CN113231007A - Method for preparing heavy metal adsorbent by using blast furnace slag and application - Google Patents
Method for preparing heavy metal adsorbent by using blast furnace slag and application Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
A method for preparing heavy metal adsorbent by using blast furnace slag and application thereof, the method comprises the steps of soaking the blast furnace slag in water, filtering, drying and grinding; reacting the ground product with alkali liquor, performing suction filtration, reserving filtrate and recording the filtrate as solution 1, and recording filter residue as solid 1; adjusting the pH value of the solution 1, carrying out suction filtration, and marking the filtrate as a solution 2; adding filter residue into alkali liquor 2, and reacting to obtain a clear solution 3; ultrasonically dispersing the solid 1 in water to obtain a suspension 1, adding the solution 3 into the suspension 1, ultrasonically dispersing to obtain a suspension 2, adding the solution 2, and finally centrifugally separating to obtain the adsorbent. The invention separates aluminum ions and silicate ions from the blast furnace slag, then mixes the aluminum ions and the silicate ions with the treated blast furnace slag framework, and prepares the adsorbent which has a fluffy and granular framework and is provided with a layer of raised and wrinkled aluminosilicate rough gel on the surface of the framework by controlling the dosage of the aluminum ions, the silicate ions and the curing conditions, and the adsorbent has large specific surface area and good adsorption rate on heavy metals.
Description
Technical Field
The invention belongs to the technical field of heavy metal sewage treatment, and particularly relates to a method for preparing a heavy metal adsorbent by using blast furnace slag and application thereof.
Background
According to incomplete statistics, 350kg of blast furnace slag is discharged every 1t of iron is produced in the process of blast furnace iron making, the utilization rate is only 70-85%, and the recovery rate of the blast furnace slag in China is still at a lower level compared with that in developed countries. In order to improve the resource recycling rate of the blast furnace slag, researchers have conducted intensive research on the blast furnace slag, and the blast furnace slag is often applied to the fields of machinery, buildings, electronics and the like according to the diversification of chemical components and chemical properties. At present, blast furnace slag is used for preparing production and living materials such as cement, concrete, waste materials, gypsum, glass and the like, but the method is single, the added value is low, and a high-value utilization technology of the blast furnace slag still needs to be developed.
Heavy metal pollution is a common kind of wastewater pollution, and after being ingested by a human body, heavy metals can cause various diseases such as kidney and liver damage, so that heavy metal pollution is one of the main problems facing the current society. The main methods for removing the heavy metal ions in the water body at the present stage comprise ion exchange, membrane filtration, chemical precipitation, adsorption, electrolytic method, advanced oxidation, reverse osmosis and the like. The adsorption method is a method for removing impurities in wastewater by using a solid adsorbent, and has the advantages of high reaction process speed, high adsorption efficiency, convenient and simple operation facilities and the like, so that more and more people use the method to remove heavy metal impurities in wastewater.
In recent years, the technology of the present invention has been developedIn the treatment of heavy metal wastewater, solid adsorbents which are frequently applied include activated carbon, agricultural solid wastes, industrial solid wastes, natural adsorbents and the like. Wherein the industrial solid waste is one direction of hot spots of heavy metal wastewater adsorbents, and the published prior art has patent CN200710175228.4 which discloses a water treatment agent prepared by using blast furnace slag and a preparation method thereof, wherein the blast furnace slag comprises: SiO 22：25-30％，CaO：40-45％，Al2O3: 15-20%, MgO: 10-20%, and (CaO + MgO)/(Al)2O3+SiO2) Is 1.08-1.5. Mixing it with pH>11, mixing the alkaline aqueous solution according to the solid-liquid ratio of 1-51, filtering, drying at 50-120 ℃ for 24-48h, taking out, crushing, and finally sieving by a standard sieve of 6-80 m. Patent CN201811406908.7 discloses a modified blast furnace slag and its application, the modified blast furnace slag is prepared by the following steps: ball-milling and screening blast furnace slag, adding the blast furnace slag into an acid solution according to a solid-to-liquid ratio of 0.05-0.15: 1, oscillating, filtering, centrifuging and drying to obtain modified blast furnace slag; it is applied to the adsorption of metal ions in rare earth solution. Although the preparation method of the technical adsorbent is simple and low in cost, the application effect is slightly poor, particularly the adsorption rate of heavy metal ions is low, and the metal ions cannot be effectively recovered and reused, so that the preparation method of the blast furnace slag adsorbent needs to be further improved to improve the adsorption rate of the heavy metal ions, so that the metal ions can be effectively recovered and reused, and the resource utilization of the blast furnace slag can be maximized.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for preparing a heavy metal adsorbent by using blast furnace slag, the blast furnace slag treated by the method has a fluffy and granular framework, a layer of raised and wrinkled aluminosilicate rough gel covers the surface of the framework, and the adsorbent with the structure has a large specific surface area and a good adsorption rate on heavy metals.
