CN112551922A - Comprehensive resource utilization method of phosphorus tailings waste residues and carbide slag - Google Patents
Comprehensive resource utilization method of phosphorus tailings waste residues and carbide slag Download PDFInfo
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- CN112551922A CN112551922A CN202011559872.3A CN202011559872A CN112551922A CN 112551922 A CN112551922 A CN 112551922A CN 202011559872 A CN202011559872 A CN 202011559872A CN 112551922 A CN112551922 A CN 112551922A
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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
- 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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- 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
- C04B7/24—Cements from oil shales, residues or waste other than slag
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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
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Abstract
The invention discloses a comprehensive resource utilization method of phosphorus tailings waste residues and carbide slag; calcining the phosphorus tailings to remove organic impurities, and grinding the calcined phosphorus tailings into powder; preparing an acid diluent, uniformly stirring, slowly adding calcined phosphorus tailings powder, heating and stirring until the powder is completely dissolved to obtain a tan emulsion; carrying out suction filtration and washing to obtain brown yellow acid leaching phosphorus tailing waste residues and light yellow filtrate; mixing the obtained acid-leaching phosphate tailing waste residue, carbide slag and bauxite in proportion, placing the mixture in a vibration mill, grinding the mixture until the fineness is less than or equal to 75 mu m, pressing and molding the mixture, calcining the mixture for 1 to 2 hours at 1150 to 1280 ℃, placing the mixture in liquid nitrogen for quick cooling, grinding the mixture again, and adding an additive to obtain the belite-sulphoaluminate cement. The obtained belite-sulphoaluminate cement has the compressive strength of 34.64MPa in 3 days, the flexural strength of 9.7MPa, the compressive strength of 48.7MPa in 28 days and the flexural strength of 10.1 MPa.
Description
Technical Field
The invention belongs to the technical field of building engineering materials, and particularly relates to a comprehensive resource utilization method of phosphorus tailings and carbide slag.
Background
The belite-sulphoaluminate cement is novel low-carbon cement, overcomes the problems of poor early strength, erosion resistance and the like of the traditional portland cement in performance, and also overcomes the problems of expansibility, strength reverse shrinkage and the like of the sulphoaluminate cement. The mineral composition of the belite-sulphoaluminate cement is calcium sulphoaluminate (3 CaO.3Al)2O3·CaSO4，C4A3S), dicalcium silicate (2 CaO. SiO)2，C2S), calcium sulfosilicate (2 CaO. SiO)2·CaSO4，C5S2S) and tetracalcium aluminoferrite (4 CaO. Al)2O3·Fe2O3，C4AF) is dominant. The calcination process of the belite-sulphoaluminate cement is lower than that of common Portland cement (generally at 1450 ℃), the clinker has good grindability and lower energy consumption. Therefore, the belite-sulphoaluminate cement has wide application prospect and is highly valued by material workers in various countries in the world.
The phosphorus tailings are products containing more phosphorus and lower impurity minerals in the flotation enrichment process of high-grade phosphorite and medium-low-grade collophanite, the existing treatment technology of the phosphorus tailings is not mature, and open-air piles are actively easy to cause environmental pollution and resource waste, so that the problem of resource recycling of the phosphorus tailings is urgently needed to be solved. The carbide slag is the waste slag generated after acetylene is obtained by hydrolyzing carbide and contains rich Ca (OH)2。
Disclosure of Invention
The invention aims to provide a comprehensive resource utilization method by combining the characteristics of the phosphorus tailings waste residue and the carbide slag, and solves the problems of low utilization rate, environment damage and the like of the acid-leaching phosphorus tailings waste residue and the carbide slag.
In order to achieve the purpose, the technical scheme is as follows:
the comprehensive resource utilization method of the phosphorus tailings waste residue and the carbide slag comprises the following steps:
(1) calcining the phosphorus tailings to remove organic impurities, and grinding the calcined phosphorus tailings into powder;
(2) preparing an acid diluent, uniformly stirring, slowly adding calcined phosphorus tailings powder, heating and stirring until the powder is completely dissolved to obtain a tan emulsion; carrying out suction filtration and washing to obtain brown yellow acid leaching phosphorus tailing waste residues and light yellow filtrate;
(3) mixing the obtained acid-leaching phosphate tailing waste residue, carbide slag and bauxite in proportion, placing the mixture in a vibration mill, grinding the mixture until the fineness is less than or equal to 75 mu m, pressing and molding the mixture, calcining the mixture for 1 to 2 hours at 1150 to 1280 ℃, placing the mixture in liquid nitrogen for quick cooling, grinding the mixture again, and adding an additive to obtain the belite-sulphoaluminate cement.
