CN111013534A - Intermediate-temperature biochar and preparation method and application thereof - Google Patents

Intermediate-temperature biochar and preparation method and application thereof Download PDF

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Publication number
CN111013534A
CN111013534A CN201911260908.5A CN201911260908A CN111013534A CN 111013534 A CN111013534 A CN 111013534A CN 201911260908 A CN201911260908 A CN 201911260908A CN 111013534 A CN111013534 A CN 111013534A
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biochar
temperature
pine
chlorobenzene
pine needle
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Inventor
晏井春
陈梦舫
钱林波
韩璐
陈云
杨磊
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Institute of Soil Science of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/722Oxidation by peroxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/485Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen

Abstract

A moderate temperature charcoal and a preparation method and application thereof are disclosed, wherein (1) pine needles of Korean pine are adopted as a biomass precursor, washed for 3-5 times by distilled water and then dried, and the pine needles are crushed and then put into a tube furnace; (2) in N2Under the protection condition, the temperature rise rate reaches 400-600 ℃ at 20-30 ℃/min, and the pine needle charcoal is obtained through cracking reaction for 8-10 h at the temperature; (3) mixing the aboveAnd washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle intermediate-temperature biochar. The invention utilizes the hole structure of the biochar, oxygen-containing groups such as carbonyl, carboxyl, hydroxyl, lactone group and the like which are rich on the surface and the self-sustaining free radical of the biochar to activate the peroxide, so that the secondary pollution of metal ions is effectively avoided while the active free radicals generated by the peroxide are efficiently activated to degrade organic pollutants.

