CN114605094A - Method for improving whiteness and purity of phosphogypsum by combination of selection and metallurgy - Google Patents
Method for improving whiteness and purity of phosphogypsum by combination of selection and metallurgy Download PDFInfo
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- CN114605094A CN114605094A CN202210314436.2A CN202210314436A CN114605094A CN 114605094 A CN114605094 A CN 114605094A CN 202210314436 A CN202210314436 A CN 202210314436A CN 114605094 A CN114605094 A CN 114605094A
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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
-
- 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
-
- 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
-
- 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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- 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
- C01P2006/80—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
Abstract
The invention discloses a method for improving the whiteness and the purity of phosphogypsum by combining selection and metallurgy, and relates to the technical field of phosphogypsum treatment. Grading phosphogypsum from wet-process phosphoric acid production, and enabling products with the grain size of +120 meshes and the grain size of-500 meshes to enter a tailing pond and enabling products with the grain size of-120 to +500 meshes to enter flotation operation; adding a desiliconized collecting agent and a desiliconized collecting agent into phosphogypsum after size mixing, performing primary roughing, adding a regulator and a desiliconized collecting agent into roughed concentrate, uniformly mixing, and performing primary concentration, wherein the cleaner concentrate is purified phosphogypsum; and drying the purified phosphogypsum, adding ammonium chloride, grinding and calcining to obtain the whitened purified phosphogypsum. After the phosphogypsum is graded, a part of organic matters and silicon dioxide are removed, further purification is carried out after primary-secondary-fine reverse flotation, and after purification, ammonium chloride is added for grinding and calcining, the phosphogypsum with high whiteness and purity is obtained, so that the high-valued application condition of the phosphogypsum is met, and the economic benefit is improved.
Description
Technical Field
The invention relates to the technical field of phosphogypsum treatment, in particular to a method for improving the whiteness and purity of phosphogypsum by combining selection and metallurgy.
Background
The phosphogypsum is a byproduct generated by preparing phosphoric acid by decomposing phosphate ore with sulfuric acid in the production process of wet-process phosphoric acid, and the main component of the phosphogypsum is calcium sulfate CaSO4·nH2O, reaction formula is Ca5F(PO4)3+5H2SO4+10H2O＝5CaSO4·nH2O+3H3PO4+ HF ↓, the content of which can reach about 70% -90% generally. The phosphogypsum contains undecomposed phosphorite and impurities such as phosphoric acid, fluorine, iron, aluminum compounds, acid insoluble substances, organic matters and the like which are not washed clean, which brings great difficulty to the resource utilization of the phosphogypsum. Generally, 4-4.5 t of phosphogypsum can be discharged when 1t of phosphoric acid is produced by a wet method. The stockpiling amount of phosphogypsum in China exceeds 5 hundred million t, and about 7000 million t of phosphogypsum is newly added every year, so the resource utilization problem of the phosphogypsum is paid much attention in China. At present, the method for treating phosphogypsum by domestic large-scale phosphate fertilizer enterprises mostly adopts wet-method slag discharge and is built and stockpiled in the valley; the small-sized phosphate fertilizer enterprises mostly adopt dry-method slag discharge and flat land stockpiling.
Along with the continuous accumulation of the phosphogypsum, the storage capacity of a slag yard is gradually reduced, and the phosphogypsum stockpiling not only occupies a large amount of land resources, but also pollutes soil and rivers and destroys the ecological environment. Whether the phosphogypsum can be effectively utilized becomes a difficult problem restricting the development of phosphorus chemical industry, and the country gradually enforces a policy of setting the yield of the device by the consumption of the phosphogypsum, so that the environmental protection pressure is higher and higher. The development and utilization of the application technology of the phosphogypsum are imminent.
