CN114635279A - Active carbon fiber loaded FeAl hydrotalcite composite material and preparation method and application thereof - Google Patents
Active carbon fiber loaded FeAl hydrotalcite composite material and preparation method and application thereof Download PDFInfo
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- CN114635279A CN114635279A CN202210337092.7A CN202210337092A CN114635279A CN 114635279 A CN114635279 A CN 114635279A CN 202210337092 A CN202210337092 A CN 202210337092A CN 114635279 A CN114635279 A CN 114635279A
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- 239000002131 composite material Substances 0.000 title claims abstract description 86
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 38
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 37
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 37
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- 229910015372 FeAl Inorganic materials 0.000 title claims abstract description 36
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- 239000000243 solution Substances 0.000 claims description 24
- 238000005067 remediation Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
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- 229910001385 heavy metal Inorganic materials 0.000 claims description 15
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 12
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 11
- 239000012498 ultrapure water Substances 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000011068 loading method Methods 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000011065 in-situ storage Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
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- 230000000694 effects Effects 0.000 abstract description 20
- 238000001179 sorption measurement Methods 0.000 abstract description 13
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- 231100000614 poison Toxicity 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 239000003440 toxic substance Substances 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 description 47
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 28
- 229910052804 chromium Inorganic materials 0.000 description 28
- 230000008439 repair process Effects 0.000 description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- -1 polytetrafluoroethylene Polymers 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 229910001430 chromium ion Inorganic materials 0.000 description 5
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
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- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
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- 206010027439 Metal poisoning Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
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Images
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/17—Halides of elements of Groups 3 or 13 of the Periodic Table
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/28—Halides of elements of Groups 8, 9, 10 or 18 of the Periodic Table
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention relates to an active carbon fiber loaded FeAl hydrotalcite composite material and a preparation method and application thereof, wherein the composite material is obtained by uniformly agglomerating and attaching FeAl hydrotalcite flake particles on carbon fiber cloth, the flake particles have the size of 200-250nm, the thickness of 40-45nm and the specific surface area of 45-55m2(ii) in terms of/g. The ACF/FeAlLDH composite material provided by the invention has the advantages of large specific surface area and good adsorption effect, can quickly adsorb and fix Cr ions compared with the traditional FeAlLDH, has the adsorption efficiency of up to 99 percent, does not precipitate toxic substances, does not generate secondary pollution, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of polluted soil regeneration, and particularly relates to an active carbon fiber loaded FeAl hydrotalcite composite material, and a preparation method and application thereof.
Background
Chromium (Cr) is an important chemical raw material and is widely applied to industries such as leather making, textile production, printing and dyeing, pigment, chromium plating and the like. With the production of a large amount of chromium-containing products, the chromium pollution in the environment is becoming serious due to the improper treatment of industrial waste liquid containing a large amount of chromium ions. Heavy metal pollutants are poor in mobility in soil, long in residence time, incapable of being degraded by microorganisms, and capable of entering human bodies through media such as water and plants to participate in metabolism and circulation of the human bodies, so that heavy metal poisoning of the human bodies can be caused under long-term influence, and the health of the human bodies is harmed.
