CN112410037B - Composite functional material for soil pollution treatment and preparation method thereof - Google Patents
Composite functional material for soil pollution treatment and preparation method thereof Download PDFInfo
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- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
- C09K17/04—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only applied in a physical form other than a solution or a grout, e.g. as granules or gases
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
Abstract
A composite functional material for treating soil pollution is prepared through crushing straw, immersing in alkali solution, immersing in sodium chlorite solution to obtain straw fibre suspension, adding calcium chloride to said solution, and regulating pH value to neutral state to obtain straw fibre/calcium carbonate mixture; calcining the straw fiber/calcium carbonate mixture under the protection of inert gas to form a biochar-coated calcium oxide composite material; mixing manganese nitrate and ferric nitrate into a precursor solution, dipping the composite material into the precursor solution, repeatedly operating to control the load capacity, and roasting to obtain the MnFeO/C @ CaO catalytic material. The catalytic material can synchronously catalyze and oxidize volatile organic compounds in the thermal desorption process, and meanwhile, after high-temperature reaction, the catalytic material is decomposed into soil conditioners such as manganese oxide, ferric oxide, calcium oxide and the like, so that the functions of improving soil and adjusting the pH value of the soil are achieved, and secondary pollution to the soil is avoided.
Description
Technical Field
The invention relates to the field of soil pollutant treatment, in particular to a composite functional material for soil pollution treatment and a preparation method thereof.
Background
With the increasing degree of soil pollution, more and more researchers are studying the remediation technology of the polluted soil. Different types of contaminated soil require different remediation techniques. At present, soil pollution remediation technologies can be classified into physical remediation technologies, chemical remediation technologies, biological remediation technologies, and combined remediation technologies according to application principles and remediation mechanisms. Heat treatment technology is one of the most widely used physical repair technologies at present. The heat treatment technology mainly comprises the following steps: contaminated soil steam extraction technology, microwave/ultrasonic heating technology, thermal desorption technology and the like.
Thermal desorption technology is widely applied to the removal treatment process of volatile organic compounds and semi-volatile organic compounds in soil. In the process of repairing soil, the method is often applied to the repair of the soil with the pollution of refractory organic matters as main pollutants. The thermal desorption technology has the advantages of wider pollutant treatment range, capability of reusing the repaired soil and the like. However, the pollutants need to be removed from the soil through a long desorption process, the treatment cost is high, and the like. Therefore, the development of an exogenous pollution-free substance for improving the removal of pollutants in soil has very important practical application significance and value.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides a composite functional material for soil pollution control and a preparation method thereof, wherein a catalytic material can synchronously catalyze and oxidize volatile organic compounds in the thermal desorption process, and meanwhile, after high-temperature reaction, the catalytic material is decomposed into soil conditioners such as manganese oxide, iron oxide, calcium oxide and the like, so that the functions of improving soil and adjusting the pH value of the soil are achieved, and secondary pollution to the soil is avoided.
The technical scheme is as follows: a preparation method of a composite functional material for treating soil pollution comprises the steps of crushing straws, soaking the crushed straws in alkali, soaking the straws in a sodium chlorite solution to form a straw fiber suspension, adding calcium chloride into the solution, and adjusting the pH value to be neutral to form a straw fiber/calcium carbonate mixture; calcining the straw fiber/calcium carbonate mixture under the protection of inert gas to form a biochar-coated calcium oxide composite material; mixing manganese nitrate and ferric nitrate into a precursor solution, dipping the composite material into the precursor solution, repeatedly operating to control the load capacity, and roasting to obtain the MnFeO/C @ CaO catalytic material.
The preparation method of the straw fiber/calcium carbonate mixture comprises the following specific steps: (1) crushing straws into 0.5-5 mm, performing alkali treatment by using 1 mol/L NaOH solution, stirring for 3 hours at 80 ℃, filtering by using a filter screen, and washing by using deionized water until the pH value is neutral, and marking as a sample 1; (2) dropwise adding acetic acid into a 1 mol/L sodium chlorite solution to adjust the pH value of the solution to 4-5, then placing a sample 1 into the prepared sodium chlorite solution, stirring for 3 hours at 80 ℃, washing for 3 times by using deionized water to remove the sodium chlorite in the solution, and finally adding the deionized water to form a straw fiber suspension liquid with the pH value of 6; (3) adding 5 g/L calcium chloride into the straw fiber suspension, adjusting the pH of the suspension to 7 by 1 mol/L sodium carbonate to form a straw fiber/calcium carbonate mixed solution, and filtering the mixed solution by using a filter screen to form a straw fiber/calcium carbonate mixture.
