CN111250034B - Modification method and application of desulfurization slag - Google Patents

Modification method and application of desulfurization slag Download PDF

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CN111250034B
CN111250034B CN202010211640.2A CN202010211640A CN111250034B CN 111250034 B CN111250034 B CN 111250034B CN 202010211640 A CN202010211640 A CN 202010211640A CN 111250034 B CN111250034 B CN 111250034B
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desulfurization slag
powder
filtering
precipitate
desulfurization
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CN111250034A (en
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杨志彬
康婷
苏童
张旗芹
冯浩
贾文锐
吴晨
姚柳
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Jiangsu University of Science and Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041—Oxides or hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00—Obtaining rare earth metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • 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
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

A modification method of desulfurization slag comprises the following steps: crushing molten iron desulfurization slag, removing iron and oxides by magnetic separation, and ball-milling to obtain desulfurization slag powder; dissolving the powder with sodium hydroxide at 80-100deg.C, filtering, dissolving the precipitate with concentrated hydrochloric acid or with SiO 2 Mixing the powder, dissolving the powder by adopting concentrated hydrochloric acid, filtering the dissolved solution again, precipitating and separating the obtained filtrate by using sodium hydroxide solution, filtering to obtain a precipitate, drying the precipitate, calcining the dried precipitate at 900-1100 ℃ for 2-4 hours, and grinding the calcined precipitate into powder to obtain modified C desulfurization slag; when using SiO 2 Mixing the powder, calcining the mixed powder at 1000-1200 ℃ for 2-4 h, and grinding the mixed powder into powder to obtain the modified C2S desulfurization slag. The invention not only aims at rare earth Ce 3+ The ion adsorption rate exceeds 93 percent, and the method is simple, convenient and efficient, and simultaneously solves the problems of desulfurization slag and Ce in the pretreatment of molten iron 3+ And (3) recycling the ions.

