CN113184921B - LDH-based composite material based on nickel-containing sludge and preparation method thereof - Google Patents
LDH-based composite material based on nickel-containing sludge and preparation method thereof Download PDFInfo
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- CN113184921B CN113184921B CN202110440510.0A CN202110440510A CN113184921B CN 113184921 B CN113184921 B CN 113184921B CN 202110440510 A CN202110440510 A CN 202110440510A CN 113184921 B CN113184921 B CN 113184921B
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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Abstract
The invention belongs to the technical field of composite materials, relates to an LDH-based composite material, and particularly relates to an LDH-based composite material based on nickel-containing sludge, which comprises sludge and LDH nanosheets, wherein the size of the LDH nanosheets is 400-800-nm, and the mass percentage content of the LDH nanosheets is not less than 10%, and the LDH nanosheets are one or more of Ni-Al LDH, mg-Al LDH and Zn-Al LDH, and are uniformly mixed with the sludge. The invention also discloses a preparation method of the material. The invention prepares the functional material by using the solid waste sludge containing heavy metals, changes the sludge into valuables, solves the problem that the heavy metal sludge is difficult to treat, has stable property and large specific surface area, and can be used in the fields of catalysis, adsorption and chemical separation; the preparation method is simple and economic, has no secondary pollution and is suitable for industrial application.
Description
Technical Field
The invention belongs to the technical field of composite materials, relates to an LDH-based composite material, and particularly relates to an LDH-based composite material based on nickel-containing sludge and a preparation method thereof.
Background
Electroplating contributes greatly to the fields of materials, energy sources, chemical industry and the like, and also causes environmental pollution, such as heavy metal ions and sludge containing heavy metals. Nickel-containing sludge is one of the main types of heavy metal-containing sludge, mainly derived from industrial production processes such as metal smelting, electroplating, leather and batteries, and wastewater discharge. Ni (Ni) 2+ The equilong metal ions can be biologically accumulated in plants, animals and human bodies through food chains, so that great influence is caused on human life and production, and sustainable development of socioeconomic performance is limited.
The traditional heavy metal sludge treatment method is mainly a landfill method, the investment is small, the treatment capacity is large, but nutrient substances contained in the sludge can create conditions for the propagation of a large number of pathogens, and if harmful components leak, groundwater pollution can be caused. At present, the methods for recovering and removing heavy metal ions from sludge mainly comprise a chemical leaching method, a stabilization/solidification method, an extraction method, a phytoremediation method, a membrane separation method, an ion exchange method and the like, and the treatment methods inevitably have the defects of high cost, low treatment efficiency, incomplete treatment, easiness in secondary pollution and the like. Because of its complex composition, few studies have focused on the resource utilization of heavy metal sludges. Therefore, there is an urgent need to perform harmless treatment and recycling of sludge.
Layered Double Hydroxides (LDHs) are inorganic functional materials with strong interlayer bonds and weak interlayer interaction force, have excellent capability of capturing organic and inorganic anions, and are widely applied to the fields of pollution control, chemical separation and the like. The invention provides an LDH-based composite material based on nickel-containing sludge, which takes nickel-containing sludge as a raw material to change sludge into valuables, solves the problem that heavy metal sludge is difficult to treat, and provides a pollution control material with very promising development, and the research and application of the material show great potential in the field of environmental protection and practical industrial application.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an LDH-based composite material based on nickel-containing sludge and a preparation method thereof.
The technical scheme is as follows:
an LDH-based composite material based on nickel-containing sludge comprises sludge and LDH nanosheets, wherein the LDH nanosheets are 400-800 nm in size and not lower than 10% in mass, and the LDH nanosheets are one or more of Ni-Al LDH, mg-Al LDH and Zn-Al LDH in any combination and are uniformly mixed with the sludge.