The volume ratio of the straw fiber suspension to 5 g/L calcium chloride in the step (3) is 3:1-1: 3.
Mixing the above mixture with N2Or calcining the mixture for 2 hours at the temperature of 600-800 ℃ under the protection of Ar to form the biochar coated calcium oxide composite material C @ CaO.
And mixing the manganese nitrate and the ferric nitrate according to the molar ratio of Mn to Fe =2:1-1:2 to prepare a precursor solution.
And (3) soaking the biochar-coated calcium oxide composite material in a precursor solution, and circularly operating according to a method of drying at the temperature of 2 h-105 ℃ until the loading capacity reaches 5-20 wt.%.
Coating the biochar loaded with Fe and Mn metal with calcium oxide composite material in N2Or roasting the mixture for 2 to 3 hours at the temperature of between 450 and 550 ℃ under the protection of Ar to form the MnFeO/C @ CaO catalytic material.
The MnFeO/C @ CaO catalytic material prepared by the preparation method.
The MnFeO/C @ CaO catalytic material is used for thermal desorption and synchronous catalytic oxidation of volatile organic compounds in soil.
Has the advantages that: the biochar is low in price and environment-friendly, is used as a carrier, calcium carbonate is introduced in the process of preparing the biochar and can be combined with straw fibers, and the calcium carbonate forms calcium oxide in the process of high-temperature calcination, so that the biochar can be used as a biochar support and can also improve the pore volume and the specific surface area of the biochar, and the effective load of a catalyst is promoted; MnFeO loaded on C @ CaO synchronously catalyzes and oxidizes volatile organic compounds under the high-temperature condition of soil thermal desorption; after high-temperature reaction, the catalytic material can be decomposed into soil conditioners such as manganese oxide, iron oxide, calcium oxide and the like, and the functions of improving soil and adjusting the pH value of the soil are achieved. The MnFeO/C @ CaO catalytic material prepared by the invention has the advantages of low price, environmental friendliness, convenience in use and the like.
Drawings
FIG. 1 is a schematic diagram of the removal rate of contaminants from soil after thermal desorption under different conditions;
fig. 2 is a schematic diagram of the removal rate of pollutants in thermal desorption tail gas under different conditions.
Detailed Description
Example 1
In the embodiment, the preparation method of the MnFeO/C @ CaO catalytic material is as follows:
(1) crushing straws into 0.5 mm, performing alkali treatment by using 1 mol/L NaOH solution, stirring for 3 hours at 80 ℃, filtering by using a filter screen, and washing by using deionized water until the pH value is neutral, and marking as a sample 1.
(2) Dropwise adding acetic acid into a 1 mol/L sodium chlorite solution to adjust the pH value of the solution to 4-5, then placing the sample 1 into the prepared sodium chlorite solution, stirring for 3 hours at 80 ℃, washing for 3 times by using deionized water to remove the sodium chlorite in the solution, and finally adding the deionized water to form a straw fiber suspension liquid with the pH value of 6.
(3) Adding 5 g/L calcium chloride into the straw fiber suspension according to the volume ratio of 3:1, adjusting the pH of the suspension to 7 by 1 mol/L sodium carbonate to form a straw fiber/calcium carbonate mixed solution, and filtering the mixed solution by using a filter screen to form a straw fiber/calcium carbonate mixture.
(4) Mixing the straw fiber/calcium carbonate mixture in N2And Ar and other inert gases are used for calcining for 2 hours at 600 ℃ to form the biochar coated calcium oxide composite material C @ CaO.
(5) And mixing manganese nitrate and ferric nitrate metal salt according to a molar ratio of Mn to Fe =2 to 1 to prepare a precursor solution.
(6) And (3) soaking C @ CaO in the precursor solution, and circularly operating according to a method of soaking for 2 h to 105 ℃ for drying until the load reaches 5 wt.%.
(7) C @ CaO loaded with Fe and Mn metals is added into N2And Ar and other inert gases are used for calcining for 3 h at 450 ℃ to form the MnFeO/C @ CaO catalytic material.
The prepared MnFeO/C @ CaO catalytic material is used for thermal desorption treatment of soil pollutants including petroleum hydrocarbon, phenanthrene and dichlorobiphenyl, wherein the concentration of the petroleum hydrocarbon is 1 mg/kg, the concentration of the phenanthrene is 1 mg/kg, and the concentration of the dichlorobiphenyl is 0.6 mg/kg.
