CN112624641B - Method for completely recycling phosphate tailings without waste residues - Google Patents
Method for completely recycling phosphate tailings without waste residues Download PDFInfo
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- CN112624641B CN112624641B CN202011559149.5A CN202011559149A CN112624641B CN 112624641 B CN112624641 B CN 112624641B CN 202011559149 A CN202011559149 A CN 202011559149A CN 112624641 B CN112624641 B CN 112624641B
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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
- C04B7/00—Hydraulic cements
- C04B7/32—Aluminous cements
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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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
- C01F7/00—Compounds of aluminium
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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
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
Abstract
The invention discloses a method for utilizing phosphorus tailings in a full-recycling manner without waste residues. Taking phosphate tailings generated by phosphorite flotation as a raw material, and performing acid dissolution, solid-liquid separation and calcination by a reasonable disposal means to obtain belite-sulphoaluminate cement clinker; dropwise adding ammonia water, carrying out solid-liquid separation, and drying to obtain ammonium dihydrogen phosphate; dropwise adding alkali liquor, carrying out solid-liquid separation, and drying to obtain hydrotalcite; and (4) dropwise adding dilute hydrochloric acid, and drying to obtain sodium chloride. No waste residue is generated in the whole disposal process, the environmental load caused by industrial waste residue accumulation is reduced, and the method has extremely high environmental benefit and economic benefit. The adopted raw materials comprise dilute hydrochloric acid, bauxite, carbide slag, ammonia water, sodium hydroxide and the like, and the raw materials are low in price and easy to obtain, and have high economic benefit.
Description
Technical Field
The invention belongs to the technical field of environmental engineering, and particularly relates to a method for full recycling of phosphorus tailings without waste residues.
Background
China is a large industrial country, and needs to exploit and utilize a large amount of mineral resources, develop the mineral resources and simultaneously generate a large amount of industrial byproducts. The random stacking of industrial waste residue causes a plurality of environmental problems, threatens the survival of human beings, and the harmless treatment becomes the scientific problem to be solved urgently at present. Therefore, mineral resources are reasonably and efficiently developed, and the problems of industrial waste residue accumulation, environmental pollution and the like can be fundamentally solved by reducing the generation of industrial waste residue.
The phosphate tailings are products containing more phosphorus and lower impurity minerals in the flotation enrichment process of high-grade phosphate ores and medium-low-grade collophanite ores. The mineral composition of the phosphate tailings is mainly CaCO 3 、CaSO 4 、MgCO 3 、SiO 2 、P 2 O 5 Etc. in the content of 40-60%, 5-10%, 20-40%, 4-6% and 4-6%, respectively. If the components in the phosphorus tailings waste residue can be recycled, the method has very important significance.
The belite-sulphoaluminate cement is novel low-carbon environment-friendly cement, mainly comprises calcium sulphoaluminate, dicalcium silicate, calcium sulphosilicate and tetracalcium aluminoferrite, has the advantages of fast condensation, high strength, excellent low-temperature performance, micro-expansion and low shrinkage, and is very suitable for the special engineering fields of marine concrete, crack repair, rapid construction in winter and the like.
Ammonium dihydrogen phosphate is white crystalline powder, is mainly used as a fire retardant for fertilizers and wood, paper and fabrics, and is also used as a feed additive for pharmacy and ruminants.
Hydrotalcite of CaO, MgO, Al 2 O 3 Laminate of main chemical composition and CO 3 2- Interlayer ionic compound, the layer plate structure is formed by CaO, MgO and Al 2 O 3 The radii of the metal elements are different, and the charge distribution in the plates is unbalanced, so that anions are filled between the plates to balance the charge. The hydrotalcite has wide application in building material asphalt, and can enhance the ultraviolet aging resistant effect of the modified asphalt and prolong the service life of the asphalt by utilizing the excellent optical characteristics of the hydrotalcite.
The sodium chloride is white crystal in appearance, is the main component of common salt, and is prepared by evaporating and crystallizing seawater.
Disclosure of Invention
The invention aims to realize the aim of no waste slag discharge in the process of resource treatment of the phosphorus tailings, utilize the whole components of the phosphorus tailings, reduce the damage to the environment and have positive environmental benefit and economic benefit.