At present, the remediation principle of heavy metal contaminated soil comprises the steps of adopting various technologies to remove heavy metal elements in the contaminated soil or reduce the activity and effective components of the heavy metal elements so as to achieve the purpose of soil remediation. Chromium generally exists in two stable valence states, namely Cr (III) and Cr (VI), and the chromium is treated and repaired by two ways: one is to change the existing form of chromium ions and reduce Cr (VI) with high toxicity and strong migration capability into Cr (III) with low toxicity and strong stability so as to achieve the aim of repair; another is to remove the chromium directly from the soil so that the chromium is retained at a concentration near or at the background level of the soil. Based on the two repair approaches, the repair technology of the chromium-contaminated soil mainly comprises a physical repair method, a biological repair method, a chemical repair method and the like. The physical remediation method mainly comprises an electrodynamic remediation technology and the like, and although the technology can realize the separation of chromium in soil, the technology has the disadvantages of large engineering quantity, high construction cost, certain requirements on soil and certain limitations on application. The chemical remediation method typically comprises a chemical leaching technology, a chemical reduction technology and the like, wherein the chemical leaching technology leaches polluted soil to enable leaching water containing hexavalent chromium to enter underground water, and then the underground water containing hexavalent chromium is pumped to the ground surface for treatment, although the treatment effect is obvious, the remediation cost is high, and the engineering quantity is large; the chemical reduction technology is characterized in that a chemical reducing agent is used for reducing pollutants into an insoluble state, so that the migration property and the bioavailability of the pollutants are reduced, and the purpose of repairing the polluted soil is achieved. The bioremediation method usually utilizes plants, animals and microorganisms to absorb heavy metals in soil to achieve the aim of soil remediation, although the technology is simple to implement and low in cost, the technology has high requirements on the environment, the remediation period is long, the biomass is small, the effect is not obvious, and the heavily polluted soil cannot be remediated. In view of the serious influence caused by soil chromium pollution, an economical, efficient and practical treatment technology is urgently needed to be developed.
Disclosure of Invention
One of the purposes of the present invention is to provide an active carbon fiber loaded FeAl hydrotalcite composite material (ACF/fealaldh composite material) that is efficient in cr (vi) adsorption, low in cost, and environmentally friendly, in view of the deficiencies in the prior art.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
an active carbon fiber loaded FeAl hydrotalcite composite material is obtained by uniformly agglomerating FeAl hydrotalcite flake particles and attaching the flake particles to carbon fiber cloth, wherein the flake particles have the size of 200-250nm, the thickness of 40-45nm and the specific surface area of 45-55m2/g。
According to the scheme, the diameter of the active carbon fiber in the carbon fiber cloth is 5-20 mu m, the thickness of the carbon fiber cloth is 2-15mm, and the pore volume is 0.8-1.2cm3/g。
According to the scheme, the FeAl hydrotalcite loading capacity of the activated carbon fiber loaded FeAl hydrotalcite composite material is 5-50% (FeAl hydrotalcite accounts for the mass percentage of the composite material).
The second purpose of the invention is to provide the preparation method of the activated carbon fiber loaded FeAl hydrotalcite composite material, which can efficiently prepare the ACF/FeAlLDH composite material with good loading effect, and has simple operation and low cost.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of the activated carbon fiber loaded FeAl hydrotalcite composite material comprises the following specific steps:
1) mixing AlCl3·6H2O、FeCl2·4H2Adding O into ultrapure water, and fully stirring to obtain a mixed solution;
2) cutting carbon fiber cloth into small pieces with uniform size, adding the small pieces into the mixed solution obtained in the step 1), adding NaOH solution to adjust the pH value of the system to 9, then transferring the solution into a reaction kettle to perform hydrothermal reaction, after the reaction is finished, cooling the reaction solution to room temperature, washing, centrifuging, and drying in vacuum to obtain the activated carbon fiber loaded FeAl hydrotalcite composite material.
According to the scheme, the AlCl is obtained in the step 1)3·6H2O and FeCl2·4H2The molar ratio of O is 1: 2-3.
According to the scheme, the small blocks in the step 2) are squares with the side length of 1-5 cm.
According to the scheme, the carbon fiber cloth and AlCl in the step 2)3·6H2The mass ratio of O is 1: 5-10.
According to the scheme, the concentration of the NaOH solution in the step 2) is 1-4 mol/L.
According to the scheme, the hydrothermal reaction temperature in the step 2) is 100-120 ℃, and the hydrothermal reaction time is 24-36 h.