The catalytic material is added in the following way: firstly stirring and mixing the MnFeO/C @ CaO catalytic material with contaminated soil according to the adding amount of 5 g/kg, then carrying out thermal desorption treatment on the soil mixed with the catalytic material at 450 ℃, and after the treatment is finished, detecting and analyzing pollutants and thermal desorption tail gas in the soil.
Example 2
In the embodiment, the preparation method of the MnFeO/C @ CaO catalytic material is as follows:
(1) crushing the straws into 1.5 mm, performing alkali treatment by using 1 mol/L NaOH solution, stirring for 3 hours at 80 ℃, filtering by using a filter screen, and washing by using deionized water until the pH value is neutral, and marking as a sample 1.
(2) Dropwise adding acetic acid into a 1 mol/L sodium chlorite solution to adjust the pH value of the solution to 4-5, then placing the sample 1 into the prepared sodium chlorite solution, stirring for 3 hours at 80 ℃, washing for 3 times by using deionized water to remove the sodium chlorite in the solution, and finally adding the deionized water to form a straw fiber suspension liquid with the pH value of 6.
(3) Adding 5 g/L calcium chloride into the straw fiber suspension according to the volume ratio of 1:1, adjusting the pH of the suspension to 7 by 1 mol/L sodium carbonate to form a straw fiber/calcium carbonate mixed solution, and filtering the mixed solution by using a filter screen to form a straw fiber/calcium carbonate mixture.
(4) Mixing the straw fiber/calcium carbonate mixture in N2And Ar and other inert gases are used for calcining for 2 h at 700 ℃ to form the biochar coated calcium oxide composite material C @ CaO.
(5) Manganese nitrate and ferric nitrate metal salt are mixed according to a molar ratio of Mn: and mixing Fe =1:1 to prepare a precursor solution.
(6) And (3) soaking C @ CaO in the precursor solution, and circularly operating according to a method of soaking for 2 h to 105 ℃ for drying until the load reaches 10 wt.%.
(7) C @ CaO loaded with Fe and Mn metals is added into N2Ar, etc. inertCalcining for 2.5 h at 500 ℃ under the protection of the gas to form MnFeO/C @ CaO catalytic material.
The prepared MnFeO/C @ CaO catalytic material is used for thermal desorption treatment of soil pollutants including petroleum hydrocarbon, phenanthrene and dichlorobiphenyl, wherein the concentration of the petroleum hydrocarbon is 1 mg/kg, the concentration of the phenanthrene is 1 mg/kg, and the concentration of the dichlorobiphenyl is 0.6 mg/kg.
The catalytic material is added in the following way: firstly stirring and mixing the MnFeO/C @ CaO catalytic material with contaminated soil according to the adding amount of 5 g/kg, then carrying out thermal desorption treatment on the soil mixed with the catalytic material at 450 ℃, and after the treatment is finished, detecting and analyzing pollutants and thermal desorption tail gas in the soil.
Example 3
In the embodiment, the preparation method of the MnFeO/C @ CaO catalytic material is as follows:
(1) crushing the straws into 3 mm, performing alkali treatment by using 1 mol/L NaOH solution, stirring for 3 hours at 80 ℃, filtering by using a filter screen, and washing by using deionized water until the pH value is neutral, and marking as a sample 1.
(2) Dropwise adding acetic acid into a 1 mol/L sodium chlorite solution to adjust the pH value of the solution to 4-5, then placing the sample 1 into the prepared sodium chlorite solution, stirring for 3 hours at 80 ℃, washing for 3 times by using deionized water to remove the sodium chlorite in the solution, and finally adding the deionized water to form a straw fiber suspension liquid with the pH value of 6.
(3) Adding 5 g/L calcium chloride into the straw fiber suspension according to the volume ratio of 2:1, adjusting the pH of the suspension to 7 by 1 mol/L sodium carbonate to form a straw fiber/calcium carbonate mixed solution, and filtering the mixed solution by using a filter screen to form a straw fiber/calcium carbonate mixture.
(4) Mixing the straw fiber/calcium carbonate mixture in N2And Ar and other inert gases are used for calcining for 2 h at 800 ℃ to form the biochar coated calcium oxide composite material C @ CaO.
(5) Manganese nitrate and ferric nitrate metal salt are mixed according to a molar ratio of Mn: and mixing Fe =1:2 to prepare a precursor solution.
(6) And (3) soaking C @ CaO in the precursor solution, and circularly operating according to a method of soaking for 2 h to 105 ℃ for drying until the load reaches 15 wt.%.