Description

Modification method and application of desulfurization slag
Technical Field
The invention belongs to the technical field of metallurgical resource recycling, and particularly relates to a modification method and application of desulfurization slag.
Background
Rare earth is an important strategic resource of world attention, and is widely applied to the scientific and technological fields of new energy sources, new materials, energy conservation and environmental protection, aerospace, electronic information and the like because of unique physical and chemical properties, is an indispensable important element in modern industry, and is known as industrial gold. The rare earth reserves in China are first, but the rare earth reserves in China are sharply reduced along with the increase of the rare earth demand and the long-term influence of factors such as rare earth resource predation exploitation. China has now strengthened protection of rare earth resources and the environment, so that rare earth exploitation and supply are drastically reduced. Under the large background of resource shortage, great improvement of cost and continuous development of technology, the rare earth recycling industry is gradually paid attention to. However, recovery of rare earth ions from raw material waste, industrial production residues and end products containing rare earth elements that are eliminated is an important approach to alleviate the contradiction between rare earth resource supply and demand in China.
Recovery of Ce 3+ The method for preparing rare earth metal ions such as ions mainly comprises a chemical precipitation method, an extraction method, an ion exchange method, a membrane separation method, an adsorption method and the like. The adsorption method has the characteristics of good separation effect, simple operation, no need of additional auxiliary conditions, low energy consumption, classification enrichment and the like, and is considered as one of the most feasible methods for recovering and separating low-concentration metal ions. In the past decade, work done to treat or recover low concentration metal ions by adsorption has been mainly around the adsorption of metal ions by adsorbents such as natural minerals, oxides, synthetic materials and microorganisms and their use.
Although Ce is 3+ The ion and other novel rare earth ion adsorbent materials have advanced to a certain extent in terms of improving the maximum adsorption capacity and desorption rate, but still have a plurality of scientific and technical problems in terms of production cost, serious degradation of adsorption capacity after regeneration, lower service life and stability and the like, thereby limiting the industrialized large-scale use of the rare earth ion adsorbent materials.
In addition, iron and steel enterprises in China can produce about 200 ten thousand tons of desulfurization slag each year, the existing desulfurization slag treatment process generally comprises the steps of firstly magnetically separating and recycling iron, and the tailings and the steel slag are treated together, so that the resource utilization rate is very low. The accumulation of a large amount of desulfurization slag not only causes resource waste and occupies a large amount of land, but also causes secondary pollution to the surrounding environment due to harmful elements in the desulfurization slag. Therefore, it is urgent to find an efficient and high-valued desulfurization slag recycling method.
Disclosure of Invention
The invention aims to solve the problems and the defects of the prior art and provides a modification method and application of desulfurization slag.
The invention takes low-cost solid waste molten iron desulfurization slag as a raw material, and the low-cost solid waste molten iron desulfurization slag is firstly modified and then is adsorbed with rare earth Ce3+ ions, and the modified desulfurization slag has good adsorption and desorption performance on the rare earth Ce3+ ions.
The invention utilizes the modified desulfurization slag to adsorb rare earth ions, thereby not only solving the recycling problem of rare earth ions, but also greatly improving the comprehensive utilization of waste of iron and steel enterprises and embodying the novel environment treatment concept of treating waste with waste.
The desulfurization slag adopted by the invention is steel slag generated by molten iron pretreatment before converter steelmaking, namely molten iron desulfurization slag, and mainly contains CaO, caS and metal Fe, and also contains a small amount of Ca2SiO4, siO2, al2O3 and the like.
In order to achieve the above purpose, the present invention is realized by adopting the following technical scheme.
The modification method of the desulfurization slag comprises the following specific steps: crushing molten iron desulfurization slag, removing iron and oxides thereof by magnetic separation, and ball-milling to obtain desulfurization slag powder; dissolving the desulfurization slag powder with sodium hydroxide at 80-100deg.C, filtering, dissolving the precipitate with concentrated hydrochloric acid or mixing with SiO 2 Mixing the powder, dissolving the powder by adopting concentrated hydrochloric acid, filtering the dissolved solution again, precipitating and separating the obtained filtrate by using sodium hydroxide solution, filtering to obtain a precipitate, drying the precipitate, calcining the dried precipitate at 900-1100 ℃ for 2-4 hours, and grinding the calcined precipitate into powder to obtain modified C desulfurization slag; when using SiO 2 Mixing the powder, calcining the mixed powder at 1000-1200 ℃ for 2-4 hours, and grinding the mixed powder into powder to obtain modified C2S desulfurization slag; the desulfurization slag powder, sodium hydroxide and SiO 2 The mass ratio of the powder is 1:0.2-0.3:0.2-0.3.
Further preferably, the oxide components of the molten iron desulphurization slag are as follows: 45-55% of CaO and 30-40% of Fe 2 O 3 10 to 15 percent of SiO 2 The balance being other oxides.
Further preferably, the concentration of the sodium hydroxide solution is 4-6 mol/L; the mass ratio of the desulfurization slag powder to the sodium hydroxide is 1:0.2-0.3.
Further preferably, the particle size of the powder is 10 to 30. Mu.m.
The application method of the C desulfurization slag or the C2S desulfurization slag prepared by the modification method of the desulfurization slag is characterized by comprising the following specific steps of: adding the C desulfurization slag into Ce with the concentration of 50-200 mg/L according to the amount of 1.5-2.5 mg/mL 3+ Stirring for 10-120 min, and filtering with microporous membrane with pore size of 20-50 μm to remove solid; the application method of the C2S desulfurization slag comprises the following specific steps: adding the C2S desulfurization slag into Ce with the concentration of 100-200 mg/L according to the amount of 1-4 mg/mL 3+ Stirring for 1-3 h, and filtering with microporous membrane with pore diameter of 20-50 μm to remove solid.
The invention has the advantages and beneficial effects that:
the invention uses low-cost solid waste-molten iron desulfurization slag (steel slag produced by molten iron pretreatment before converter steelmaking mainly contains CaO and metal Fe, and also contains Fe 2 O 3 、SiO 2 And Al 2 O 3 Etc.) as raw materials, which are first modified and then the rare earth Ce in the solution 3+ As a result of ion adsorption, the modified desulfurization slag is found to be used for rare earth Ce 3+ The ion has good adsorptivity and desorption performance. The invention utilizes the modified desulfurization slag to adsorb rare earth ions, thereby not only solving the recycling problem of rare earth ions, but also greatly improving the comprehensive utilization of waste of iron and steel enterprises and embodying the novel environment treatment concept of treating waste with waste.