The invention also aims to provide application of the activated carbon fiber loaded FeAl hydrotalcite composite material in-situ remediation of heavy metal chromium contaminated soil, so as to solve the problems of low treatment efficiency, high energy consumption, long period, complex engineering and the like of the traditional treatment method.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
an application of the activated carbon fiber loaded FeAl hydrotalcite composite material in-situ remediation of heavy metal chromium contaminated soil.
According to the scheme, the specific method for carrying out in-situ remediation on the soil polluted by the heavy metal chromium by using the activated carbon fiber loaded FeAl hydrotalcite composite material comprises the following steps: the activated carbon fiber loaded FeAl hydrotalcite composite material is uniformly applied to heavy metal chromium-polluted soil for in-situ remediation, wherein the application amount of the activated carbon fiber loaded FeAl hydrotalcite composite material is 30-100g/Kg of heavy metal chromium-polluted soil. In order to promote the FeAl hydrotalcite composite material loaded on the activated carbon fiber to be fully contacted with the soil, a proper amount of water can be added.
The invention uses FeAlLDH compounds on the carbon fiber cloth, easy to separate from soil, can change the load capacity of carbon fiber cloth load FeAlLDH through adjusting the carbon fiber cloth quality in the saline solution, and the LDH that the invention provides is large in adsorption capacity, the adsorption capacity is good, in the adsorption process, Cr is2O7 2-CO interlamination with hydrotalcite3 2-Carrying out anion exchange, and simultaneously, adsorbing Fe separated out from the main laminate2+Cr (VI) can be reduced to Cr (III).
The invention has the beneficial effects that:
(1) the ACF/FeAlLDH composite material provided by the invention has the advantages of large specific surface area and good adsorption effect, can quickly adsorb and fix Cr ions compared with the traditional FeAlLDH, has the adsorption efficiency of up to 99 percent, does not precipitate toxic substances, and does not generate secondary pollution;
(2) the preparation method is simple to operate and low in cost;
(3) the repair technology is suitable for in-situ repair of soil with severe chromium pollution, and compared with other repair methods, the repair technology has the advantages of low cost, capability of achieving the aim of soil repair in a short time, and good repair effect on acid and alkaline soil, so that the repair technology has wide application prospect.
Drawings
Fig. 1 is an SEM image of the FeAlLDH composite material prepared in comparative example 1;
FIG. 2 is an XRD pattern of the FeAlLDH composite material prepared in comparative example 1 and the ACF/FeAlLDH composite material prepared in example 1;
FIG. 3 is an SEM image of the ACF/FeAlLDH composite material prepared in example 1;
FIG. 4 is an EDS image of the ACF/FeAlLDH composite material prepared in example 1 before soil remediation;
FIG. 5 is an EDS image of the ACF/FeAlLDH composite prepared in example 1 after soil remediation;
FIG. 6 is a graph showing the repairing effect of the ACF/FeAlLDH composite materials with different loading amounts prepared in examples 1-3 on the chromium-containing soil adsorbed and treated;
FIG. 7 is a graph showing the repairing effect of the ACF/FeAlLDH composite material prepared in example 1 on adsorbing chromium-containing soil of different concentrations for 30 min;
FIG. 8 is a graph showing the time-dependent change of the repairing effect of the ACF/FeAlLDH composite material prepared in example 1 in treating soil containing chromium at different concentrations;
FIG. 9 is a graph showing the total iron content of the solution of the ACF/FeAlLDH composite material prepared in example 1 after adsorbing a chromium-contaminated soil sample with a chromium concentration of 1000mg/Kg for different periods of time;
FIG. 10 is a graph showing the results of repairing chromium-contaminated soil with different addition amounts of the ACF/FeAlLDH composite material prepared in example 1;
FIG. 11 is a graph showing the results of repairing chromium-contaminated soil at different pH values for the ACF/FeAlLDH composite material prepared in example 1.
Detailed Description
For the sake of understanding, the present invention will be further explained below with reference to the following embodiments and the accompanying drawings, but the present invention is not limited to the following embodiments.