Description

Intermediate-temperature biochar and preparation method and application thereof
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to intermediate-temperature biochar and a preparation method and application thereof.
Background
The biochar is porous carbon-rich solid produced by cracking biomass raw materials (such as pine needles, straws, rice hulls and the like) at a certain temperature (generally lower than 700 ℃) under the condition of oxygen limitation. After the foreign scholars put forward that the biochar can be used as a novel green repair material in 2006, the research on the biochar gradually draws the attention of a plurality of scholars at home and abroad.
As a carbon-rich layered porous material, the biochar has the characteristics of wide source, simple preparation, large specific surface area, rich pore structure and surface functional groups and the like. Many researchers have been successful for a long time in applying biochar to the adsorption of environmental pollutants. Recent studies have shown that the oxygen-containing groups such as carbonyl, carboxyl, hydroxyl and lactone groups, which are rich in the cavity structure and surface of biochar, can activate peroxides (hydrogen peroxide, H)2O2Or persulfates, Na2S2O8) Active free radicals are generated to degrade organic pollutants. In addition, the persistent free radicals of the biochar can also activate peroxides to generate active free radicals. The ability of the biochar to activate freely is related to the specific surface area, the content of functional groups, the number of cavities and other factors for preparing the biochar.
Therefore, aiming at the problem of secondary metal ion pollution caused by the traditional metal ion or metal solid material activated peroxide, the invention adopts medium-temperature preparation of the Korean pine needle biochar activated peroxide. Compared with other biomass precursors, the pine needle of the Korean pine has the advantages of wide sources and low price. In addition, the charcoal prepared from the Korean pine needles is weak in alkalinity (the pH value is 7.5-8.0), large in specific surface area and high in surface active free radical content, and has a layered pore structure and oxygen-containing functional groups such as carboxyl-COOH, carbonyl C = O and the like. The Korean pine needle biochar can effectively avoid secondary pollution of metal ions while efficiently activating peroxide to degrade organic pollutants.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the problem of secondary pollution of metal ions caused by the traditional peroxide activated by metal ions or metal solid materials, the invention provides the intermediate-temperature biochar and the preparation method and application thereof.
The technical scheme is as follows: a preparation method of intermediate-temperature biochar comprises the following steps: (1) taking Korean pine needles as a biomass precursor, washing the biomass precursor with distilled water for 3-5 times, drying the biomass precursor, crushing the pine needles, and putting the crushed pine needles into a tube furnace; (2) in N2Under the protection condition, the temperature rise rate reaches 400-600 ℃ at 20-30 ℃/min, and the pine needle charcoal is obtained through cracking reaction for 8-10 h at the temperature; (3) and (3) washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle intermediate-temperature biochar.
Preferably, the temperature of the drying is controlled at 60 ℃.
Preferably, in the step (1), the temperature increase rate is 20 ℃/min.
Preferably, in step (1), the cleavage temperature is 500 ℃.
The biochar prepared by the preparation method.
The application of the biochar prepared at the medium temperature in the preparation of products for adsorbing and degrading chlorobenzene, dioxane and trichloroethylene.
A product for removing organic pollutants comprises at least one of hydrogen peroxide or persulfate and the biochar as effective components.
Has the advantages that: (1) the method for preparing the intermediate-temperature biochar has the advantages of easily obtained raw materials, simplicity and controllable conditions; (2) a method for preparing intermediate temperature biochar has multiple cavity structures, oxygen-containing groups on the surface and high active free radical content; (3) the biochar activated peroxide prepared at the medium temperature degrades organic pollutants, the prepared biochar has excellent performance of adsorbing organic matters, and the organic pollutants can be rapidly degraded in the presence of the peroxide.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of biochar prepared at 500 ℃;
FIG. 2 is a graph of an infrared spectrum (FT-IR) of biochar prepared at 300-600 ℃;
FIG. 3 is a Raman spectrum (Raman) diagram of biochar prepared at 300-600 ℃;
FIG. 4 shows the preparation of a biochar Persistent Free Radical (PFR) at 300-600 deg.CS) Figure (a).
Detailed Description
The present invention will be described in detail with reference to the following specific examples. But the embodiments of the present invention are not limited thereto.
Example 1
And (3) taking 10 g of pine needles of the Korean pine, washing the pine needles with distilled water for 3-5 times, and drying the pine needles at 60 ℃. Pulverizing folium Pini, placing into a tube furnace, and heating in N2Under the protection condition, the temperature is raised to 400 ℃ at the temperature raising rate of 20 ℃/min, and the pine needle charcoal is obtained after the cracking reaction is carried out for 8 hours at the temperature. And (3) washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle biochar.
Chlorobenzene in the biochar-activated hydrogen peroxide degradation aqueous solution prepared in example 1:
20.0 mg of biochar with a lysis temperature of 400 ℃ was added to 20 mL of a chlorobenzene solution with a concentration of 20.0. mu. mol/L, and the initial solution pH of the above solution was adjusted to 4.0 with sulfuric acid. Stirring for 5 h at the room temperature of 25 ℃, adding 2 mol/L hydrogen peroxide after chlorobenzene is adsorbed and saturated, and continuing to react for 24 h. After the reaction, a certain amount of solution is taken, ethanol is added to quench the reaction, then the solution is filtered and separated, and the concentration of chlorobenzene in the solution is detected by adopting GC-MS.
The result shows that after chlorobenzene is adsorbed for 5 hours, the adsorption removal rate of the biochar with the cracking temperature of 400 ℃ to chlorobenzene is 37.0 percent; after hydrogen peroxide is added for reaction for 24 hours, the removal rate of the biochar to chlorobenzene with the cracking temperature of 400 ℃ is 64.3 percent.
Example 2