Because the phosphogypsum contains a large amount of organic matters, silicon dioxide, unreacted apatite, iron magnesium oxide and other impurities, 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 the phosphogypsum is improved, the phosphogypsum can be used in the fields of building wall materials, PVC/PE fillers and the like to replace natural gypsum, the natural gypsum resources are saved, the added value of the phosphogypsum is improved, and the aim of changing waste into valuable is fulfilled. Therefore, the development of a phosphogypsum treatment method with short flow, good whiteness improving effect and low energy consumption is urgently needed.
Disclosure of Invention
The invention aims to provide a method for improving the whiteness and the purity of phosphogypsum by combination of selection and metallurgy, and solves the problem that the existing phosphogypsum has low whiteness and low development and utilization rate due to the fact that the existing phosphogypsum contains a large amount of impurities.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for improving the whiteness and purity of phosphogypsum by combination of concentration and metallurgy is characterized by comprising the following steps:
s1, classifying phosphogypsum from wet-process phosphoric acid production, and enabling products with a grain size of +120 meshes and a grain size of-500 meshes to enter a tailing pond and enabling products with a grain size of-120 to +500 meshes to enter flotation operation;
s2, pulping phosphogypsum of-120 to +500 meshes to the concentration of 25-30%, adding a desiliconization collecting agent and a de-organic matter collecting agent, uniformly mixing, performing primary roughing, and taking flotation foam as roughing tailings; adding a regulator and a desiliconization collecting agent into the rough concentration 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, drying the purified phosphogypsum, adding ammonium chloride, grinding for 1-1.2 hours, and calcining for 1-1.5 hours at 650-700 ℃ to obtain the whitened purified phosphogypsum.
The further technical scheme is that the desiliconization collecting agent in the primary rough separation in the step S2 is prepared from dodecyl trimethyl ammonium bromide, dodecylamine and acetic acid, the adding amount is 180-250 g/t, and the organic matter removing 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 primary fine selection in the step S2, a desilication collecting agent prepared from dodecyl trimethyl ammonium bromide, dodecylamine and acetic acid is added, the adding amount is 150-200 g/t, and CaO is added after full reaction to adjust the pH value of ore pulp.
The further technical scheme is that the adding amount of the ammonium chloride in the step S3 is 2-4% of the mass of the purified phosphogypsum.
The further technical scheme is that the whiteness of the whitened phosphogypsum is more than or equal to 92.9 percent and the purity is more than or equal to 98.1 percent in the step S3.
The working principle is as follows: grading phosphogypsum, removing products with a grain size of +120 meshes and a grain size of-500 meshes, removing a part of organic matters and silicon dioxide, taking the phosphogypsum with the grain size of-120 to +500 meshes as a flotation feed, mixing pulp, adopting a primary-secondary-fine reverse flotation process to further remove 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 percent and the purity of more than or equal to 98.1 percent.
Compared with the prior art, the invention has the beneficial effects that: the phosphogypsum is graded to remove a part of organic matters and silicon dioxide, further purified after rough-fine reverse flotation, purified, added with ammonium chloride, ground and calcined to obtain the phosphogypsum with high whiteness and purity. The whole process flow is short, the dosage of the medicament is small, the addition of the auxiliary agent during the calcination greatly shortens the calcination time, obtains the phosphogypsum with higher whiteness and purity, meets the high-valued application condition of the phosphogypsum, and improves the economic benefit.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
After phosphogypsum produced by a wet-process phosphoric acid device of a certain fertilizer plant is classified, the plus 120 mesh size fraction and the minus 500 mesh size fraction are removed, phosphogypsum with the minus 120 to the plus 500 mesh size fraction is selected as a flotation feed, and a 'primary coarse-primary fine' reverse flotation process is adopted. The phosphogypsum is slurried to the concentration of 26.67 percent, and dodecyl trimethyl ammonium bromide, lauryl amine and acetic acid are added according to a certain proportion during roughing200g/t of desiliconized collecting agent and 160g/t of organic matter removing collecting agent which are prepared according to a certain proportion, wherein the desiliconized collecting agent is formed by mixing kerosene and terpineol according to a mass ratio of 1.1:1, flotation foam is used as rougher tailings, 200g/t of desiliconized collecting agent prepared by dodecyl trimethyl ammonium bromide, dodecylamine and acetic acid according to a certain proportion is added into rougher tailings to adjust the pH value of ore pulp, primary concentration is carried out, silicon dioxide in phosphogypsum is further removed, the flotation foam is used as cleaner tailings, and the cleaner concentrate is purified phosphogypsum. After the concentrated concentrate is dried, NH with the mass of 2.5 percent of the purified phosphogypsum is added4And Cl grinding for 1h, then placing the ground material in a muffle furnace, setting the calcining temperature at 660 ℃ and the calcining time at 1h, and obtaining the whitened purified phosphogypsum.