According to the scheme, the calcining temperature and the calcining time in the step 1) are respectively 500-800 ℃ and 0.5-2 h; the fineness of the powder reaches 200-300 meshes.
According to the scheme, the concentration of the acid diluent in the step 2) is 1-10 mol/L; the acid is one or mixture of hydrochloric acid, sulfuric acid, nitric acid and organic phosphonic acid.
According to the scheme, the temperature is raised and the stirring temperature is 50-80 ℃ in the step 2), and the time is 0.5-2 h.
According to the scheme, the light yellow filtrate obtained in the step 2) is further used for preparing a flame retardant or hydrotalcite.
According to the scheme, the acid-leaching phosphorus tailings waste residue, the carbide slag and the bauxite in the step 3) are as follows according to the mass percentage:
15-40 wt% of acid-leaching phosphorus tailing waste residues, 30-60 wt% of carbide slag and 10-30 wt% of bauxite.
According to the scheme, the additive in the step 3) is one or more of dihydrate gypsum, hemihydrate gypsum, phosphogypsum and anhydrite, and the addition amount of the additive is 5-20 wt%.
The mineral composition of the phosphate tailings comprises CaCO3、CaSO4、MgCO3、SiO2Etc., CaCO therein3、CaSO4、SiO2The mineral is suitable for preparing belite-sulphoaluminate cement, and CaCO is used simultaneously3、MgCO3Is suitable for synthesizing calcium magnesium aluminum layered hydroxide. According to the invention, a large amount of Mg ions and part of Ca ions in the phosphate tailings after acid leaching treatment are dissolved, the filtrate is partially suitable for synthesizing calcium-magnesium-aluminum layered hydroxide, and the residual filter residue has high-purity CaSO4、SiO2The method is very suitable for preparing the belite-sulphoaluminate cement, and the phosphate tailings are effectively recycled.
The carbide slag is the waste slag generated after acetylene is obtained by hydrolyzing carbide and contains rich Ca (OH)2The calcium raw material used as cement not only reduces the utilization of limestone natural resources, but also reduces CO2The natural environment is greatly protected, and the environmental pollution caused by the accumulation of the carbide slag is reduced.
The phosphorus tailings and the carbide slag are used as industrial waste slag, and the open stacking is a waste of resources and damages the environment, so that a reasonable disposal mode is urgently needed to solve the problem of the random stacking of the industrial waste slag. In order to carry out the maximum resource utilization of the components of the phosphate tailings, the calcium magnesium aluminum layered hydroxide is produced, and the carbide slag is used as a calcium raw material supplement, so that the problem of random stacking of the phosphate tailings and the carbide slag can be solved, and the belite-sulphoaluminate cement with high grade and high quality is produced, and has a very wide application prospect.
Compared with the prior art, the invention has the beneficial effects that:
the belite-sulphoaluminate cement is prepared by using the acid-leaching phosphate tailing waste residues and the carbide slag as main raw materials, various chemical components in the acid-leaching phosphate tailing waste residues and the carbide slag can be fully and efficiently utilized, the serious dependence of sulphoaluminate cement (belite-sulphoaluminate cement) production on natural gypsum and limestone is overcome, the preparation process is simple, the utilization rate of the raw materials is high, and the prepared sulphoaluminate cement has high compressive strength and rupture strength, is environment-friendly and has better environmental benefit and economic benefit.
The prepared belite-sulphoaluminate cement has the compressive strength of 34.64MPa after 3 days, the flexural strength of 9.7MPa, the compressive strength of 48.7MPa after 28 days and the flexural strength of 10.1MPa after strength tests.
Drawings
FIG. 1: the X-ray diffraction pattern of the acid-leached phosphorus tailings waste residue obtained in example 1.
FIG. 2: the X-ray diffraction pattern of the cement clinker 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 company Limited in Ezhou, Hubei province, as CaCO3、CaSO4、MgCO3、SiO2The contents are respectively 20% -40%, 15% -25%, 25% -35% and 5% -10%.