In order to achieve the purpose, the technical scheme is as follows:
a method for utilizing phosphorus tailings in a waste residue-free full-recycling manner comprises the following steps:
(1) calcining the phosphorus tailings to remove organic impurities, and grinding the calcined phosphorus tailings into powder;
(2) preparing hydrochloric acid diluent, adding calcined phosphorus tailing powder, heating and stirring until the calcined phosphorus tailing powder is completely dissolved to obtain a tan emulsion; carrying out suction filtration to obtain brown yellow filter residue and light yellow filtrate;
(3) adding carbide slag and bauxite into the obtained filter residue, placing the mixture into a vibration mill for grinding, uniformly mixing, and pressing and forming; placing the mixture in a muffle furnace for high-temperature calcination to obtain belite-sulphoaluminate cement clinker;
(4) dropwise adding ammonia water into the obtained light yellow filtrate, adjusting the pH value to 6-7, heating for reaction, and performing suction filtration to obtain milky filter residues and a clear solution;
(5) drying the milky white filter residue to obtain ammonium dihydrogen phosphate crystals;
(6) adding aluminum salt into the obtained clear solution to obtain a mixed salt solution, dropwise adding a sodium hydroxide solution into the clear solution, adjusting the pH value to 10-11, carrying out coprecipitation reaction, heating, stirring, aging, and carrying out suction filtration to obtain white filter residues and a transparent solution;
(7) drying the obtained white filter residue to obtain hydrotalcite; and adding a dilute hydrochloric acid solution into the obtained transparent solution, adjusting the pH value to 6-8, and drying to obtain sodium chloride.
According to the scheme, the calcining temperature in the step 1) is 600-900 ℃, and the time is 1-3 h.
According to the scheme, the temperature rise in the step 2) is 50-80 ℃, and the stirring time is 0.5-2 h.
According to the scheme, the raw materials in the step 3) are as follows by mass percent: 25 to 40 percent of filter residue; 30% -60% of carbide slag; 10 to 30 percent of bauxite.
According to the scheme, in the step 3), the grinding fineness is less than 200 meshes, the calcining temperature is 1150-1280 ℃, the calcining time is 1-4 hours, and the calcined powder is placed into liquid nitrogen for rapid cooling.
According to the scheme, the concentration of ammonia water in the step 4) is 8-35 wt%, the temperature rise is 30-50 ℃, and the reaction time is 0.5-2 h.
According to the scheme, the drying temperature in the step 5) is 80-100 ℃, and the drying time is 20-30 h.
According to the above scheme, Mg in the clarified solution of step 6) 2+ 、Ca 2+ The molar ratio of (1-3) to 1; the molar ratio of the aluminum ions to the divalent metal ions is 1: (1-4); the concentration of the sodium hydroxide solution is 0.3-0.5 mol/L.
According to the scheme, the temperature of the coprecipitation method in the step 6) is raised to 45-75 ℃, and the stirring reaction time is 0.5-1.5 h; the aging temperature in the step 6) is 90-110 ℃, the time is 15-30 h, and the pH value of the transparent solution obtained by suction filtration is 7-8.
According to the scheme, the concentration of the dilute hydrochloric acid solution in the step 7) is 0.1-2.5 mol/L; the drying temperature of the hydrotalcite is 60-120 ℃, and the drying time is 15-30 h.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes phosphate tailings generated by phosphorite flotation as raw materials, and the belite-sulphoaluminate cement clinker is obtained by reasonable disposal means, acid dissolution, solid-liquid separation and calcination; dropwise adding ammonia water, carrying out solid-liquid separation, and drying to obtain ammonium dihydrogen phosphate; dropwise adding alkali liquor, carrying out solid-liquid separation, and drying to obtain hydrotalcite; and (4) dropwise adding dilute hydrochloric acid, and drying to obtain sodium chloride. No waste residue is generated in the whole disposal process, the environmental load caused by industrial waste residue accumulation is reduced, and the method has extremely high environmental benefit and economic benefit.
The raw materials adopted by the invention comprise dilute hydrochloric acid, bauxite, carbide slag, ammonia water, sodium hydroxide and the like, and the raw materials are low in price and easy to obtain, so that the method has high economic benefit.
The process flow adopted by the invention is simple and convenient, and has extremely high practical value, thereby being beneficial to popularization and industrial application.
Drawings
FIG. 1: XRD pattern of milky white residue obtained in example 1.
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
The phosphorus tailings used in the following examples were produced from ecological limited company in Ehou, Hubei province and had the chemical composition shown in Table 1, and the contents of MgO, SiO2, P2O5, SO3 and CaO in major oxides were 26.62%, 4.57%, 5.44%, 3.11% and 45.96%.