The method of the invention not only aims at rare earth Ce 3+ The ion adsorption effect is good (the adsorption rate exceeds 93%), and the adsorbent has simple preparation process and low cost. At the same time greatly improve the steel enterpriseThe industrial waste steel slag is comprehensively utilized, and the purposes of treating waste with waste and changing waste into valuable are realized.
Drawings
FIG. 1 is a diagram showing the appearance of molten iron desulphurization slag of a steel enterprise in Jiangsu province used in example 1;
FIG. 2 is a diagram showing Ca (OH) obtained after modification of the desulfurization slag used in example 2 2 X-ray diffraction pattern (XRD);
FIG. 3 is a Ca obtained after modification of the desulfurization slag used in example 3 2 SiO 4 X-ray diffraction pattern (XRD);
FIG. 4 is an X-ray diffraction (XRD) pattern of the desorbed product of the modified desulfurization slag used in example 4.
Detailed Description
Example 1
The desulfurization slag used in the invention is from a certain iron and steel enterprise in Jiangsu, and the morphology of the desulfurization slag is shown in figure 1; x-ray fluorescence analysis was conducted to find the oxide composition of the desulfurization slag as shown in Table 1 below.
TABLE 1 main oxide composition of desulphurized slag of converter
The desulfurization slag is crushed, then iron and oxides thereof are removed by magnetic separation, and finally the desulfurization slag powder with the particle size of about 20 mu m is obtained by ball milling.
EXAMPLE 2 modification of desulphurized slag to C desulphurized slag and application to Ce 3+ Adsorption of (3)
100g of the desulfurization residue powder obtained in example 1 was dissolved with 20g of sodium hydroxide (reaction temperature 90 ℃ C.) for 2 hours, and then filtered, the obtained precipitate was dissolved with 70ml of concentrated hydrochloric acid, and then filtered, and the obtained filtrate was separated by precipitation with 200ml of 5mol/L sodium hydroxide solution, and the obtained precipitate was Ca (OH) after filtration 2 As shown in FIG. 2, caO is obtained by drying and calcining (1000 ℃ C., 2 h), and then ground into powder of about 20 μm, namely, C desulfurization slag.
Preparing cerium nitrate into 2g/L Ce by deionized water 3+ Standard solution, then diluting the standard solution into Ce with different solubilities 3+ A solution.
0.1g of C desulfurization slag is weighed and added into 50mL of Ce with the concentration of 200mg/L 3+ The solution was stirred at constant temperature 25℃for 2h. Then filtering with microporous membrane (pore size of 50 μm) to remove solid, and detecting and analyzing Ce with ultraviolet-visible spectrophotometer 3+ The concentration was calculated to give an adsorption rate of 95.1%.
0.1g of C desulfurization slag is weighed and added into 50mL of Ce with the concentration of 100mg/L 3+ The solution was stirred at constant temperature of 25℃for 10 minutes. Then filtering with microporous membrane (pore size of 50 μm) to remove solid, and detecting and analyzing Ce with ultraviolet-visible spectrophotometer 3+ The concentration was calculated to give an adsorption rate of 95.2%.
0.1g of C desulfurization slag is weighed and added into 50mL of Ce with the concentration of 50mg/L 3+ The solution was stirred at constant temperature 25℃for 2h. The solids were then removed by filtration through a microporous membrane (pore size 50 μm) and the resulting supernatant was analyzed for detection. Ce (Ce) 3+ The concentration was measured by an ultraviolet-visible spectrophotometer, and the calculated adsorption rate was 94.3%.
EXAMPLE 3 modification of desulphurized slag to C2S desulphurized slag and application to Ce 3+ Adsorption of (3)
100g of the desulfurization residue powder obtained in example 1 was dissolved with 20g of sodium hydroxide (reaction temperature: 90 ℃ C.) for 2 hours, and then filtered, and 25g of SiO was added to the obtained precipitate 2 Mixing the powder, and calcining at 1100 ℃ for 2 hours to obtain Ca 2 SiO 4 (the phase composition is shown in figure 3), and grinding into powder of about 20 μm, namely the C2S desulfurization slag.
Preparing cerium nitrate into 2g/L Ce by deionized water 3+ Standard solution, then diluting the standard solution into Ce with different solubilities 3+ A solution.
0.05g of C2S desulfurization slag is weighed and added into 50mL of Ce with the concentration of 150mg/L 3+ The solution was stirred at constant temperature 25℃for 2h. Then filtering with microporous membrane (pore size of 50 μm) to remove solid, and detecting and analyzing Ce with ultraviolet-visible spectrophotometer 3+ The concentration was calculated to give an adsorption rate of 93.8%.
0.15g of C2S desulfurization slag is weighedAdding the mixture into 50mL of Ce with the concentration of 150mg/L 3+ The solution was stirred at constant temperature 25℃for 2h. Then filtering with microporous membrane (pore size of 50 μm) to remove solid, and detecting and analyzing Ce with ultraviolet-visible spectrophotometer 3+ The concentration was calculated to give an adsorption rate of 95.6%.
0.20g of C2S desulfurization slag is weighed and added into 50mL of Ce with the concentration of 150mg/L 3+ The solution was stirred at constant temperature 25℃for 2h. Then filtering with microporous membrane (pore size of 50 μm) to remove solid, and detecting and analyzing Ce with ultraviolet-visible spectrophotometer 3+ The concentration was calculated to give an adsorption rate of 96.0%.
EXAMPLE 4 adsorption of Ce by C2S desulfurization slag 3+ Post desorption
Ce was adsorbed in example 3 above 3+ Separating the C2S desulfurization slag from the white jelly coated on the surface of the desulfurization slag after the ion solution, enabling the separated white jelly to be easily changed into a purple jelly under the air atmosphere condition, drying and calcining (1100 ℃ for 2 h) the purple jelly to finally obtain a red solid substance, and carrying out XRD phase analysis on the red solid substance to obtain a result shown in figure 4. As can be seen from FIG. 4, the red color material mainly consists of ceria and ceria phases, illustrating that the C2S desulfurization slag adsorbs Ce 3+ And then is easy to desorb.
Example 5 Effect of different reaction temperatures on the adsorption Properties of two desulphurized slag
Table 2 shows the effect of different reaction temperatures on the adsorption performance of two modified desulphurized residues. From Table 2, it is understood that the reaction temperature has little effect on the adsorption performance of the two modified desulfurization residues in the range of examined reaction temperature (30 to 70 ℃ C.).
TABLE 2 reaction temperature Ce is adsorbed on two modified desulphurized residues 3+ Influence of Performance
The foregoing description is directed to the preferred embodiments of the present invention, but the scope of the present invention is not limited to the above, and all equivalent changes or modifications made under the technical spirit of the present invention shall be construed to fall within the scope of the present invention.