In order to achieve the purpose, the invention adopts the following specific technical scheme:
a method for preparing a heavy metal adsorbent by using blast furnace slag comprises the following steps:
s1: soaking blast furnace slag in water, filtering, drying, taking out, putting into a ball mill, and grinding for later use;
s2: mixing the ground product obtained in the step S1 with alkali liquor 1, heating, raising the temperature, keeping constant temperature, stirring for reaction, cooling, performing suction filtration, keeping the filtrate as solution 1, washing the filter residue with water to constant weight, and drying for later use as solid 1;
s3: adding acid liquor into the solution 1 to adjust the pH value, then carrying out suction filtration, and keeping the filtrate as a solution 2 for later use; washing the filter residue with water, gradually adding alkali liquor 2, adjusting pH, and performing ultrasonic treatment to obtain clear solution 3 for use.
S4: adding the solid 1 into water, performing primary ultrasonic dispersion to obtain a suspension 1, adding the solution 3 into the suspension 1, uniformly mixing, performing secondary ultrasonic dispersion to obtain a suspension 2, continuously adding the solution 2 into the suspension 2, finally heating and maintaining constant temperature for solidification, performing centrifugal separation, and drying precipitates to obtain the heavy metal adsorbent.
Step S1, the weight ratio of the blast furnace slag to the water is 1:1.2-2.0, the soaking time is 10-20min, and soluble substances in the blast furnace slag can be removed in the step; the grinding is carried out until the particle size is 50-200 meshes, preferably 100-180 meshes.
The lye 1 used in the step S2 is not particularly limited, and may be those commonly used in the art, including but not limited to at least one of sodium hydroxide solution or potassium hydroxide solution, wherein the concentration of the lye 1 is 5-10mol/L, and the weight ratio of the lye 1 to the blast furnace slag is 3-6: 1; the heating temperature is increased to 40-80 ℃, the reaction time is 0.5-1.5h, and the cooling is performed to room temperature. The method comprises the step of dissolving amorphous substances such as silicon, aluminum, sodium silicate and sodium chlorate in the blast furnace slag by using alkali liquor to obtain a solution 1 containing silicon, aluminum and sodium and a blast furnace slag framework.
The acid solution in step S3 is not particularly limited, and is commonly used in the art, including but not limited to at least one of sulfuric acid or hydrochloric acid solution, the concentration of the acid solution is 2-4mol/L, the pH is adjusted to 7.5-8.5, the number of washing times is 1-3, the alkali solution 2 is not particularly limited, and is commonly used in the art, including but not limited to at least one of sodium hydroxide solution or potassium hydroxide solution, the concentration of the alkali solution 2 is 0.5-2mol/L, the weight ratio of the alkali solution 2 to the filter residue is 5-10:1, and the pH is adjusted to 8.5-10.5; the ultrasonic treatment power is 1-3kW, the ultrasonic treatment frequency is 60-80kHz, and the ultrasonic treatment time is 1-3 h. The pH value of the solution 1 is adjusted to be neutral or slightly alkaline, silicon and aluminum are separated, the silicon exists in silicic acid filter residue, and the aluminum exists in the solution 2 in the form of sodium aluminate; and adding the filter residue into the alkali liquor 2, controlling the pH value within the range of 8.5-10.5, and dissolving silicic acid to obtain a stable sodium silicate solution 3.