Example 1
Weighing 100g of phosphorus tailings, placing the phosphorus tailings in a high-temperature furnace, setting the temperature to be 800 ℃, calcining for 2 hours, and grinding the calcined phosphorus tailings into powder;
mixing 116ml of hydrochloric acid with the content of 36-38% with pure water with the same volume, adding the mixture into a stirring reactor, stirring, heating to 60 ℃, slowly adding the phosphorus tailings subjected to impurity removal in the step 1), stirring, performing acidolysis reaction for 1.5 hours, then performing heat preservation and filtration, stirring, and filtering to obtain refined pale yellow filtrate dissolved by hydrochloric acid and brown yellow filter residues;
adding 2 parts of carbide slag and 0.5 part of bauxite into the brown yellow filter residue in proportion and mixing; grinding the mixture in a vibration mill until the fineness is below 200 mm. Pressing and molding the powder, placing the powder in a muffle furnace, calcining at 1200 ℃ for 1 hour to obtain calcined clinker, and placing the calcined clinker in liquid nitrogen for extremely cooling to obtain cement clinker;
adding the light yellow filtrate into a three-neck flask, stirring, dropwise adding 8% ammonia water, adjusting the pH of the light yellow transparent solution to 4, reacting at 30 ℃, and reacting for 1 h. After the reaction is finished, filtering and washing to obtain milky filter residues and a clear solution;
placing the milky white filter residue in a vacuum drying oven, and drying for 30 hours at 80 ℃ to obtain ammonium dihydrogen phosphate crystals; the XRD pattern of the dried milky white filter residue is shown in figure 1, and the main product is ammonium phosphate.
Adding 30g of aluminum chloride hexahydrate into the clear solution, adding a sodium hydroxide solution with the concentration of 2.5mol/L into the clear solution in a dropwise manner, adjusting the pH value to 9, setting the temperature of a magnetic stirrer to be 40 ℃, stirring for 1.5 hours violently, stopping stirring after the mixed salt solution reacts sufficiently, setting the temperature of the magnetic stirrer to be 90 ℃, aging for 18 hours, carrying out vacuum filtration to obtain white filter residues and a transparent solution, and washing a white precipitate to be neutral.
Placing the white filter residue in a vacuum drying oven, and drying for 30 hours at 80 ℃ to obtain hydrotalcite; and adding a 0.1mol/L dilute hydrochloric acid solution into the transparent solution, adjusting the pH value to 6-8, and drying at 60 ℃ to obtain sodium chloride crystals.
The components and contents (wt%) of the phosphorus tailings used in this example and the brownish yellow filter residues and milky white filter residues obtained in the resource utilization process are shown in table 1.
TABLE 1
CO 2 | F | MgO | Al 2 O 3 | SiO 2 | P 2 O 5 | SO 3 | Cl | K 2 O | CaO | TiO 2 | MnO | Fe 2 O 3 | |
Phosphate tailings | 10.60 | 0.67 | 26.62 | 0.91 | 4.57 | 5.44 | 3.11 | 0.05 | 0.39 | 45.96 | 0.10 | 0.36 | 1.07 |
Brown yellow filter residue | 22.37 | 0.71 | 1.28 | 0.77 | 35.10 | 0.34 | 18.79 | 3.61 | 1.10 | 14.09 | 0.45 | 0.03 | 1.07 |
Milky white residue | - | 1.55 | 3.25 | 3.56 | 0.14 | 73.78 | 0.54 | 4.83 | 0.14 | 6.44 | 0.09 | 0.63 | 4.90 |
Example 2
Weighing 100g of phosphorus tailings, placing the phosphorus tailings in a high-temperature furnace, setting the temperature to 900 ℃, calcining for 1 hour, and grinding the calcined phosphorus tailings into powder;
mixing 120ml of hydrochloric acid with the content of 36-38% with pure water with the same volume, adding the mixture into a stirring reactor, stirring, heating to 55 ℃, slowly adding the phosphorus tailings subjected to impurity removal in the step 1), stirring, performing acidolysis reaction for 2 hours, then performing heat preservation, filtration, stirring and filtration to obtain refined hydrochloric acid-dissolved light yellow filtrate and brown yellow filter residues;
adding 2.5 parts of carbide slag and 0.3 part of bauxite into the brown yellow filter residue in proportion and mixing; grinding in a vibration mill to obtain powder with fineness below 200 mm. Pressing and molding the powder, placing the powder in a muffle furnace, calcining at 1250 ℃ for 1 hour to obtain calcined clinker, and placing the calcined clinker in liquid nitrogen for extremely cooling to obtain cement clinker;
adding the light yellow filtrate into a three-neck flask, stirring, dropwise adding 25% ammonia water by mass, adjusting the pH of the light yellow transparent solution to 6, reacting at 40 ℃, and reacting for 0.5 h. After the reaction is finished, filtering to obtain milky filter residues and a clear solution;
placing the milky white filter residue in a vacuum drying oven, and drying for 24 hours at 80 ℃ to obtain ammonium dihydrogen phosphate crystals;
adding 40g of aluminum nitrate nonahydrate into the clear solution, dropwise adding a sodium hydroxide solution with the concentration of 2mol/L into the clear solution, adjusting the pH to 9, setting the temperature of a magnetic stirrer to be 60 ℃, stirring vigorously for 0.5 hour to ensure that the mixed salt solution fully reacts, stopping stirring, setting the temperature of the magnetic stirrer to be 90 ℃, aging for 24 hours, carrying out vacuum filtration to obtain white filter residue and a transparent solution, and washing the white precipitate to be neutral.
