CN114605094B - Method for improving whiteness and purity of phosphogypsum by combination of dressing and smelting - Google Patents
Method for improving whiteness and purity of phosphogypsum by combination of dressing and smelting Download PDFInfo
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- CN114605094B CN114605094B CN202210314436.2A CN202210314436A CN114605094B CN 114605094 B CN114605094 B CN 114605094B CN 202210314436 A CN202210314436 A CN 202210314436A CN 114605094 B CN114605094 B CN 114605094B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
- C04B11/266—Chemical gypsum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
- C04B11/024—Ingredients added before, or during, the calcining process, e.g. calcination modifiers
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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Abstract
The application discloses a method for improving whiteness and purity of phosphogypsum by combining dressing and smelting, and relates to the technical field of phosphogypsum treatment. Phosphogypsum from wet phosphoric acid production is classified, products of +120 mesh size fraction and-500 mesh size fraction enter a tailing slag warehouse, and the products of-120 mesh to +500 mesh size fraction enter flotation operation; adding a desilication collecting agent and a desilication collecting agent after phosphogypsum pulp mixing, carrying out primary roughing, adding a regulator and the desilication collecting agent into roughing concentrate, carrying out primary concentration after uniform mixing, and concentrating the concentrate into purified phosphogypsum; and (3) drying the purified phosphogypsum, adding ammonium chloride, grinding and calcining to obtain the whitened purified phosphogypsum. The phosphogypsum is classified to remove a part of organic matters and silicon dioxide, then is subjected to coarse-fine reverse flotation and further purified, ammonium chloride is added after the purification, and the phosphogypsum with high whiteness and purity is obtained by grinding and calcining, so that the high-valued application condition of the phosphogypsum is met, and the economic benefit is improved.
Description
Technical Field
The application relates to the technical field of phosphogypsum treatment, in particular to a method for improving whiteness and purity of phosphogypsum by combining dressing and smelting.
Background
Phosphogypsum is a byproduct produced by decomposing phosphate ore by sulfuric acid in the wet-process phosphoric acid production process, and the main component of phosphogypsum is calcium sulfate CaSO 4 ·nH 2 O, the reaction formula is Ca 5 F(PO 4 ) 3 +5H 2 SO 4 +10H 2 O＝5CaSO 4 ·nH 2 O+3H 3 PO 4 The content of the +HF ≡is generally about 70% -90%. The phosphogypsum contains non-decomposed phosphorite, and impurities such as phosphoric acid, fluorine, iron, aluminum compounds, acid insoluble substances, organic matters and the like which are not washed cleanly, so that the resource utilization of the phosphogypsum is difficult. The phosphoric acid of 1t is generally produced by a wet method, and 4 to 4.5t phosphogypsum can be discharged. The phosphogypsum stock in China is more than 5 hundred million t, and about 7000 ten thousand t phosphogypsum is newly added each year, so the problem of resource utilization of phosphogypsum is valued in China. At present, wet deslagging is mostly adopted in the method for treating phosphogypsum in large-scale phosphate fertilizer enterprises in China, and the phosphogypsum is piled up in the mountain valley to build a dam; dry deslagging is mostly adopted by small phosphate fertilizer enterprises, and the phosphate fertilizer enterprises are piled up on flat ground.
Along with the continuous accumulation of phosphogypsum, the storage capacity of a slag yard is gradually reduced, and phosphogypsum is piled up to occupy a large amount of land resources, pollute soil and rivers and destroy ecological environment. Whether phosphogypsum can be effectively utilized becomes a difficult problem for restricting the development of phosphorus chemical industry, and the country is gradually pushing the policy of determining the yield of the device according to the consumption of phosphogypsum, so that the environmental protection pressure is increased. The development and utilization of phosphogypsum application technology is urgent.
