypsum is obtained, the purity of the regenerated gypsum can exceed 90 percent, the whiteness of the regenerated gypsum exceeds 85 percent, the quality of the regenerated gypsum is superior to the national standards of first-grade natural gypsum and first-grade phosphogypsum, the regenerated gypsum can be stored in a harmless manner, can replace natural gypsum ore and be used as a building gypsum raw material, and the screened gravel can be used as building materials such as water permeable bricks, concrete mortar and the like.
4. The harmless treatment method is simple, convenient to operate, low in operation and investment cost, strong in controllability and convenient for industrial application.
Detailed Description
The present invention is described in detail below with reference to specific examples, but these examples are not to be construed as limiting the scope of the present invention in any way.
Example 1
The phosphogypsum immersion cleaning agent is composed of the following components in percentage by mass:
48.8 percent of sulfuric acid
48.8 percent of citric acid
2.4 percent of butyl acetate,
the mass fraction of the sulfuric acid is 25%.
Example 2
The phosphogypsum immersion cleaning agent is composed of the following components in percentage by mass:
sulfuric acid 46.0%
50.5 percent of citric acid
3.5 percent of n-butyl alcohol,
the mass fraction of the sulfuric acid is 30%.
Example 3
The phosphogypsum immersion cleaning agent is composed of the following components in percentage by mass:
nitric acid 40.0%
Acetic acid 55.0%
5.0 percent of n-butyl alcohol,
the mass fraction of the nitric acid is 35%.
Example 4
The phosphogypsum immersion cleaning agent is composed of the following components in percentage by mass:
nitric acid 46.7%
Acetic acid 48.3%
5.0 percent of butyl acetate,
the mass fraction of the nitric acid is 30%.
Example 5
S 1 100g of fresh dry-discharged phosphogypsum of a phosphorite enterprise A in Hubei is taken, the whiteness is 38.96%, the water content is 11.30%, and the pH value is 2.3. Adding 80ml of water into fresh dry-discharged phosphogypsum, and stirring for 5min on a magnetic stirrer to prepare phosphogypsum slurry with the water content of 50.72 percent.
S 2 Taking sulfuric acid, citric acid and butyl acetate according to the proportion of the embodiment 1, and stirring and mixing the sulfuric acid, the citric acid and the butyl acetate uniformly to prepare the immersion cleaning agent.
S 3 Adding 3g of pickling agent into the phosphogypsum slurry, stirring and pickling for 40min, then putting the phosphogypsum slurry into a centrifugal machine, concentrating and dehydrating for 10min at 3000rad/min, and pouring out the upper-layer liquid to obtain the pickled phosphogypsum, wherein the water content of the pickled phosphogypsum is less than 40%, and the upper-layer liquid is enriched with impurities such as phosphorus, fluorine, organic matters and the like.
The three components of sulfuric acid, citric acid and butyl acetate in the leaching agent are matched with each other and have synergistic effect, so that eutectic phosphorus in the phosphogypsum can be effectively removed, meanwhile, the three components can also react with fluoride to generate a complex which is easy to dissolve in water, organic impurities in the phosphogypsum are removed by extraction, and the complex is removed by subsequent water washing.
S 4 Adding 80ml of water into the washed phosphogypsum, fully and uniformly shaking the washed phosphogypsum and the water for 2min by using an oscillator, then carrying out vibration friction filtration by using a vibrating screen of 20 meshes, and carrying out centrifugal dehydration on the solid obtained by filtration to obtain the washed phosphogypsum. In the step, minerals, gravels and the like which are not completely decomposed in the extraction process of the phosphogypsum and the phosphoric acid are separated, and the vibrating screen can play a role in scrubbing the phosphogypsum, so that the soluble impurities adsorbed on the surface can be more effectively removed.
S 5 Adding 20ml of water into the washed phosphogypsum, oscillating for 2min by using an oscillator, dispersing and uniformly mixing, then adding 1.5g of hydrogen peroxide with the concentration of 30%, and stirring for 40min by using a magnetic stirrer to obtain a solid-liquid mixture containing the whitened phosphogypsum.
S 6 Adding into the solid-liquid mixture containing the whitening phosphogypsumAdding 2.4g of calcium oxide (CaO), stirring for reaction for 20min, adjusting the pH value to 6.8, then dehydrating by using a centrifugal machine, and then drying by using a 45 ℃ oven to constant weight to obtain harmless high-purity high-whiteness regenerated gypsum.
The change of the mass fraction of the main components before and after the phosphogypsum innocent treatment in the embodiment is shown in the table 1:
TABLE 1 comparison of the mass fractions of the principal components before and after the phosphogypsum innocent treatment
As is clear from Table 1, P was treated without any harm 2 O 5 F and MgO impurities are reduced remarkably, and calcium oxide and SO 3 Etc. the content of the useful components increases. Therefore, the method can obviously remove impurities such as phosphorus, fluorine and the like in the phosphogypsum and improve the content of available components.
Example 6
S 1 100g of fresh dry-discharged phosphogypsum of a certain phosphorite enterprise B in Hubei is taken, the whiteness is 42.56 percent, the water content is 12.14 percent, and the pH value is 2.8. Adding 80ml of water into fresh dry-discharged phosphogypsum, and stirring for 5min on a magnetic stirrer to prepare phosphogypsum slurry with the water content of 51.19 percent.