And (3) taking 10 g of pine needles of the Korean pine, washing the pine needles with distilled water for 3-5 times, and drying the pine needles at 60 ℃. Pulverizing folium Pini, placing into a tube furnace, and heating in N2Under the protection condition, the temperature rise rate reaches 500 ℃ at 25 ℃/min, and the pine needle charcoal is obtained after the cracking reaction is carried out for 9 h at the temperature. And (3) washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle biochar.
Chlorobenzene in the biochar-activated hydrogen peroxide degradation aqueous solution prepared in example 2:
20.0 mg of biochar with a cleavage temperature of 500 ℃ was added to 20 mL of a chlorobenzene solution with a concentration of 20.0. mu. mol/L, and the initial solution pH of the above solution was adjusted to 4.0 with sulfuric acid. Stirring for 5 h at the room temperature of 25 ℃, adding 2 mol/L hydrogen peroxide after chlorobenzene is adsorbed and saturated, and continuing to react for 24 h. After the reaction, a certain amount of solution is taken, ethanol is added to quench the reaction, then the solution is filtered and separated, and the concentration of chlorobenzene in the solution is detected by adopting GC-MS. Meanwhile, chlorobenzene adsorbed by the biochar extracted by normal hexane is detected by GC-MS (gas chromatography-mass spectrometry).
The result shows that after chlorobenzene is adsorbed for 5 hours, the adsorption removal rate of the biochar with the cracking temperature of 500 ℃ to chlorobenzene is 43.3 percent; after hydrogen peroxide is added for reaction for 24 hours, the removal rate of the biochar to chlorobenzene with the cracking temperature of 500 ℃ is 99.4 percent. The chlorobenzene concentration in n-hexane was not detected, indicating that chlorobenzene was completely degraded.
Example 3
And (3) taking 10 g of pine needles of the Korean pine, washing the pine needles with distilled water for 3-5 times, and drying the pine needles at 60 ℃. Pulverizing folium Pini, placing into a tube furnace, and heating in N2In the case of the protection,the temperature reaches 600 ℃ at the temperature rise rate of 30 ℃/min, and the pine needle biochar is obtained after the cracking reaction is carried out for 10 hours at the temperature. And (3) washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle biochar.
Chlorobenzene in biochar-activated hydrogen peroxide degradation aqueous solution prepared in example 3:
20.0 mg of biochar with a cleavage temperature of 600 ℃ was added to 20 mL of a chlorobenzene solution with a concentration of 20.0. mu. mol/L, and the initial solution pH of the above solution was adjusted to 4.0 with sulfuric acid. Stirring for 5 hours at the room temperature of 25 ℃, adding 2 mol/L hydrogen peroxide after chlorobenzene is adsorbed and saturated, and continuing to react for 24 hours. After the reaction, a certain amount of solution is taken, ethanol is added to quench the reaction, then the solution is filtered and separated, and the concentration of chlorobenzene in the solution is detected by adopting GC-MS.
The result shows that after chlorobenzene is adsorbed for 5 hours, the adsorption removal rate of the biochar with the cracking temperature of 600 ℃ to chlorobenzene is 50.7%; after hydrogen peroxide is added for reaction for 24 hours, the removal rate of the biochar to chlorobenzene with the cracking temperature of 600 ℃ reaches 66.5 percent.
Example 4
And (3) taking 10 g of pine needles of the Korean pine, washing the pine needles with distilled water for 3-5 times, and drying the pine needles at 60 ℃. Pulverizing folium Pini, placing into a tube furnace, and heating in N2Under the protection condition, the temperature rise rate reaches 500 ℃ at 30 ℃/min, and the pine needle charcoal is obtained after the cracking reaction is carried out for 8 hours at the temperature. And (3) washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle biochar.
Dioxane in aqueous biochar-activated sodium persulfate degradation solution prepared in example 4:
20.0 mg of biochar having a cleavage temperature of 500 ℃ was added to 20 mL of a 20.0. mu. mol/L dioxane solution, and the initial solution pH of the above solution was adjusted to 4.0 with sulfuric acid. Stirring the mixture for 5 hours at the room temperature of 25 ℃, adding 2 mol/L sodium persulfate after the dioxane is adsorbed and saturated, and continuing the reaction for 24 hours. After the reaction, a certain amount of solution is taken, ethanol is added to quench the reaction, then the solution is filtered and separated, and the concentration of chlorobenzene in the solution is detected by adopting GC-MS.
The result shows that after the dioxane is adsorbed for 5 hours, the adsorption removal rate of the biological carbon with the cracking temperature of 500 ℃ to the chlorobenzene is 8.8 percent; after sodium persulfate is added for reaction for 24 hours, the removal rate of the biochar to chlorobenzene with the cracking temperature of 500 ℃ reaches 53.5 percent.
Example 5
And (3) taking 10 g of pine needles of the Korean pine, washing the pine needles with distilled water for 3-5 times, and drying the pine needles at 60 ℃. Pulverizing folium Pini, placing into a tube furnace, and heating in N2Under the protection condition, the temperature rise rate reaches 500 ℃ at 30 ℃/min, and the pine needle charcoal is obtained after the cracking reaction is carried out for 10 h at the temperature. And (3) washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle biochar.
The biochar prepared in example 5 activates sodium persulfate to degrade trichloroethylene in aqueous solution:
20.0 mg of biochar with a lysis temperature of 500 ℃ was added to 20 mL of 20.0. mu. mol/L trichloroethylene solution, and the initial solution pH of the above solution was adjusted to 4.0 with sulfuric acid. Stirring for 5 h at the room temperature of 25 ℃, adding 2 mol/L sodium persulfate after the trichloroethylene is adsorbed and saturated, and continuing to react for 24 h. After the reaction, a certain amount of solution is taken, ethanol is added to quench the reaction, then the solution is filtered and separated, and the concentration of chlorobenzene in the solution is detected by adopting GC-MS.
The result shows that after the trichloroethylene is adsorbed for 5 hours, the adsorption removal rate of the biochar with the cracking temperature of 500 ℃ to the chlorobenzene is 44.8 percent; after sodium persulfate is added for reaction for 24 hours, the removal rate of the chlorobenzene by the biochar with the cracking temperature of 500 ℃ reaches 100 percent.
TABLE 1 preparation of biochar activated peroxide for degradation of organic contaminants at different cracking temperatures
Temperature of cracking of biochar Oxidizing agent Contaminants Adsorption removal rate Degradation removal rate
400 ℃ Hydrogen peroxide Chlorobenzene 37.0% 64.3%
500 ℃ Hydrogen peroxide Chlorobenzene 43.3% 99.4%
600 ℃ Hydrogen peroxide Chlorobenzene 50.7% 66.5%
500 ℃ Sodium persulfate Dioxane (dioxane) 8.8% 53.5%
500 ℃ Sodium persulfate Trichloroethylene 44.8% 100%