Phosphogypsum contains a large amount of organic matters, silicon dioxide, unreacted apatite, iron magnesium oxide and other impurities, so that the phosphogypsum has low whiteness, can only be applied to the directions of cement, roadbed, soil conditioner and the like, and cannot realize high-value application. The whiteness of phosphogypsum is improved, the phosphogypsum can be used as a building wall material, PVC/PE filler and other fields to replace natural gypsum, the added value of the phosphogypsum is improved while the natural gypsum resource is saved, and the aim of changing waste into valuables is fulfilled. Therefore, development of a phosphogypsum treatment method with short process, good whiteness improvement effect and low energy consumption is needed.
Disclosure of Invention
The application aims to provide a method for improving the whiteness and purity of phosphogypsum by combining dressing and smelting, which solves the problems of low whiteness, low development and utilization rate of the existing phosphogypsum caused by a large amount of impurities.
In order to solve the technical problems, the application adopts the following technical scheme: a method for improving whiteness and purity of phosphogypsum by combining dressing and smelting is characterized by comprising the following steps:
s1, classifying phosphogypsum from wet phosphoric acid production, enabling products with the size of +120 meshes and products with the size of-500 meshes to enter a tailing pond, and enabling the products with the size of-120 meshes to +500 meshes to enter flotation operation;
s2, pulping phosphogypsum of a size fraction of-120- +500 meshes to a concentration of 25% -30%, adding a desilication collecting agent and a deorganization collecting agent, uniformly mixing, and performing primary roughing, wherein flotation foam is used as roughing tailings; adding a regulator and a desilication collector into the roughing concentrate, uniformly mixing, and then carrying out primary concentration, wherein flotation foam is used as concentration tailings, and the concentration concentrate is purified phosphogypsum;
s3, adding ammonium chloride into the purified phosphogypsum after drying for grinding for 1-1.2 h, and calcining at 650-700 ℃ for 1-1.5 h to obtain the whitened purified phosphogypsum.
The further technical scheme is that the desilication collecting agent in the primary roughing in the step S2 is prepared from dodecyl trimethyl ammonium bromide, dodecyl amine and acetic acid, the adding amount is 180-250 g/t, and the desilication collecting agent is prepared from kerosene and pine oil according to the mass ratio of 1-1.5: 1, and the addition amount is 120-200 g/t.
The further technical scheme is that in the step S2, a desilication collecting agent prepared from dodecyl trimethyl ammonium bromide, dodecyl amine and acetic acid is firstly added in the primary refining, the adding amount is 150-200 g/t, and CaO is added to adjust the pH value of ore pulp after full reaction.
The further technical proposal is that the adding amount of the ammonium chloride in the step S3 is 2 to 4 percent of the mass of the purified phosphogypsum.
The further technical proposal is that the whiteness of the phosphogypsum after the whitening in the step S3 is more than or equal to 92.9 percent, and the purity is more than or equal to 98.1 percent.
Working principle: classifying phosphogypsum, removing products of +120 mesh grade and-500 mesh grade, removing a part of organic matters and silicon dioxide, taking the phosphogypsum of-120- +500 mesh grade as flotation feed, adopting a coarse-fine reverse flotation process after size mixing, further removing the organic matters and the silicon dioxide, adding ammonium chloride into the purified phosphogypsum after flotation, grinding and calcining to obtain the high-purity phosphogypsum with the whiteness of more than or equal to 92.9% and the purity of more than or equal to 98.1%.