Step S4, the weight ratio of the solid 1 to the water is 1:3-6, preferably 1:4-5, the primary ultrasonic dispersion power is 0.5kW-1.5kW, the dispersion frequency is 40-60kHz, the dispersion time is 1-3h, the weight ratio of the suspension 1 to the solution 3 is 1:1-3, the secondary ultrasonic dispersion power is 0.5kW-1.5kW, the dispersion frequency is 60-80kHz, the dispersion time is 30-90min, the weight ratio of the suspension 2 to the solution 2 is 1:0.5-4, preferably 1:2-4, the temperature rise is 50-100 ℃, preferably 50-80 ℃, and the constant temperature curing time is 5-10 d. The blast furnace slag framework is dispersed into a uniform suspension 1, and a continuous special raised and wrinkled coarse aluminosilicate gel structure with a certain thickness is generated on the surface of the blast furnace slag framework by regulating and controlling the using amount of blast furnace slag particles in the suspension 1 and the mixing ratio of the blast furnace slag particles to the solution 2 and the solution 3, wherein the structure has large blast furnace slag specific surface area and good adsorption performance on heavy metals.
The invention also provides an application of the heavy metal adsorbent, the adsorbent and sewage with the concentration of the divalent heavy metal ions of 1.0-1.2g/L are uniformly mixed according to the proportion of (0.1-1) g to 100ml, the mixture is oscillated on an oscillator with the oscillation speed of 50-100r/min for 20-50min, and the adsorption rate of the divalent heavy metal ions in the sewage is more than or equal to 65%.
Compared with the prior art, the invention has the beneficial effects that:
the invention separates aluminum ions and silicate ions from the blast furnace slag, then mixes the aluminum ions and the silicate ions with the treated blast furnace slag framework, and prepares the adsorbent which has a fluffy and granular framework and a layer of raised and wrinkled aluminosilicate rough gel covered on the surface of the framework by controlling the dosage of the aluminum ions, the silicate ions and the silicate ions, and the adsorbent with the structure has large specific surface area and good adsorption rate on heavy metal ions.
The preparation method is safe and simple, does not need strict equipment and process conditions, has cheap raw materials and low cost, and is suitable for large-scale production.
Drawings
Fig. 1 is an SEM image of the heavy metal adsorbent prepared in preparation example 1 at 3000 times magnification.
Fig. 2 is an SEM image of the heavy metal adsorbent prepared in preparation example 1 at 1000 times magnification.
Fig. 3 is an EDS spectrum of the heavy metal adsorbent prepared in preparation example 1.
FIG. 4 is a process flow for preparing a heavy metal adsorbent according to the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the descriptions in the following. Unless otherwise specified, "parts" in the examples are parts by weight.
The blast furnace slag used in the examples of the present invention was obtained from Shanxi Huaxing aluminum industries, Inc. The main chemical composition content of the blast furnace slag was analyzed by X-ray fluorescence spectroscopy (instrument model: XRF-1800), and the results are shown in Table 1:
TABLE 1
Preparation example 1
S1: soaking 100 parts of blast furnace slag in 200 parts of water for 20 minutes, filtering, drying, taking out, putting into a ball mill, and grinding until the particle size is 120 meshes for later use;
s2: mixing the ground product obtained in the step S1 with a sodium hydroxide solution with the concentration of 10mol/L in a weight ratio of 1:6, mixing, heating to 60 ℃, then keeping constant temperature, stirring and reacting for 1.5h, finally cooling and carrying out suction filtration, keeping filtrate as solution 1, washing filter residue with water for 4 times until constant weight, and drying for later use as solid 1; the step is to separate aluminum and silicon from blast furnace slag by using alkali liquor.
S3: adding a hydrochloric acid solution with the concentration of 4mol/L into the solution 1 to adjust the pH value to 8, then carrying out suction filtration, and keeping the filtrate as a solution 2 for later use; washing the filter residue with water for 3 times, adding 1mol/L sodium hydroxide solution, adjusting pH to 10, and treating with 2kW power and 60kHz ultrasonic wave for 1.5h to obtain clear solution 3 for use.