The preparation method of the LDH-based composite material based on the nickel-containing sludge comprises the following steps:
a) Drying the nickel-containing sludge at 120-200 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 400-800 ℃ for 4-8 h to obtain pretreated sludge;
b) Dispersing porous alumina, pretreated sludge and divalent metal salt in 0.05-0.5 mol/L of precipitator solution according to the mol ratio of the porous alumina to the precipitator of 2:1-1:4, uniformly mixing, transferring to a reaction kettle, carrying out hydrothermal reaction at 140-220 ℃ for 12-48 h, filtering, washing with water and ethanol for 2-6 times respectively, drying at 50-90 ℃ for 12-24 h, and cooling to room temperature to obtain the LDH-based composite material of nickel-containing sludge, wherein the mol ratio of the divalent metal salt to the alumina is 0-1:1, and the mol ratio of the porous alumina to (divalent metal salt+nickel in nickel-containing sludge) is 1:8-1:2.
In a preferred embodiment of the present invention, the nickel content in the nickel-containing sludge in the step a) is not less than 5% wt%.
In the preferred embodiment of the present invention, the porous alumina in the step b) is one or more of alumina fiber, alumina microsphere and flower-like alumina, and the specific surface area is not less than 100m 2 /g。
In a preferred embodiment of the present invention, the precipitant in step b) is one or any combination of hexamethylenetetramine and urea, preferably hexamethylenetetramine.
In a preferred embodiment of the present invention, the divalent metal salt in step b) is one or any combination of magnesium salt and zinc salt.
In a preferred embodiment of the present invention, the magnesium salt in step b) is magnesium nitrate, magnesium sulfate, magnesium chloride, preferably magnesium nitrate.
In a preferred embodiment of the present invention, the zinc salt in step b) is zinc nitrate, zinc acetate, zinc sulfate or zinc chloride.
The invention prepares the functional material by using the solid waste sludge containing heavy metals, prepares the functional material with high specific surface area, and provides a method for recycling the nickel-containing sludge, and the prepared functional material has the advantages of high specific surface area and developed porosity and has potential application in the fields of adsorption, catalysis, chemical separation and the like.
Advantageous effects
The LDH-based composite material based on nickel-containing sludge is prepared from solid waste sludge containing heavy metals serving as a raw material through hydrothermal reaction, and comprises sludge and LDH nanosheets, wherein the size of the LDH nanosheets is 400-800 nm, the content of the LDH nanosheets is not less than 10%, and the LDH nanosheets are one or a combination of a plurality of Ni-Al LDH, mg-Al LDH and Zn-Al LDH. The invention changes the sludge into valuable, solves the problem that heavy metal sludge is difficult to treat, has stable property and large specific surface area, and can be used in the fields of catalysis, adsorption and chemical separation; the preparation method is simple and economic, has no secondary pollution and is suitable for industrial application.
Drawings
Fig. 1. Example 1 electron microscopy images of LDH-based composite materials based on nickel-containing sludge, a being SEM images and B being TEM images.
Detailed Description
The present invention will be described in detail with reference to the following examples, so that those skilled in the art can better understand the present invention, but the present invention is not limited to the following examples.
Example 1
A method for preparing an LDH-based composite material containing nickel sludge, comprising the following steps:
a) Drying sludge containing 13.78 and wt percent of nickel at 120 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 400 ℃ for 4h to obtain pretreated sludge;
b) Sequentially adding 0.178 g magnesium nitrate, 4.251 g pretreated sludge and 1.12 g hexamethylenetetramine into 50 mL deionized water, uniformly stirring, then adding 0.204 g aluminum oxide microspheres, uniformly mixing, transferring into a reaction kettle for hydrothermal treatment, and carrying out static reaction at 180 ℃ for 24 h. After the reaction, cooling to room temperature, filtering, washing with water and ethanol for 3 times respectively, and drying at 70 ℃ for 12 h to obtain the LDH-based composite material of the nickel-containing sludge.
The prepared LDH-based composite material of the nickel-containing sludge has the specific surface area of 216.96 m 2 Per g, a total pore volume of 0.44 cm 3 /g。
As can be seen from FIG. 1, multi-layered flower-shaped LDH nano-sheets are successfully grown vertically on the uneven and rough surface sludge surface, the nano-sheets are overlapped in a staggered way and are in a micro-bending shape, and the average diameter is 0.5-1.5 mu m.