Example 1:
1) weighing 50g of phosphorus tailings, placing the phosphorus tailings in a muffle furnace, calcining the phosphorus tailings for 1.5 hours at 700 ℃, removing organic impurities, and grinding the phosphorus tailings to obtain 200-300 meshes of powder fineness;
2) mixing 100ml of hydrochloric acid with the content of 36-38% and purified water with the same volume, adding the mixture into a stirring reactor, stirring, heating to 60 ℃, slowly adding the phosphorus tailing powder subjected to impurity removal in the step 1), stirring, and carrying out acidolysis reaction for 2.5 hours to obtain a tan emulsion; carrying out suction filtration, washing and drying to obtain acid-leaching phosphorus tailings waste residues, wherein an X-ray diffraction spectrum of the acid-leaching phosphorus tailings waste residues is shown in figure 1; the filtrate obtained by suction filtration is used for preparing a flame retardant or hydrotalcite;
3) mixing the obtained acid-leaching phosphate tailing waste residue, carbide slag and bauxite according to the mass percent of 35 wt%, 50 wt% and 15 wt%; grinding in a vibration mill until the fineness is below 75 μm;
4) pressing and molding the powder, placing the powder in a muffle furnace, calcining at 1200 ℃ for 1.5 hours to obtain calcined clinker, and placing the calcined clinker in liquid nitrogen for extremely cooling to obtain cement clinker, wherein an X-ray diffraction spectrum of the cement clinker is shown in figure 2;
5) and placing the cement clinker and the anhydrite in a vibration mill according to the ratio of 5:1, and grinding the mixture into powder with the fineness of less than 200mm to finally obtain the belite-sulphoaluminate cement.
Example 2:
1) weighing 50g of phosphorus tailings, placing the phosphorus tailings in a muffle furnace, calcining the phosphorus tailings for 2 hours at 500 ℃, removing organic impurities, and grinding the phosphorus tailings to obtain 200-300 meshes of powder fineness;
2) mixing 120ml of 65 percent nitric acid and twice the volume of purified water, 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, and performing acidolysis reaction for 2 hours to obtain a tan emulsion; carrying out suction filtration, washing and drying to obtain acid leaching phosphorus tailing waste residues; the filtrate obtained by suction filtration is used for preparing a flame retardant or hydrotalcite;
3) mixing 30 wt%, 50 wt% and 20 wt% of acid-leaching phosphorus tailings waste residue, carbide slag and bauxite; grinding in a vibration mill until the fineness is below 75 μm;
4) pressing and molding the powder, placing the powder in a muffle furnace, calcining at 1150 ℃ for 2 hours to obtain calcined clinker, and placing the calcined clinker in liquid nitrogen for extremely cooling to obtain cement clinker;
5) placing the cement clinker and the dihydrate gypsum in a vibration mill according to the mass ratio of 17:3, and grinding the mixture to powder with the fineness of less than 200mm to finally obtain the belite-sulphoaluminate cement.
Example 3:
1) weighing 50g of phosphorus tailings, placing the phosphorus tailings in a muffle furnace, calcining the phosphorus tailings for 1 hour at 800 ℃, removing organic impurities, and grinding the phosphorus tailings to obtain 200-300 meshes of powder fineness;
2) mixing 120ml of 98% sulfuric acid and three times of pure water by 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, and performing acidolysis reaction for 1.5 hours to obtain a tan emulsion; carrying out suction filtration, washing and drying to obtain acid leaching phosphorus tailing waste residues; the filtrate obtained by suction filtration is used for preparing a flame retardant or hydrotalcite;
3) mixing the acid-leaching phosphorus tailings waste residue, the carbide slag and the bauxite according to the mass ratio of 0.4:0.5: 0.1; grinding in a vibration mill until the fineness is below 75 μm;
4) pressing and molding the powder, placing the powder in a muffle furnace, calcining at 1280 ℃ for 1 hour to obtain calcined clinker, and placing the calcined clinker in liquid nitrogen for extremely cold to obtain cement clinker;
5) placing the cement clinker and the dihydrate gypsum in a vibration mill according to the ratio of 20:1, and grinding the mixture into powder with the fineness of less than 200mm to finally obtain the belite-sulphoaluminate cement.
The setting time and the strength related to the embodiment are respectively carried out according to a monitoring method for water consumption, setting time and stability of standard consistency of cement (GB/T1346) and a detection method for strength of cement mortar (GB/T17671-1999).
The belite-sulphoaluminate cement obtained in example 1 had an initial setting time of 20min, a final setting time of 31min, a compressive strength of 29.4Mpa at 1 day, a flexural strength of 5.7Mpa, a compressive strength of 34.1Mpa at 3 days, a flexural strength of 8.2Mpa, a compressive strength of 39.3Mpa at 28 days and a flexural strength of 8.4 Mpa.