Claims (4)

1. The modification method of the desulfurization slag is characterized by comprising the following steps: crushing molten iron desulfurization slag, removing iron and oxides thereof by magnetic separation, and ball-milling to obtain desulfurization slag powder; dissolving the desulfurization slag powder with sodium hydroxide at 80-100deg.C, filtering, dissolving the precipitate with concentrated hydrochloric acid or mixing with SiO 2 Mixing the powder, dissolving the powder by adopting concentrated hydrochloric acid, filtering the dissolved solution again, precipitating and separating the obtained filtrate by using sodium hydroxide solution, filtering to obtain a precipitate, drying the precipitate, calcining the dried precipitate at 900-1100 ℃ for 2-4 hours, and grinding the calcined precipitate into powder to obtain modified C desulfurization slag; when using SiO 2 Mixing the powder, calcining the mixed powder at 1000-1200 ℃ for 2-4 hours, and grinding the mixed powder into powder to obtain modified C2S desulfurization slag; the desulfurization slag powder, sodium hydroxide and SiO 2 The mass ratio of the powder is 1:0.2-0.3:0.2-0.3;
the oxide components of the molten iron desulfurization slag are as follows: 45-55% of CaO and 30-40% of Fe 2 O 3 10 to 15 percent of SiO 2 The balance being other oxides;
the application method of the modified C desulfurization slag comprises the following specific steps: adding the C desulfurization slag into Ce with the concentration of 50-200 mg/L according to the amount of 1.5-2.5 mg/mL 3+ Stirring for 10-120 min, and filtering with microporous membrane with pore size of 20-50 μm to remove solid;
the application method of the modified C2S desulfurization slag comprises the following specific steps: adding the C2S desulfurization slag into Ce with the concentration of 100-200 mg/L according to the amount of 1-4 mg/mL 3+ Stirring for 1-3 h, and filtering with microporous membrane with pore diameter of 20-50 μm to remove solid.
2. The method for modifying desulfurization residues according to claim 1, wherein the concentration of the sodium hydroxide solution is 4 to 6mol/L.
3. The method for modifying desulfurization slag according to claim 1, wherein the powder has a particle diameter of 10 to 30. Mu.m.
4. A method for applying the C desulfurization slag or the C2S desulfurization slag prepared by the modification method of the desulfurization slag according to any one of claims 1 to 3, characterized in that the specific steps of the modified C desulfurization slag application method are as follows: adding the C desulfurization slag into Ce with the concentration of 50-200 mg/L according to the amount of 1.5-2.5 mg/mL 3+ Stirring for 10-120 min, and filtering with microporous membrane with pore size of 20-50 μm to remove solid; the application method of the modified C2S desulfurization slag comprises the following specific steps: adding the C2S desulfurization slag into Ce with the concentration of 100-200 mg/L according to the amount of 1-4 mg/mL 3+ Stirring for 1-3 h, and filtering with microporous membrane with pore diameter of 20-50 μm to remove solid.
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