Example 2
A method for preparing an LDH-based composite material containing nickel sludge, comprising the following steps:
a) Drying sludge containing 15.63 and wt percent of nickel at 150 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 500 ℃ for 4h to obtain pretreated sludge;
b) Sequentially adding 0.151 g zinc nitrate, 4.506 g pretreated sludge and 1.12 g hexamethylenetetramine into 50 mL deionized water, uniformly stirring, then adding 0.204 g aluminum oxide microspheres, uniformly mixing, transferring into a reaction kettle for hydrothermal treatment, and carrying out static reaction at 160 ℃ for 36 h. After the reaction, cooling to room temperature, filtering, washing with water and ethanol for 2 times respectively, and drying at 90 ℃ to 14 and h to obtain the LDH-based composite material of the nickel-containing sludge.
The prepared LDH-based composite material of the nickel-containing sludge has the specific surface area of 217.35 m 2 Per gram, a total pore volume of 0.46. 0.46 cm 3 /g。
Example 3
A method for preparing an LDH-based composite material containing nickel sludge, comprising the following steps:
a) Drying sludge containing 8.43 and wt percent of nickel at 180 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 800 ℃ for 5 h to obtain pretreated sludge;
b) Adding zinc sulfate 0.644 g, pretreated sludge 22.548 g and urea 1.44 g into deionized water 50 mL in sequence, stirring uniformly, adding flower-like alumina 0.419 g, mixing uniformly, transferring into a reaction kettle for hydrothermal treatment, carrying out static reaction at 220 ℃ for 24h, filtering, washing with water and ethanol for 4 times respectively, and drying at 70 ℃ for 16 h to obtain the LDH-based composite material containing nickel sludge.
The prepared LDH-based composite material of the nickel-containing sludge has the specific surface area of 203.87 m 2 Per g, a total pore volume of 0.39 cm 3 /g。
Example 4
A method for preparing an LDH-based composite material containing nickel sludge, comprising the following steps:
a) Drying sludge containing 20.09 and wt percent of nickel at 195 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 600 ℃ for 5 h to obtain pretreated sludge;
b) Sequentially adding 0.096 g magnesium sulfate, 0.076 g magnesium chloride, 5.864 g pretreated sludge and 2.24 g hexamethylenetetramine into 50 mL deionized water, uniformly stirring, then adding 0.306 g alumina microspheres, uniformly mixing, transferring into a reaction kettle for hydrothermal treatment, carrying out static reaction at 180 ℃ for 48h, filtering, washing with water and ethanol for 4 times respectively, and drying at 90 ℃ for 18 h to obtain the LDH-based composite material containing nickel sludge.
The prepared LDH-based composite material of the nickel-containing sludge has the specific surface area of 217.69 m 2 Per gram, a total pore volume of 0.46. 0.46 cm 3 /g。
Example 5
A method for preparing an LDH-based composite material containing nickel sludge, comprising the following steps:
a) Drying sludge containing 14.18 percent wt percent of nickel at 130 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 700 ℃ for 8h to obtain pretreated sludge;
b) Adding 0.653 g zinc chloride, 7.450 g pretreated sludge and 0.264 g urea into 50 mL deionized water in sequence, stirring uniformly, adding 0.308 g alumina microspheres, mixing uniformly, transferring into a reaction kettle for hydrothermal treatment, performing static reaction at 200 ℃ for 48h, filtering, washing with water and ethanol for 6 times respectively, and drying at 90 ℃ for 12 h to obtain the LDH-based composite material of nickel-containing sludge.
The prepared LDH-based composite material of the nickel-containing sludge has the specific surface area of 206.19 m 2 Per g, a total pore volume of 0.40 cm 3 /g。
Example 6
A method for preparing an LDH-based composite material containing nickel sludge, comprising the following steps:
a) Drying sludge containing 16.87 and wt% of nickel at 200 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 450 ℃ for 6 h to obtain pretreated sludge;
b) Adding 0.384 g magnesium sulfate, 0.218 g magnesium chloride, 5.567 g pretreated sludge and 3.782 g hexamethylenetetramine into 50 mL deionized water in sequence, stirring uniformly, adding 0.459 g alumina fibers, mixing uniformly, transferring into a reaction kettle for hydrothermal treatment, carrying out static reaction at 160 ℃ for 18 h, filtering, washing with water and ethanol for 3 times respectively, and drying at 80 ℃ for 12 h to obtain the LDH-based composite material containing nickel sludge.