Example 2
After phosphogypsum produced by a wet-process phosphoric acid device of a certain fertilizer plant is classified, the plus 120 mesh size fraction and the minus 500 mesh size fraction are removed, phosphogypsum with the minus 120 to the plus 500 mesh size fraction is selected as a flotation feed, and a 'primary coarse-primary fine' reverse flotation process is adopted. The phosphogypsum is subjected to size mixing until the concentration is 27.4%, 230g/t of desilication collecting agent prepared by dodecyl trimethyl ammonium bromide, lauryl amine and acetic acid according to a certain proportion is added during roughing, 180g/t of organic matter removal collecting agent is added, the desilication collecting agent is formed by mixing kerosene and terpineol according to the mass ratio of 1.3:1, flotation foam is used as roughing tailings, 180g/t of desilication collecting agent prepared by dodecyl trimethyl ammonium bromide, lauryl amine and acetic acid according to a certain proportion is added into the roughing tailings, CaO is added to adjust the pH value of ore pulp, primary concentration is carried out, silicon dioxide in the phosphogypsum is further removed, the flotation foam is used as concentrating tailings, and the concentrate concentration is purified phosphogypsum. After the concentrated concentrate is dried, NH with the mass of 3 percent of the purified phosphogypsum is added4And (3) Cl grinding for 1h, then placing the ground material in a muffle furnace, setting the calcining temperature to 680 ℃, and the calcining time to 1h to obtain the whitened purified phosphogypsum.
Example 3
After phosphogypsum produced by a wet-process phosphoric acid device of a certain fertilizer plant is classified, the plus 120 mesh size fraction and the minus 500 mesh size fraction are removed, phosphogypsum with the minus 120 to the plus 500 mesh size fraction is selected as a flotation feed material, and a 'first coarse and first fine' reverse reaction is adoptedAnd (4) a flotation process. The phosphogypsum is subjected to size mixing until the concentration is 29.3 percent, 220g/t of desilication collecting agent prepared by dodecyl trimethyl ammonium bromide, lauryl amine and acetic acid according to a certain proportion is added during roughing, 170g/t of organic matter removal collecting agent is added, the desilication collecting agent is formed by mixing kerosene and terpineol according to the mass ratio of 1.4:1, flotation foam is used as roughing tailings, 200g/t of desilication collecting agent prepared by dodecyl trimethyl ammonium bromide, lauryl amine and acetic acid according to a certain proportion is added into the roughing tailings, CaO is added to adjust ore pulp, primary concentration is carried out, silicon dioxide in the phosphogypsum is further removed, the flotation foam is used as concentrating tailings, and the concentrating concentrate is purified phosphogypsum. After the concentrated concentrate is dried, NH with the mass of 3.5 percent of the purified phosphogypsum is added4And Cl grinding for 1h, then placing the ground material in a muffle furnace, setting the calcining temperature at 690 ℃, and the calcining time at 1h to obtain the whitened purified phosphogypsum.
The whiteness of the phosphogypsum raw material, the flotation concentrate and the final calcined concentrate of the examples 1-3 is detected, and the specific results are shown in table 1. From the table 1, the whiteness of the phosphogypsum products obtained by the treatment methods of the embodiments 1 to 3 of the invention is higher than 92%, the purity is higher than 98%, and the high-value utilization of the phosphogypsum can be realized.