The diameter of the active carbon fiber in the carbon fiber cloth used in the embodiment of the invention is 5-10 μm, the thickness of the carbon fiber cloth is 3mm, and the pore volume is 1cm3/g。
Comparative example 1
The preparation method of the FeAlLDH composite material by a coprecipitation method comprises the following specific steps: weighing 4.8g of AlCl3·6H2Adding O into a beaker filled with 210mL of ultrapure water, placing the beaker on a magnetic stirrer, adjusting the temperature to be 25 ℃, rotating at 500rpm, sealing the opening of the beaker by using a safety film, and weighing 8g of FeCl2·4H2Adding O (Fe: Al molar ratio is 2: 1) into the beaker, continuously adding 4mol/L NaOH solution to keep the pH value of the aqueous solution at about 7 in the process, immediately transferring the generated suspended matters into a polytetrafluoroethylene tank, keeping the polytetrafluoroethylene tank at 120 ℃ for 24 hours to carry out hydrothermal reaction, washing the reaction product by using an alcohol-water solution (volume ratio of ethanol to water is 3: 7) for one time to remove redundant impurity ions in the salt solution, washing the reaction product by using ethanol for 2-3 times, then drying the reaction product in vacuum at 50 ℃, and finally grinding the reaction product to obtain the FeAlLDH composite material.
Fig. 1 is an SEM image of the fealdh composite material prepared in this comparative example, and it can be seen that the fealdh synthesized in this comparative example by the conventional method has a regular hexagonal layered structure.
Example 1
An ACF/FeAlLDH composite material is prepared by the following steps:
1) 4.8g of AlCl3·6H2O and 8gFeCl2·4H2Adding O into a beaker filled with 200mL of ultrapure water in advance, and stirring to completely dissolve the O to obtain a mixed solution;
2) weighing 0.76g of carbon fiber cloth, cutting the carbon fiber cloth into small square blocks of 1cm multiplied by 1cm, adding the small square blocks into the mixed solution, stirring for half an hour to enable activated carbon fibers to fully absorb the solution, adding 4mol/L NaOH solution into the system to adjust the pH value to 9, then transferring the salt solution and the carbon fiber cloth into a polytetrafluoroethylene tank, placing the polytetrafluoroethylene tank at 120 ℃ for 24 hours, taking out a reaction kettle after the reaction is finished, cooling, and then using an alcohol-water solution (volume ratio ethanol: water 3: 7) washing once, washing with pure ethanol for 2-3 times, and vacuum drying the product in a vacuum drying oven at 50 ℃ to obtain 0.97g of ACF/FeAlLDH composite material (FeAlLDH loading 21.6%).
Fig. 2 is an XRD pattern of the feallh composite material prepared in comparative example 1 and the ACF/feallh composite material prepared in this example, comparing it to see that a typical feallh structure appears on the activated carbon fiber.
Fig. 3 is an SEM image of the ACF/feallh composite material prepared in this example, and it can be observed that the flaky hydrotalcite particles are supported on the smooth activated carbon fibers.
Example 2
An ACF/FeAlLDH composite material is prepared by the following steps:
1) 4.8g of AlCl3·6H2O and 8gFeCl2·4H2Adding O into a beaker filled with 200mL of ultrapure water in advance, and stirring to completely dissolve the O to obtain a mixed solution;
2) weighing 0.38g of carbon fiber cloth, cutting the carbon fiber cloth into small square blocks of 1cm multiplied by 1cm, adding the small square blocks into the mixed solution, stirring for half an hour to enable active carbon fibers to fully absorb the solution, adding 4mol/L NaOH solution into the system to adjust the pH value to 9, then transferring the salt solution and the carbon fiber cloth into a polytetrafluoroethylene tank, placing the polytetrafluoroethylene tank at 120 ℃ for keeping for 24 hours, taking out a reaction kettle after the reaction is finished, cooling, and then using an alcohol-water solution (volume ratio ethanol: water 3: 7) washing once, washing with pure ethanol for 2-3 times, and vacuum drying the product in a vacuum drying oven at 50 ℃ to obtain 0.45g of ACF/FeAlLDH composite material (the FeAlLDH loading is 15.5%).