S4: adding the solid 1 and water into water according to the weight ratio of 1:5, and performing primary ultrasonic dispersion, wherein the ultrasonic dispersion power is 1.2kW, the dispersion frequency is 50kHz, and the dispersion time is 2.0h to obtain a suspension 1; adding the solution 3 into the suspension 1 and the solution 3 in a weight ratio of 1:1, uniformly mixing, and then performing ultrasonic dispersion again, wherein the ultrasonic dispersion power is 1.5kW, the dispersion frequency is 60kHz, and the dispersion time is 60min to obtain a suspension 2; and continuously adding the solution 2 into the suspension 2 according to the weight ratio of the solution 2 to the suspension 2 being 1:2, finally heating to 80 ℃, keeping the constant temperature for solidification for 8 days, and performing centrifugal separation and precipitate drying to obtain the heavy metal adsorbent.
Fig. 1 is an SEM image of the heavy metal adsorbent prepared in preparation example 1 at 3000 times magnification. Fig. 2 is an SEM image of the heavy metal adsorbent prepared in preparation example 1 at 1000 times magnification. Fig. 3 is an EDS spectrum of the heavy metal adsorbent prepared in preparation example 1. Table 2 is the EDS spectrogram surface micro-area chemical composition analysis table
TABLE 2
Preparation example 2
The same as preparation example 1 except that suspension 1 was prepared at a weight ratio of solid 1 to water of 1:4 in step S4.
Preparation example 3
The same as preparation example 1 except that suspension 2 was prepared in a weight ratio of 1:3 of suspension 1 and solution 3 in step S4.
Preparation example 4
The same as in preparation example 1 except that the weight ratio of suspension 2 to solution 2 in step S4 was 1: 0.5.
Preparation example 5
The same as preparation example 1 except that suspension 1 was prepared at a weight ratio of solid 1 to water of 1:3 in step S4.
Preparation example 6
The same as preparation example 1 except that suspension 1 was prepared at a weight ratio of solid 1 to water of 1:6 in step S4.
Preparation example 7
The same as in preparation example 1 except that the weight ratio of suspension 2 to solution 2 in step S4 was 1: 4.
Preparation example 8
The same as in preparation example 1 except that the temperature was finally raised to 50 ℃ in step S4 and the temperature was maintained constant to cure for 8 d.
Preparation example 9
The same as in preparation example 1 except that the temperature was finally raised to 100 ℃ in step S4 and the temperature was maintained constant to cure for 8 d.
Examples 1 to 9
Adsorbing agent and Pb2+Mixing 1.0g/L sewage uniformly at a ratio of 1g:100ml, oscillating for 50min on an oscillator with oscillation speed of 80r/min, filtering to obtain adsorbed equilibrium solution, and measuring Pb in the equilibrium solution by ICP-AES method2+Concentration, and recovery was calculated. ICP-AES, equipment: ICP emission spectrometer SPS 1200AR model; atomic absorption spectrophotometer: AA 8200 type. Two-point standard curve methods of 0mg/L and 1.0mg/L are adopted for measurement.
In the formula: r is the recovery rate;
C0is Pb in solution2+Initial concentration (g/L);
Ceis Pb in solution2+Equilibrium concentration (g/L);
m is the mass (g) of the adsorbent;
v is the volume of the adsorption solution (L).
The adsorbents prepared in preparation examples 1 to 9 were subjected to the experimental tests in the examples in order, corresponding to examples 1 to 9, respectively.
Replacement of Pb-containing2+The sewage is Cu-containing sewage with the same concentration2+Sewage, Mn2+Sewage, Mn4+Sewage, Ni2+Sewage, Cd2+Sewage, Co3+The experimental tests in the above examples were repeated with the results shown in table 3 below.
TABLE 3
As can be seen from figures 1 and 2, the adsorbent prepared by the invention has a fluffy and granular framework, the surface of the framework is also covered with a layer of convex and wrinkled aluminosilicate rough gel adsorbent, and the adsorbent with the structure has large specific surface area and is very helpful for adsorbing heavy metal ions.