Claims (7)

1. A preparation method of intermediate-temperature biochar is characterized by comprising the following steps: (1) taking Korean pine needles as a biomass precursor, washing the biomass precursor with distilled water for 3-5 times, drying the biomass precursor, crushing the pine needles, and putting the crushed pine needles into a tube furnace; (2) in N2Under the protection condition, the temperature rise rate reaches 400-600 ℃ at 20-30 ℃/min, and the pine needle charcoal is obtained through cracking reaction for 8-10 h at the temperature; (3) and (3) washing the prepared pine needle biochar with distilled water for 3-5 times until the pH value is neutral, and filtering and drying to obtain the pine needle intermediate-temperature biochar.
2. The method for preparing mesophilic biochar according to claim 1, characterized in that the temperature of the drying is controlled at 60 ℃.
3. The method for preparing mesophilic biochar according to claim 1, characterized in that in step (1), the temperature rise rate is 20 ℃/min.
4. The method for preparing mesophilic biochar according to claim 1, characterized in that in step (1), the cracking temperature is 500 ℃.
5. Biochar produced by the production method according to any one of claims 1 to 4.
6. The use of the intermediate-temperature biochar preparation method in claim 5 in preparation of adsorptive degradation products of chlorobenzene, dioxane and trichloroethylene.
7. A product for removing organic pollutants, which is characterized in that the active ingredients are at least one of hydrogen peroxide or persulfate and the biochar as claimed in claim 5.
CN201911260908.5A 2019-12-10 2019-12-10 Intermediate-temperature biochar and preparation method and application thereof Pending CN111013534A (en)

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