Example 3
An ACF/FeAlLDH composite material, the preparation method comprises the following steps:
1) 4.8g of AlCl3·6H2O and 8gFeCl2·4H2Adding O into a beaker filled with 200mL of ultrapure water in advance, and stirring to completely dissolve the O to obtain a mixed solution;
2) weighing 3.82g of carbon fiber cloth, cutting the carbon fiber cloth into small square blocks of 1cm multiplied by 1cm, adding the small square blocks into the mixed solution, stirring for half an hour to enable activated carbon fibers to fully absorb the solution, adding 4mol/L NaOH solution into the system to adjust the pH value to 9, then transferring the salt solution and the carbon fiber cloth into a polytetrafluoroethylene tank, placing the polytetrafluoroethylene tank at 120 ℃ for 24 hours, taking out a reaction kettle after the reaction is finished, cooling, and then using an alcohol-water solution (volume ratio ethanol: water 3: 7) washing once, washing with pure ethanol for 2-3 times, and vacuum drying the product in a vacuum drying oven at 50 ℃ to obtain 5.32g of ACF/FeAlLDH composite material (the FeAlLDH loading is 28.2%).
Example 4
In this example, soil samples containing different chromium concentrations were treated using the ACF/fealdh composite material prepared in example 1 using a laboratory test.
The soil to be tested is soil which is collected from uncontaminated soil in the residential city of Jiangsu province, is air-dried after being collected, is sieved by a 100-mesh sieve, is sealed and stored in a dryer for later use, and the pH value is measured to be 6.21. The soil was artificially contaminated with analytically pure potassium dichromate to prepare a chromium-contaminated soil sample so that the concentrations of Cr (VI) in the soil were 200mg/Kg, 400mg/Kg, 800mg/Kg, and 1000mg/Kg, respectively.
Taking 10mL of a centrifuge tube, respectively adding 5mL of ultrapure water and 1g of a chromium-contaminated soil sample (the concentrations of Cr (VI) in the soil are respectively 200mg/Kg, 400mg/Kg, 800mg/Kg and 1000mg/Kg), placing the centrifuge tube on a rotary mixer, treating the mixture for 60min at 30rpm, then extracting a clear solution through an injector and a filter tip with the diameter of 0.45 mu m, and measuring the concentrations of hexavalent chromium ions in the clear solution by an ultraviolet spectrophotometry, wherein the concentrations are respectively 6.75mg/L, 42.49mg/L, 112.47mg/L and 164.84mg/L and are used as initial concentration values of Cr (VI) in subsequent treatment experiments.
Then 5mL of ultrapure water, 1g of chromium-contaminated soil sample (the concentrations of Cr (VI) in the soil are respectively 200mg/Kg, 400mg/Kg, 800mg/Kg and 1000mg/Kg) and 0.05g of the ACF/FeAlLDH composite material prepared in the embodiment 1-3 are respectively added into a 10mL centrifuge tube, the mixture is placed on a rotary mixer to be treated for 60min under the condition of 30rpm, and the concentration of hexavalent chromium ions in clear liquid is tested, so that the repairing effect of the material on the chromium-contaminated soil is evaluated.
Fig. 4 and 5 are EDS images of the ACF/fealdh composite material prepared in example 1 before and after repairing soil (the concentration of cr (vi) in soil is 1000mg/kg, and the soil is treated at 30rpm for 60min), respectively, and it can be seen from the images that Fe and Al elements can be detected before and after repairing, which can indicate that the load of the ACF/fealdh composite material is stable after adsorption reaction.