(7) C @ CaO loaded with Fe and Mn metals is added into N2And Ar and other inert gases are used for calcining for 2 h at 550 ℃ to form the MnFeO/C @ CaO catalytic material.
The prepared MnFeO/C @ CaO catalytic material is used for thermal desorption treatment of soil pollutants including petroleum hydrocarbon, phenanthrene and dichlorobiphenyl, wherein the concentration of the petroleum hydrocarbon is 1 mg/kg, the concentration of the phenanthrene is 1 mg/kg, and the concentration of the dichlorobiphenyl is 0.6 mg/kg.
The catalytic material is added in the following way: firstly stirring and mixing the MnFeO/C @ CaO catalytic material with contaminated soil according to the adding amount of 5 g/kg, then carrying out thermal desorption treatment on the soil mixed with the catalytic material at 450 ℃, and after the treatment is finished, detecting and analyzing pollutants and thermal desorption tail gas in the soil.
Example 4
In the embodiment, the preparation method of the MnFeO/C @ CaO catalytic material is as follows:
(1) crushing the straws into 5 mm, performing alkali treatment by using 1 mol/L NaOH solution, stirring for 3 hours at 80 ℃, filtering by using a filter screen, and washing by using deionized water until the pH value is neutral, and marking as a sample 1.
(2) Dropwise adding acetic acid into a 1 mol/L sodium chlorite solution to adjust the pH value of the solution to 4-5, then placing the sample 1 into the prepared sodium chlorite solution, stirring for 3 hours at 80 ℃, washing for 3 times by using deionized water to remove the sodium chlorite in the solution, and finally adding the deionized water to form a straw fiber suspension liquid with the pH value of 6.
(3) Adding 5 g/L calcium chloride into the straw fiber suspension according to the volume ratio of 1:3, adjusting the pH of the suspension to 7 by 1 mol/L sodium carbonate to form a straw fiber/calcium carbonate mixed solution, and filtering the mixed solution by using a filter screen to form a straw fiber/calcium carbonate mixture.
(4) Mixing the straw fiber/calcium carbonate mixture in N2And Ar and other inert gases are used for calcining for 2 h at 700 ℃ to form the biochar coated calcium oxide composite material C @ CaO.
(5) Manganese nitrate and ferric nitrate metal salt are mixed according to a molar ratio of Mn: and mixing Fe =1:2 to prepare a precursor solution.
(6) And (3) soaking C @ CaO in the precursor solution, and circularly operating according to a method of soaking for 2 h to 105 ℃ for drying until the load reaches 20 wt.%.
(7) C @ CaO loaded with Fe and Mn metals is added into N2And Ar and other inert gases are used for calcining for 2 h at 550 ℃ to form the MnFeO/C @ CaO catalytic material.
The prepared MnFeO/C @ CaO catalytic material is used for thermal desorption treatment of soil pollutants including petroleum hydrocarbon, phenanthrene and dichlorobiphenyl, wherein the concentration of the petroleum hydrocarbon is 1 mg/kg, the concentration of the phenanthrene is 1 mg/kg, and the concentration of the dichlorobiphenyl is 0.6 mg/kg.
The catalytic material is added in the following way: firstly stirring and mixing the MnFeO/C @ CaO catalytic material with contaminated soil according to the adding amount of 5 g/kg, then carrying out thermal desorption treatment on the soil mixed with the catalytic material at 450 ℃, and after the treatment is finished, detecting and analyzing pollutants and thermal desorption tail gas in the soil.
The removal rate of the pollutants in the soil after thermal desorption under different conditions is shown in fig. 1, and the removal rate of the pollutants in the thermal desorption tail gas under different conditions is shown in fig. 2.
Comparative experiment 1
And (3) carrying out thermal desorption treatment on the contaminated soil at 450 ℃ under the condition of no catalytic material addition, and detecting and analyzing the contaminants and thermal desorption tail gas in the soil after the treatment is finished.
Comparative experiment 2
The biochar material is prepared according to the method in the embodiment 1, marked as C, the material C is firstly stirred and mixed with contaminated soil according to the adding amount of 5 g/kg, then the soil mixed with the catalytic material is subjected to thermal desorption treatment at 450 ℃, and after the treatment is finished, pollutants and thermal desorption tail gas in the soil are detected and analyzed.