Placing the white filter residue in a vacuum drying oven, and drying for 20 hours at 100 ℃ to obtain hydrotalcite; and adding a dilute hydrochloric acid solution with the concentration of 1mol/L into the transparent solution, adjusting the pH value to 6-8, and drying at 60 ℃ to obtain sodium chloride crystals.
Claims (1)
1. A method for utilizing phosphorus tailings in a waste residue-free full-recycling manner is characterized by comprising the following steps:
(1) calcining the phosphorus tailings to remove organic impurities, and grinding the calcined phosphorus tailings into powder; the calcining temperature is 600-900 ℃, and the time is 1-3 h;
(2) preparing hydrochloric acid diluent, adding calcined phosphorus tailing powder, heating and stirring until the calcined phosphorus tailing powder is completely dissolved to obtain a tan emulsion; carrying out suction filtration to obtain brown yellow filter residue and light yellow filtrate; the temperature is raised to 50-80 ℃, and the stirring time is 0.5-2 h;
(3) adding carbide slag and bauxite into the obtained filter residue, placing the mixture into a vibration mill for grinding, uniformly mixing, and pressing and forming; placing the mixture in a muffle furnace for high-temperature calcination to obtain a belite-sulphoaluminate cement clinker; the raw materials are as follows by mass percent: 25 to 40 percent of filter residue; 30-60% of carbide slag; 10 to 30 percent of bauxite; grinding to fineness of less than 200 meshes, calcining at 1150-1280 ℃ for 1-4 hours, and placing into liquid nitrogen for quick cooling after calcining;
(4) dropwise adding ammonia water into the obtained light yellow filtrate, adjusting the pH value to 6-7, heating for reaction, and performing suction filtration to obtain milky filter residues and a clear solution; the concentration of ammonia water is 8-35 wt%, the temperature rise is 30-50 ℃, and the reaction time is 0.5-2 h;
(5) drying the milky white filter residue to obtain ammonium dihydrogen phosphate crystals; the drying temperature is 80-100 ℃, and the drying time is 20-30 h;
(6) adding aluminum salt into the obtained clear solution to obtain a mixed salt solution, dropwise adding a sodium hydroxide solution into the clear solution, adjusting the pH value to 10-11, carrying out coprecipitation reaction, heating, stirring, aging, and carrying out suction filtration to obtain white filter residues and a transparent solution; mg in clear solution 2+ 、Ca 2 + The molar ratio of (1-3) to 1; the molar ratio of the aluminum ions to the divalent metal ions is 1: (1-4); the concentration of the sodium hydroxide solution is 0.3-0.5 mol/L; the temperature of the coprecipitation method is raised to 45-75 ℃, and the stirring reaction time is 0.5-1.5 h; the aging temperature is 90-110 ℃, the time is 15-30 h, and the pH of the transparent solution obtained by suction filtration is 7-8;
(7) drying the obtained white filter residue to obtain hydrotalcite; adding a dilute hydrochloric acid solution into the obtained transparent solution, adjusting the pH to 6-8, and drying to obtain sodium chloride; the concentration of the dilute hydrochloric acid solution is 0.1-2.5 mol/L; the drying temperature of the hydrotalcite is 60-120 ℃, and the drying time is 15-30 h.
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