The belite-sulphoaluminate cement obtained in example 2 has an initial setting time of 25min, a final setting time of 35min, a compressive strength of 26.2Mpa in 1 day, a compressive strength of 4.6Mpa in 3 days, a compressive strength of 32.1Mpa in 3 days, a compressive strength of 6.5Mpa in 28 days, a compressive strength of 35.3Mpa in 28 days and a compressive strength of 7.7Mpa in 3 days.
The belite-sulphoaluminate cement obtained in example 3 had an initial setting time of 20min, a final setting time of 28min, a 1-day compressive strength of 31.2Mpa, a flexural strength of 5.6Mpa, a 3-day compressive strength of 41.3Mpa, a flexural strength of 7.5Mpa, a 28-day compressive strength of 48.7Mpa and a flexural strength of 10.1 Mpa.
Claims (7)
1. The comprehensive resource utilization method of the phosphorus tailings waste residue and the carbide slag is characterized by comprising the following steps of:
(1) calcining the phosphorus tailings to remove organic impurities, and grinding the calcined phosphorus tailings into powder;
(2) preparing an acid diluent, uniformly stirring, slowly adding calcined phosphorus tailings powder, heating and stirring until the powder is completely dissolved to obtain a tan emulsion; carrying out suction filtration and washing to obtain brown yellow acid leaching phosphorus tailing waste residues and light yellow filtrate;
(3) mixing the obtained acid-leaching phosphate tailing waste residue, carbide slag and bauxite in proportion, placing the mixture in a vibration mill, grinding the mixture until the fineness is less than or equal to 75 mu m, pressing and molding the mixture, calcining the mixture for 1 to 2 hours at 1150 to 1280 ℃, placing the mixture in liquid nitrogen for quick cooling, grinding the mixture again, and adding an additive to obtain the belite-sulphoaluminate cement.
2. The comprehensive resource utilization method of the phosphorus tailings and the carbide slag as claimed in claim 1, wherein the calcination temperature and the calcination time in the step 1) are 500 to 800 ℃ and 0.5 to 2 hours respectively; the fineness of the powder reaches 200-300 meshes.
3. The comprehensive resource utilization method of the phosphorus tailings and the carbide slag as claimed in claim 1, wherein the concentration of the acid diluent in the step 2) is 1mol/L to 10 mol/L; the acid is one or mixture of hydrochloric acid, sulfuric acid, nitric acid and organic phosphonic acid.
4. The comprehensive resource utilization method of the phosphorus tailings and the carbide slag as claimed in claim 1, wherein the temperature of the step 2) is raised and the stirring temperature is 50 ℃ to 80 ℃ for 0.5h to 2 h.
5. The comprehensive resource utilization method of the phosphorus tailings and the carbide slag as claimed in claim 1, wherein the light yellow filtrate obtained in the step 2) is further used for preparing a flame retardant or hydrotalcite.
6. The comprehensive resource utilization method of the phosphorus tailing waste residue and the carbide slag according to claim 1, which is characterized in that the acid leaching of the phosphorus tailing waste residue, the carbide slag and the bauxite in the step 3) comprises the following components in percentage by mass:
15-40 wt% of acid-leaching phosphorus tailing waste residues, 30-60 wt% of carbide slag and 10-30 wt% of bauxite.
7. The comprehensive resource utilization method of the phosphorus tailing slag and the carbide slag according to claim 1, wherein the additive in the step 3) is one or more of dihydrate gypsum, hemihydrate gypsum, phosphogypsum and anhydrite, and the addition amount of the additive is 5-20 wt%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113307517A (en) * | 2021-06-18 | 2021-08-27 | 登电集团水泥有限公司 | Quick-setting curing material and preparation method thereof |
| CN114292041A (en) * | 2021-11-11 | 2022-04-08 | 上海胜义环境科技有限公司 | Preparation method of cementing material based on phosphorus tailings |
| CN114988443A (en) * | 2022-06-02 | 2022-09-02 | 中南大学 | Method for recovering aluminum oxide from aluminum-rich slag |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113307517A (en) * | 2021-06-18 | 2021-08-27 | 登电集团水泥有限公司 | Quick-setting curing material and preparation method thereof |
| CN114292041A (en) * | 2021-11-11 | 2022-04-08 | 上海胜义环境科技有限公司 | Preparation method of cementing material based on phosphorus tailings |
| CN114988443A (en) * | 2022-06-02 | 2022-09-02 | 中南大学 | Method for recovering aluminum oxide from aluminum-rich slag |
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Application publication date: 20210326 |