TABLE 1 examination of phosphogypsum products at various stages
As for the particle size screening data table 2 of the phosphogypsum obtained in the wet-process phosphoric acid production process, the removal of the plus 120-mesh fraction and the minus 500-mesh fraction during the classification of the phosphogypsum can remove the fraction with high silicon content and part of organic matters in the phosphogypsum from the table 2.
Table 2 phosphogypsum particle size screening data
TABLE 3 whiteness distribution of each grade in raw phosphogypsum ore
While the invention 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 particularly, various variations and modifications are possible in the component parts or arrangements within the scope of the disclosure and the claims. In addition to variations and modifications in the component parts or arrangements, other uses will also be apparent to those skilled in the art.
Claims (5)
1. A method for improving the whiteness and purity of phosphogypsum by combination of concentration and metallurgy is characterized by comprising the following steps:
s1, classifying phosphogypsum from wet-process phosphoric acid production, and enabling products with a grain size of +120 meshes and a grain size of-500 meshes to enter a tailing pond and enabling products with a grain size of-120 to +500 meshes to enter flotation operation;
s2, pulping phosphogypsum of-120 to +500 meshes to 25-30%, adding a desiliconization collecting agent and a de-organic matter collecting agent, uniformly mixing, performing primary roughing, and taking flotation foam as roughing tailings; adding a regulator and a desiliconization collecting agent into the rough concentration concentrate, uniformly mixing, and then carrying out primary concentration, wherein flotation foam is used as concentration tailings, and the concentration concentrate is purified phosphogypsum;
and S3, drying the purified phosphogypsum, adding ammonium chloride, grinding for 1-1.2 h, and calcining for 1-1.5 h at 650-700 ℃ to obtain the whitened purified phosphogypsum.
2. The method for combined dressing and metallurgy for improving the whiteness and purity of phosphogypsum according to claim 1, which is characterized in that: step (ii) of
The desilication collecting agent in the primary rough separation in the S2 is prepared from dodecyl trimethyl ammonium bromide, dodecylamine and acetic acid, and the adding amount is 180-250 g/t; the organic matter removing collecting agent is prepared from kerosene and terpineol oil in a mass ratio of 1-1.5: 1, and the addition amount is 120-200 g/t.
3. The method for combined dressing and metallurgy for improving the whiteness and purity of phosphogypsum according to claim 1, which is characterized in that: step (ii) of
In the primary fine selection of S2, 150-200 g/t desilication collecting agent is added firstly, and then CaO is added to adjust the pH value of the ore pulp.
4. The method for combined dressing and metallurgy for improving the whiteness and purity of phosphogypsum according to claim 1, which is characterized in that: in the step S3, the adding amount of the ammonium chloride is 2-4% of the mass of the purified phosphogypsum.
5. The method for combined dressing and metallurgy for improving the whiteness and purity of phosphogypsum according to claim 1, which is characterized in that: the whiteness of the whitened phosphogypsum is more than or equal to 92.9 percent and the purity is more than or equal to 98.1 percent in the step S3.
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Cited By (3)
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| CN115672568A (en) * | 2022-12-30 | 2023-02-03 | 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 |
| CN115784290A (en) * | 2022-11-08 | 2023-03-14 | 宜都兴发化工有限公司 | Process for purifying phosphogypsum by molten salt leaching method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115650276A (en) * | 2022-10-25 | 2023-01-31 | 湖北三峡实验室 | Comprehensive recovery method of phosphogypsum resources |
| CN115784290A (en) * | 2022-11-08 | 2023-03-14 | 宜都兴发化工有限公司 | Process for purifying phosphogypsum by molten salt leaching method |
| 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 |
| CN115672568A (en) * | 2022-12-30 | 2023-02-03 | 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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