Compared with the prior art, the application has the beneficial effects that: the method for improving the whiteness and purity of phosphogypsum by combining dressing and smelting is provided, wherein part of organic matters and silicon dioxide are removed from phosphogypsum after classification, the phosphogypsum is further purified after reverse flotation of coarse material and fine material, and ammonium chloride is added after the purification for grinding and calcining to obtain phosphogypsum with high whiteness and purity. The whole process flow is short, the dosage of the agent is small, the addition agent is added during calcination, the calcination time is greatly shortened, the phosphogypsum with higher whiteness and purity is obtained, the high-valued application condition of the phosphogypsum is satisfied, and the economic benefit is improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application will be described in further detail with reference to the following examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
Example 1
After phosphogypsum produced by a wet-process phosphoric acid device of a certain fertilizer plant is classified, removing the phosphogypsum with the size of +120 meshes and the phosphogypsum with the size of-500 meshes, selecting the phosphogypsum with the size of-120 to +500 meshes as a flotation feed, and adopting a 'coarse and fine' reverse flotation process. Mixing phosphogypsum to a concentration of 26.67%, adding 200g/t of desilication collector prepared from dodecyl trimethyl ammonium bromide, dodecyl diamine and acetic acid according to a certain proportion during roughing, mixing 160g/t of desilication collector with a mass ratio of 1.1:1, taking flotation foam as roughing tailings, adding 200g/t of desilication collector prepared from dodecyl trimethyl ammonium bromide, dodecyl diamine and acetic acid according to a certain proportion into roughing concentrate, adding CaO to adjust the pH of ore pulp, carrying out primary concentration, further removing silicon dioxide in phosphogypsum, taking flotation foam as concentrating tailings, and taking the concentrating concentrate as purified phosphogypsum. Drying the concentrate, adding NH 2.5% of the purified phosphogypsum 4 Cl was milled for 1h, followed by placing the milled material inSetting the calcining temperature in a muffle furnace at 660 ℃ and the calcining time at 1h to obtain the whitened purified phosphogypsum.
Example 2
After phosphogypsum produced by a wet-process phosphoric acid device of a certain fertilizer plant is classified, removing the phosphogypsum with the size of +120 meshes and the phosphogypsum with the size of-500 meshes, selecting the phosphogypsum with the size of-120 to +500 meshes as a flotation feed, and adopting a 'coarse and fine' reverse flotation process. Mixing phosphogypsum to a concentration of 27.4%, adding 230g/t of desilication collector prepared from dodecyl trimethyl ammonium bromide, dodecyl diamine and acetic acid according to a certain proportion during roughing, 180g/t of organic matters removing collector which is prepared by mixing kerosene and pine oil according to a mass ratio of 1.3:1, taking flotation foam as roughing tailings, adding 180g/t of desilication collector prepared from dodecyl trimethyl ammonium bromide, dodecyl diamine and acetic acid according to a certain proportion into roughing concentrate, adding CaO to adjust the pH of ore pulp, carrying out primary concentration, further removing silicon dioxide in phosphogypsum, taking flotation foam as concentrating tailings, and taking the concentrating concentrate as purified phosphogypsum. Drying the concentrate, and adding NH 3% of the mass of the purified phosphogypsum 4 Cl is ground for 1h, the ground material is placed in a muffle furnace, the calcination temperature is set to 680 ℃, and the calcination time is set to 1h, so that the whitened purified phosphogypsum is obtained.
Example 3
After phosphogypsum produced by a wet-process phosphoric acid device of a certain fertilizer plant is classified, removing the phosphogypsum with the size of +120 meshes and the phosphogypsum with the size of-500 meshes, selecting the phosphogypsum with the size of-120 to +500 meshes as a flotation feed, and adopting a 'coarse and fine' reverse flotation process. Mixing phosphogypsum to a concentration of 29.3%, adding 220g/t of desilication collector prepared from dodecyl trimethyl ammonium bromide, dodecyl diamine and acetic acid according to a certain proportion during roughing, 170g/t of organic matters removing collector which is prepared by mixing kerosene and pine oil according to a mass ratio of 1.4:1, taking flotation foam as roughing tailings, adding 200g/t of desilication collector prepared from dodecyl trimethyl ammonium bromide, dodecyl diamine and acetic acid according to a certain proportion into roughing concentrate, adding CaO to regulate pulp, carrying out primary concentration, further removing silicon dioxide in phosphogypsum, taking flotation foam as concentrating tailings, and concentrating concentrate as purified concentratePhosphogypsum. Drying the concentrate, adding NH 3.5% of the purified phosphogypsum 4 Cl is ground for 1h, the ground material is placed in a muffle furnace, the calcination temperature is set to 690 ℃, and the calcination time is set to 1h, so that the whitened purified phosphogypsum is obtained.