Comparative experiment 3
The C @ CaO composite material is prepared according to the method in the embodiment 2, the C @ CaO composite material is firstly stirred and mixed with polluted soil according to the adding amount of 5 g/kg, then the soil mixed with the catalytic material is subjected to thermal desorption treatment at 450 ℃, and after the treatment is finished, pollutants and thermal desorption tail gas in the soil are detected and analyzed.
Comparative experiment 4
The MnFeO catalytic material is prepared according to the method in the embodiment 3, firstly the MnFeO catalytic material is stirred and mixed with the polluted soil according to the adding amount of 5 g/kg, then the soil mixed with the catalytic material is subjected to thermal desorption treatment at 450 ℃, and after the treatment is finished, the pollutants and thermal desorption tail gas in the soil are detected and analyzed.
Comparative experiment 5
The MnFeO/C catalytic material is prepared according to the method in the embodiment 4, firstly the MnFeO/C catalytic material is stirred and mixed with the polluted soil according to the adding amount of 5 g/kg, then the soil mixed with the catalytic material is subjected to thermal desorption treatment at 450 ℃, and after the treatment is finished, the pollutants and thermal desorption tail gas in the soil are detected and analyzed.
The present invention is not limited to the above embodiments, and those skilled in the art can make various equivalent changes and substitutions without departing from the principle of the present invention after learning the content of the present invention, and these equivalent changes and substitutions should be considered as belonging to the protection scope of the present invention.
Claims (3)
1. A preparation method of a composite functional material for treating soil pollution is characterized by comprising the following steps: (1) crushing straws into 3 mm, performing alkali treatment by using 1 mol/L NaOH solution, stirring for 3 hours at 80 ℃, filtering by using a filter screen, and washing by using deionized water until the pH value is neutral, wherein the sample is marked as 1; (2) dropwise adding acetic acid into a 1 mol/L sodium chlorite solution to adjust the pH value of the solution to 4-5, then placing a sample 1 into the prepared sodium chlorite solution, stirring for 3 hours at 80 ℃, washing for 3 times by using deionized water to remove the sodium chlorite in the solution, and finally adding the deionized water to form a straw fiber suspension liquid with the pH value of 6; (3) adding 5 g/L calcium chloride into the straw fiber suspension according to the volume ratio of 2:1, adjusting the pH of the suspension to 7 by 1 mol/L sodium carbonate to form a straw fiber/calcium carbonate mixed solution, and filtering the mixed solution by using a filter screen to form a straw fiber/calcium carbonate mixture; (4) mixing the strawsFibre/calcium carbonate mixture in N2Or calcining the mixture for 2 hours at 800 ℃ under the protection of Ar gas to form a biochar coated calcium oxide composite material C @ CaO; (5) manganese nitrate and ferric nitrate metal salt are mixed according to a molar ratio of Mn: mixing Fe =1:2 to prepare a precursor solution; (6) dipping C @ CaO in the precursor solution, and circularly operating according to a dipping 2 h-105 ℃ drying method until the load reaches 15 wt%; (7) c @ CaO loaded with Fe and Mn metals is added into N2Or calcining for 2 h at 550 ℃ under the protection of Ar gas to form the MnFeO/C @ CaO catalytic material.
2. The MnFeO/C @ CaO catalytic material prepared by the preparation method of claim 1.
3. The MnFeO/C @ CaO catalytic material as set forth in claim 2 is used for simultaneous catalytic oxidation of volatile organic compounds by thermal desorption of soil.
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| CN113877598B (en) * | 2021-08-06 | 2023-12-08 | 南京工业大学 | Organic matter contaminated soil thermal desorption catalyst and preparation method thereof |
| CN113789175A (en) * | 2021-08-19 | 2021-12-14 | 桂林理工大学 | Preparation method and application of calcium carbonate biomass charcoal composite material |
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| CN103861598A (en) * | 2012-12-17 | 2014-06-18 | 南开大学 | Preparation of calcium-doped iron oxide hollow sphere and application of hollow sphere to catalytically oxidize chloro-substituted volatile organic compounds |
| CN105945049A (en) * | 2016-06-08 | 2016-09-21 | 北京神雾环境能源科技集团股份有限公司 | Restorative method and device for organic matter-heavy metal compound contaminated soil |
| CN107519860A (en) * | 2016-06-21 | 2017-12-29 | 康宁股份有限公司 | Manganese oxide catalyst, the integral catalyzer comprising the Mn oxide and their application |
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| CN109821569A (en) * | 2019-03-15 | 2019-05-31 | 深圳市力德环保工程有限公司 | A kind of honeycomb substrate catalyst and its preparation method and application |
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