As shown in FIG. 6, which is a graph of the repairing effect of the ACF/FeAlLDH composite materials with different loading amounts prepared in examples 1-3 on the chromium-containing soil by adsorption treatment, the removal rate of Cr (VI) in the soil by the composite materials is gradually increased along with the increase of the FeAlLDH loading amount in the ACF/FeAlLDH composite materials.
Example 5
Soil samples prepared in example 2 with different chromium concentrations were treated with the ACF/fealdh composite prepared in example 1.
Taking a 10mL centrifuge tube, respectively adding 5mL ultrapure water, 1g chromium-contaminated soil sample (the concentrations of Cr (VI) in the soil are respectively 200mg/Kg, 400mg/Kg, 800mg/Kg and 1000mg/Kg) and 0.05g ACF/FeAlLDH composite material, placing the sample on a rotary mixer to react for different time (5min, 10min, 15min, 30min and 60min) under the condition of 30rpm, sampling, extracting clear liquid through an injector and a filter head with the particle size of 0.45 mu m, and measuring the concentration of hexavalent chromium ions in the clear liquid by using an ultraviolet spectrophotometry method so as to evaluate the repair efficiency of the ACF/FeAlLDH composite material on the heavy metal chromium-contaminated soil.
As shown in fig. 7, the repair effect of the ACF/fealdh composite material prepared in example 1 in adsorbing and treating chromium-containing soil with different concentrations for 30min is shown, when the soil with different degrees of chromium pollution is treated, the repair effect of the ACF/fealdh composite material is slightly reduced with the increase of the chromium pollution degree, but the repair rate of the soil with different degrees of chromium pollution is higher than 80%, and the maximum repair rate can reach 98%.
As shown in fig. 8, which is a graph showing the time-dependent change of the repair effect of the ACF/fealdh composite material prepared in example 1 when used for treating chromium-contaminated soil with different concentrations, it can be seen that the removal rate of the ACF/fealdh composite material for 200mg/Kg of chromium-contaminated soil is as high as 98% or more in 15min, the removal rate fluctuation is small as the treatment time increases, the repair efficiency for soil gradually decreases as the chromium concentration in soil increases, and the removal rate for 60min after treatment can reach 98% when the chromium concentration in soil is 1000mg/Kg, indicating that the repair effect of the material for chromium-contaminated soil is good.
After a chromium-contaminated soil sample with the chromium concentration of 1000mg/Kg in the soil of the embodiment is subjected to adsorption treatment by using the ACF/fealaldh composite material prepared in the embodiment 1 for different periods of time, the solution is subjected to content measurement of total iron by using an ultraviolet spectrophotometry, and the result is shown in fig. 9, the content of total iron in the solution is close to zero in the adsorption treatment process, that is, the iron dissolution amount is small in the adsorption reaction process, which indicates that the chromium-contaminated soil treated by the method cannot generate secondary pollution.
Example 6
Contaminated soil with the concentration of Cr (VI) prepared in example 2 being 1g/Kg is treated by the ACF/FeAlLDH composite material prepared in example 1, and the repairing effect of different ACF/FeAlLDH composite material dosage on the heavily chromium-contaminated soil is researched.
5mL of ultrapure water, 1g of chromium-contaminated soil sample and different amounts (0.03g, 0.05g, 0.08g and 0.10g) of ACF/FeAlLDH composite material were sequentially added to a 10mL centrifuge tube, and the sample was taken after the reaction was carried out for 60min at 30rpm in a rotary homogenizer under the same reaction conditions and measurement manner as in example 2.
The results of the repair of the chromium-contaminated soil by using different addition amounts of the ACF/FeAlLDH composite material are shown in FIG. 10, and it can be seen that the removal rate of Cr (VI) is increased with the increase of the addition amount of the ACF/FeAlLDH composite material, and the removal rate is up to 99%.
Example 7
The ACF/FeAlLDH composite material prepared in the embodiment 1 is used for treating polluted soil with Cr (VI) concentration of 1g/Kg and different pH values, and the influence of different pH values of the soil on the remediation effect is researched.