The prepared LDH-based composite material of the nickel-containing sludge has the specific surface area of 218.47 m 2 Per gram, a total pore volume of 0.45. 0.45 cm 3 /g。
Example 7
A method for preparing an LDH-based composite material containing nickel sludge, comprising the following steps:
a) Drying sludge containing 10.98 and wt percent of nickel at 200 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 650 ℃ for 4h to obtain pretreated sludge;
b) Sequentially adding 0.152 g magnesium chloride, 10.695 g pretreated sludge and 0.485 g urea into 50 mL deionized water, stirring uniformly, then adding 0.227 g flower-shaped alumina, mixing uniformly, transferring into a reaction kettle for hydrothermal treatment, carrying out static reaction at 190 ℃ for 36 h, filtering, washing with water and ethanol for 5 times respectively, and drying at 50 ℃ for 24h to obtain the LDH-based composite material of nickel-containing sludge.
The prepared LDH-based composite material of the nickel-containing sludge has the specific surface area of 201.94 m 2 Per g, a total pore volume of 0.41 cm 3 /g。
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. The preparation method of the LDH-based composite material based on the nickel-containing sludge is characterized by comprising the following steps of:
a) Drying the nickel-containing sludge at 120-200 ℃, grinding and sieving to obtain powder with the particle size smaller than 100 mu m, and calcining at 400-800 ℃ for 4-8 hours to obtain pretreated sludge;
b) Dispersing porous alumina, pretreated sludge and divalent metal salt in 0.05-0.5 mol/L of precipitator solution according to the mol ratio of the porous alumina to the precipitator of 2:1-1:4, uniformly mixing, transferring to a reaction kettle, carrying out hydrothermal reaction for 12-48 h at 140-220 ℃, filtering, washing with water and ethanol for 2-6 times respectively, drying for 12-24 h at 50-90 ℃, and cooling to room temperature to obtain the LDH-based composite material of nickel-containing sludge, wherein the mol ratio of the divalent metal salt to the alumina is 0-1:1, and the mol ratio of the porous alumina to the divalent metal salt to nickel in the nickel-containing sludge is 1:8-1:2.
2. The method for producing an LDH-based composite material based on nickel-containing sludge according to claim 1, wherein: the nickel in the nickel-containing sludge in the step a) is not less than 5wt%.
3. The method for producing an LDH-based composite material based on nickel-containing sludge according to claim 1, wherein: the porous alumina in the step b) is one or more of alumina fiber, alumina microsphere and flower-like alumina, and the specific surface area is not less than 100m 2 /g。
4. The method for producing an LDH-based composite material based on nickel-containing sludge according to claim 1, wherein: the precipitant in the step b) is one or any combination of hexamethylenetetramine and urea.
5. The method for producing an LDH-based composite material based on a nickel-containing sludge according to claim 4, wherein: the precipitant in step b) is hexamethylenetetramine.
6. The method for producing an LDH-based composite material based on nickel-containing sludge according to claim 1, wherein: the divalent metal salt in the step b) is one or any combination of magnesium salt and zinc salt.
7. The method for producing an LDH-based composite material based on a nickel-containing sludge according to claim 6, wherein: the magnesium salt in step b) is magnesium nitrate, magnesium sulfate or magnesium chloride.
8. The method for producing an LDH-based composite material based on nickel-containing sludge according to claim 7, wherein: the magnesium salt in step b) is magnesium nitrate.
9. The method for producing an LDH-based composite material based on a nickel-containing sludge according to claim 6, wherein: the zinc salt in the step b) is zinc nitrate, zinc acetate, zinc sulfate or zinc chloride.
10. The nickel-containing sludge-based LDH-based composite material prepared by the method according to any one of claims 1 to 9, comprising sludge and LDH nanosheets, wherein the size of the LDH nanosheets is 400 to 800nm, and the mass percentage content is not less than 10%, and the nickel-containing sludge-based LDH-based composite material is characterized in that: the LDH nanosheets are one or more of Ni-Al LDH, mg-Al LDH and Zn-Al LDH, and are uniformly mixed with sludge.
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