It can be seen from fig. 3 and 4 that the surfaces of fluffy and granular frameworks are tightly wrapped by the convex and wrinkled gel substances, and the element composition research of the gel substances in the red square boxes by EDS finds that the gel substances mainly comprise calcium silicoaluminate and sodium elements (carbon elements are caused by carbon spraying on the surfaces of samples during sample preparation), so that the gel is proved to be an aluminosilicate substance with a special structure.
As can be seen from the above table, the adsorbent of the present invention prepared from blast furnace slag has a good adsorption effect on heavy metals, particularly Pb2+、Cu2+、Mn2+、Ni2+、Cd2+The adsorption rate of the divalent heavy metal ions is all 80 percent, but the divalent heavy metal ions also have certain selectivity, particularly when the heavy metal ions are Mn4+、Co3+When the non-divalent heavy metal ions are used, the adsorption rate is only 78.77 percent at most.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (10)
1. A method for preparing a heavy metal adsorbent by using blast furnace slag comprises the following steps:
s1: soaking blast furnace slag in water, filtering, drying, taking out, putting into a ball mill, and grinding for later use;
s2: mixing the ground product obtained in the step S1 with alkali liquor 1, heating, raising the temperature, keeping constant temperature, stirring for reaction, cooling, performing suction filtration, keeping the filtrate as solution 1, washing the filter residue with water to constant weight, and drying for later use as solid 1;
s3: adding acid liquor into the solution 1 to adjust the pH value, then carrying out suction filtration, and keeping the filtrate as a solution 2 for later use; washing the filter residue with water, gradually adding alkali liquor 2, adjusting pH, and performing ultrasonic treatment to obtain a clear solution 3 for later use;
s4: adding the solid 1 into water, performing primary ultrasonic dispersion to obtain a suspension 1, adding the solution 3 into the suspension 1, uniformly mixing, performing secondary ultrasonic dispersion to obtain a suspension 2, continuously adding the solution 2 into the suspension 2, finally heating and maintaining constant temperature for solidification, performing centrifugal separation, and drying precipitates to obtain the heavy metal adsorbent.
2. The method according to claim 1, wherein the weight ratio of the blast furnace slag to the water in step S1 is 1:1.2-2.0, and the soaking time is 10-20 min.
3. The method according to claim 1, wherein the alkali solution 1 in step S2 is at least one selected from sodium hydroxide solution and potassium hydroxide solution, the concentration of the alkali solution 1 is 5-10mol/L, and the weight ratio of the alkali solution 1 to the blast furnace slag is 3-6: 1.
4. The method according to claim 1, wherein the heating in step S2 is carried out at a temperature of 40-80 ℃, the reaction time is 0.5-1.5h, and the cooling is carried out at room temperature.
5. The method according to claim 1, wherein the acid solution in step S3 is at least one selected from sulfuric acid and hydrochloric acid, the acid solution has a concentration of 2 to 4mol/L, the pH is adjusted to 7.5 to 8.5, and the number of washing is 1 to 3.
6. The preparation method according to claim 1, wherein the concentration of the lye 2 in step S3 is 0.5-2mol/L, the weight ratio of the lye 2 to the filter residue is 5-10:1, and the pH is adjusted to 8.5-10.5; the ultrasonic treatment power is 1-3kW, the ultrasonic treatment frequency is 60-80kHz, and the ultrasonic treatment time is 1-3 h.
7. The method according to claim 1, wherein the weight ratio of the solid 1 to the water in step S4 is 1:3 to 6, preferably 1:4 to 5, the primary ultrasonic dispersion power is 0.5kW to 1.5kW, the dispersion frequency is 40 kHz to 60kHz, and the dispersion time is 1 h to 3 h.
8. The method according to claim 1, wherein the weight ratio of the suspension 1 to the solution 3 in the step S4 is 1:1-3, the power of the re-ultrasonic dispersion is 0.5kW-1.5kW, the dispersion frequency is 60-80kHz, and the dispersion time is 30-90 min.
9. The method according to claim 1, wherein the weight ratio of the suspension 2 to the solution 2 in step S4 is 1:0.5-4, preferably 1:2-4, the temperature is increased to 50-100 ℃, preferably 50-80 ℃, and the constant temperature curing time is 5-10 days.
10. Use of the adsorbent according to any one of claims 1 to 9 for adsorbing heavy metal ions in sewage.
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