5mL of ultrapure water, 1g of a chromium-contaminated soil sample (pH values of 3, 4, 7 and 10, respectively) and 0.05g of an ACF/FeAlLDH composite material were sequentially added to a 10mL centrifuge tube, and the mixture was placed on a rotary homogenizer to react at 30rpm for 60min, followed by sampling, wherein the reaction conditions and the measurement manner were the same as in example 2.
The repairing effect of the ACF/FeAlLDH composite material under different pH values is shown in FIG. 11, the influence of the pH value on the repairing effect of the ACF/FeAlLDH composite material is small, the removal rate of Cr (VI) by the ACF/FeAlLDH composite material is about 80%, and the material can be used for treating acid soil and alkaline soil and has wide applicability in the aspect of soil repairing.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. The active carbon fiber loaded FeAl hydrotalcite composite material is characterized in that the composite material is obtained by uniformly agglomerating FeAl hydrotalcite flake particles adhered to carbon fiber cloth, the flake particles have the size of 200-250nm, the thickness of 40-45nm and the specific surface area of 45-55m2/g。
2. The FeAl hydrotalcite composite material loaded on activated carbon fiber according to claim 1, wherein the diameter of the activated carbon fiber in the carbon fiber cloth is 5-20 μm, the thickness of the carbon fiber cloth is 2-15mm, and the pore volume is 0.8-1.2cm3/g。
3. The activated carbon fiber-loaded FeAl hydrotalcite composite material according to claim 1, wherein the FeAl hydrotalcite loading in the activated carbon fiber-loaded FeAl hydrotalcite composite material is 5-50%.
4. A preparation method of the activated carbon fiber loaded FeAl hydrotalcite composite material as claimed in any one of claims 1 to 3 is characterized by comprising the following specific steps:
1) mixing AlCl3·6H2O、FeCl2·4H2Adding O into ultrapure water, and fully stirring to obtain a mixed solution;
2) cutting carbon fiber cloth into small pieces with uniform size, adding the small pieces into the mixed solution obtained in the step 1), adding NaOH solution to adjust the pH value of the system to 9, then transferring the solution into a reaction kettle to perform hydrothermal reaction, after the reaction is finished, cooling the reaction solution to room temperature, washing, centrifuging, and drying in vacuum to obtain the activated carbon fiber loaded FeAl hydrotalcite composite material.
5. The method for preparing the activated carbon fiber loaded FeAl hydrotalcite composite material according to claim 4, wherein the AlCl in the step 1) is adopted3·6H2O and FeCl2·4H2The molar ratio of O is 1: 2-3.
6. The preparation method of the activated carbon fiber loaded FeAl hydrotalcite composite material according to claim 4, wherein the carbon fiber cloth and AlCl in the step 2)3·6H2The mass ratio of O is 1: 5-10.
7. The preparation method of the activated carbon fiber-supported FeAl hydrotalcite composite material according to claim 4, wherein the concentration of the NaOH solution in the step 2) is 1-4 mol/L.
8. The method for preparing the activated carbon fiber loaded FeAl hydrotalcite composite material as claimed in claim 4, wherein the hydrothermal reaction temperature in step 2) is 100-120 ℃, and the hydrothermal reaction time is 24-36 h.
9. The application of the activated carbon fiber-loaded FeAl hydrotalcite composite material as defined in any one of claims 1 to 3 in-situ remediation of heavy metal chromium-contaminated soil.
10. The application of the activated carbon fiber loaded FeAl hydrotalcite composite material in-situ remediation of heavy metal chromium-contaminated soil according to claim 9 is characterized in that the specific method comprises the following steps: the activated carbon fiber loaded FeAl hydrotalcite composite material is uniformly applied to heavy metal chromium-polluted soil for in-situ remediation, wherein the application amount of the activated carbon fiber loaded FeAl hydrotalcite composite material is 30-100g/Kg of heavy metal chromium-polluted soil.
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