S 2 And taking sulfuric acid, citric acid and butyl acetate according to the mixture ratio of the embodiment 1, and uniformly stirring and mixing the sulfuric acid, the citric acid and the butyl acetate to prepare the lotion.
S 3 Adding 3g of leaching agent into the phosphogypsum slurry, stirring and leaching for 30min, then putting the phosphogypsum slurry into a centrifuge, concentrating and dehydrating for 10min at 3000rad/min, and pouring out the upper-layer liquid to obtain the leached phosphogypsum, wherein the concentration of the leached phosphogypsum is more than 60%.
S 4 Adding 80ml of water into the washed phosphogypsum, fully and uniformly shaking the washed phosphogypsum and the water for 2min by using an oscillator, then carrying out vibration friction filtration by using a vibrating screen of 20 meshes, and carrying out centrifugal dehydration on the solid obtained by filtration to obtain the washed phosphogypsum.
S 5 Adding into the washed phosphogypsumAdding 20ml of water, oscillating for 2min by using an oscillator, dispersing and uniformly mixing, then adding 1.5g of hydrogen peroxide with the concentration of 30%, and stirring for 40min by using a magnetic stirrer to obtain a solid-liquid mixture containing the whitening phosphogypsum.
S 6 Adding 2.2g of quicklime (CaO) into the solid-liquid mixture containing the whitening phosphogypsum, stirring for reacting for 20min, adjusting the pH value to 6.6, then dehydrating by using a centrifugal machine, and then air-drying by using a 45 ℃ drying oven to constant weight to obtain the harmless high-purity high-whiteness regenerated gypsum.
The change of the mass fraction of the main components before and after the phosphogypsum innocent treatment in the embodiment is shown in the table 2:
TABLE 2 comparison of the mass fractions of the principal components before and after the phosphogypsum innocent treatment
As is clear from Table 2, P was treated without any harm 2 O 5 F and MgO impurities are reduced remarkably, and calcium oxide and SO 3 Etc. the content of the useful components increases. Therefore, the method can obviously remove impurities such as phosphorus, fluorine and the like in the phosphogypsum and improve the content of available components.
The indexes of the regenerated gypsum obtained by the innocent treatment of the examples 5 to 6 are compared with national standards of first-grade natural gypsum (GB/T5483-2008) and first-grade phosphogypsum (GB/T23456-018), and are shown in the following table 3:
TABLE 3 comparison of phosphogypsum before and after innocent treatment with national standard
Remarking: nd indicates that no detection was made
As can be seen from Table 3, the regenerated gypsum obtained by treating the fresh dry-exhaust phosphogypsum by the method completely meets the standards of first-grade natural gypsum and first-grade phosphogypsum, has high whiteness and excellent quality, and meets the requirements of building gypsum on raw materials.
Claims (10)
1. The phosphogypsum immersion cleaning agent is characterized by comprising the following components in percentage by mass:
40 to 55 percent of inorganic acid
40 to 55 percent of organic acid
2 to 5 percent of organic extractant.
2. The pickling agent of phosphogypsum according to claim 1, characterized in that: the inorganic acid is at least one of sulfuric acid and nitric acid.
3. The pickling agent of phosphogypsum according to claim 2, characterized in that: the mass fraction of the sulfuric acid is 20-30%, and the mass fraction of the nitric acid is 25-35%.
4. The pickling agent of phosphogypsum according to claim 1, characterized in that: the organic acid is at least one of citric acid and acetic acid.
5. The pickling agent of phosphogypsum according to claim 1, characterized in that: the organic extractant is at least one of butyl acetate and n-butanol.
6. A method for innocent treatment of phosphogypsum is characterized by comprising the following steps:
S 1 uniformly mixing fresh dry-discharged phosphogypsum with water to prepare phosphogypsum slurry;
S 2 carrying out leaching treatment on the phosphogypsum slurry by using the leaching agent of any one of claims 1 to 5, and concentrating and dehydrating after the leaching is finished to obtain leached phosphogypsum;
S 3 screening and rubbing the washed phosphogypsum;
S 4 dehydrating the phosphogypsum concentrated slurry after friction washing to obtain washed phosphogypsum;
S 5 oxidizing the washed phosphogypsum by using an oxidant to obtainTo whiten phosphogypsum;
S 6 and performing acid-base neutralization treatment on the whitening phosphogypsum by using quick lime to obtain harmless high-purity high-whiteness regenerated gypsum.
7. The method for the innocent treatment of phosphogypsum according to claim 6, which is characterized in that: the water content of the fresh dry-discharge phosphogypsum is 10-20%, and the water content of the phosphogypsum slurry is 40-70%.
8. The method for the innocent treatment of phosphogypsum according to claim 6, which is characterized in that: the dosage of the pickling agent is 6-35kg/t of fresh dry-discharged phosphogypsum, and the pickling time is 30-60min.
9. The method for the innocent treatment of phosphogypsum according to claim 6, characterized in that: the oxidant is hydrogen peroxide, the mass fraction of the hydrogen peroxide is 15-30%, the dosage of the hydrogen peroxide is 5-15kg/t, the phosphogypsum is washed by water, and the time of the oxidation treatment is 20-60min.
10. The method for the innocent treatment of phosphogypsum according to claim 6, which is characterized in that: step S 6 Adjusting pH to 6.5-8.0 with calx, and neutralizing for 10-20min.
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