The phosphogypsum raw materials, the flotation concentrate and the final calcined concentrate of examples 1 to 3 were tested for whiteness, and the specific results are shown in Table 1. As can be seen from Table 1, the phosphogypsum products obtained by the treatment methods of examples 1 to 3 of the present application have whiteness higher than 92% and purity higher than 98%, and can realize high-value utilization of phosphogypsum.
Table 1 phosphogypsum product test at each stage
For the particle size sieve analysis data of phosphogypsum obtained in the wet process phosphoric acid production process, table 2 shows that the removal of +120 mesh fraction and-500 mesh fraction can remove the fraction and part of organic matters with high silicon content in phosphogypsum when the phosphogypsum is classified.
TABLE 2 phosphogypsum particle size Screen analysis data
TABLE 3 whiteness distribution of various grades in phosphogypsum raw ore
While the application has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope of the disclosure. More specifically, various modifications and improvements may be made to the component parts or arrangements within the scope of the disclosure and claims. In addition to variations and modifications in the component parts or arrangements, other uses will be apparent to those skilled in the art.
Claims (1)
1. A method for improving whiteness and purity of phosphogypsum by combining dressing and smelting is characterized by comprising the following steps:
s1, classifying phosphogypsum from wet phosphoric acid production, enabling products with the size of +120 meshes and products with the size of-500 meshes to enter a tailing pond, and enabling the products with the size of-120 meshes to +500 meshes to enter flotation operation;
s2, mixing phosphogypsum of a size fraction of-120- +500 meshes to 26.67% -29.3%, adding a desilication collector and a desilication organic matter collector, uniformly mixing, and performing primary roughing, wherein flotation foam is used as roughing tailings; adding a regulator and a desilication collector into the roughing concentrate, uniformly mixing, and then carrying out primary concentration, wherein flotation foam is used as concentration tailings, and the concentration concentrate is purified phosphogypsum; the desilication collecting agent is prepared from dodecyl trimethyl ammonium bromide, dodecyl amine and acetic acid, wherein the regulator is CaO, and the desilication organic matter collecting agent is prepared from kerosene and terpineol oil according to the mass ratio of 1-1.5: 1, mixing; the addition amount of the desilication collecting agent in one roughing is 200-230 g/t, and the addition amount of the organic matters removing collecting agent is 160-180 g/t; in the primary refining, 150-200 g/t desilication collecting agent is added, and then CaO is added to adjust the pH value of ore pulp;
s3, adding ammonium chloride into the purified phosphogypsum after drying for grinding for 1-1.2 h, and calcining at 650-690 ℃ for 1-1.5 h to obtain the whitened purified phosphogypsum; the addition amount of the ammonium chloride is 2 to 4 percent of the mass of the purified phosphogypsum; the whiteness of the whitened phosphogypsum is more than or equal to 92.9%, and the purity is more than or equal to 98.1%.
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| CN115650276A (en) * | 2022-10-25 | 2023-01-31 | 湖北三峡实验室 | Comprehensive recovery method of phosphogypsum resources |
| CN115784290B (en) * | 2022-11-08 | 2024-03-12 | 宜都兴发化工有限公司 | Process for purifying phosphogypsum by molten salt leaching method |
| CN115672568B (en) * | 2022-12-30 | 2023-03-14 | 矿冶科技集团有限公司 | Method for preparing low-silicon high-grade phosphogypsum by reverse flotation and desiliconization of phosphogypsum waste residues |
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Inventor after: Guo Yongjie Inventor after: Li Jiangli Inventor after: Peng Hua Inventor after: Li Haibing Inventor after: Chen Ciyun Inventor after: Fan Peiqiang Inventor after: Wang Menglai Inventor after: Du Lingpan Inventor before: Guo Yongjie Inventor before: Li Jiangli Inventor before: Peng Hua Inventor before: Li Haibing Inventor before: Chen Ciyun Inventor before: Fan Peiqiang Inventor before: Wang Menglai |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |