CN114832778A - Shaddock peel biochar for adsorbing arsenic as well as preparation method and application thereof - Google Patents
Shaddock peel biochar for adsorbing arsenic as well as preparation method and application thereof Download PDFInfo
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- CN114832778A CN114832778A CN202210541375.3A CN202210541375A CN114832778A CN 114832778 A CN114832778 A CN 114832778A CN 202210541375 A CN202210541375 A CN 202210541375A CN 114832778 A CN114832778 A CN 114832778A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides shaddock peel biochar for adsorbing arsenic as well as a preparation method and application thereof, wherein the preparation method comprises the steps of sequentially carrying out pretreatment, solid-phase carbonization and grinding on shaddock peel. According to the technical scheme, the shaddock peel biochar obtained by carbonizing and grinding the shaddock peel in a solid phase comprises a biochar body and particles attached to the surface of the biochar body, wherein the particle size of the particles is 200-400 nm, and the particles are small in nano size and high in adsorption performance. In addition, the shaddock peel biochar has high content of metals such as potassium, calcium and the like, has a good adsorption and fixation effect on trivalent arsenic, and can be applied to remediation of arsenic pollution in water and soil environments.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of agricultural wastes, in particular to soil heavy metal pollution remediation, and further relates to a preparation method of shaddock peel biochar for adsorbing arsenic, the shaddock peel biochar and application thereof.
Background
Arsenic (As) is a metal element widely distributed in nature. Arsenic is often present in soils in the form of compounds, the most predominant of which are inorganic arsenic (III) and arsenic (V) compounds. As pollution to paddy field soil and long-term flooding cultivation obviously increase the bioavailability of As, often resulting in the over-standard content of inorganic As in rice. In China Hunan, Guangxi, Yunnan, Guizhou, Sichuan and other major rice production areas, the overproof rate of inorganic arsenic of rice is as high as 40-60%. Inorganic arsenic is a known carcinogen in humans, and chronic exposure to low levels of arsenic increases the risk of various cancers, diabetes and cardiovascular diseases, seriously threatening the health of our country. With the concern on health problems caused by inorganic arsenic pollution of rice, the treatment of arsenic-polluted rice fields becomes a task which is urgently needed to be solved in the field of environmental protection.
At present, the common chemical methods for treating the arsenic-polluted soil comprise a fixation method, a leaching method, an electric remediation method and the like. Among them, the immobilization method is a technique of adsorbing or precipitating contaminants in soil by using an immobilizing agent, thereby reducing potential risks caused by excessive contaminants in soil. The core of the immobilization method is the selection and preparation of the immobilizing agent. The existing arsenic removal fixing agent comprises iron oxide, lime, solid waste and the like. These materials are costly to produce, or alter soil properties, or carry other contaminants that increase health risks. At present, the biochar material in the natural fixing agent has the advantages of low preparation cost and ecological environmental protection, but the capacity of adsorbing arsenic is limited generally.
The biochar is obtained by utilizing waste such as straws and the like to pyrolyze and burn under the anoxic or anaerobic condition, and has the characteristics of large specific surface area, high porosity, strong adsorbability and stable chemical property. The biochar not only can perform the functions of passivation and restoration on pollutants in soil, but also can fix carbon, reduce emission and improve the soil environment. In recent years, biochar is popular among students as a carrier or an adsorbent commonly used for treating arsenic pollution of soil. However, all biochar with better adsorption effect is modified biochar, and the modifying substance rather than the biochar plays a role. This not only increases the number of steps in the manufacturing process, but also increases the cost and technical difficulty.
The white pulp structure of the shaddock peel is white cotton flocculent, has more pores, has a large amount of white tendons and rich nutrient substances, has rough surface of the shaddock peel, and is a good raw material for preparing the active carbon. At present, there are also reports on the adsorption of heavy metal ions such as zinc, cadmium, lead, copper and the like by performing hydrothermal carbonization on shaddock peel to obtain the shaddock peel biochar. However, the chemical forms of arsenic as a metalloid element and heavy metal ions such as zinc, cadmium, lead, and copper are different, and the effect of biochar is different, and thus the biochar of shaddock peel cannot achieve a good effect of adsorbing arsenic.
Disclosure of Invention
Based on the problems, the invention aims to provide a preparation method of shaddock peel biochar, the shaddock peel biochar and application thereof, wherein the shaddock peel biochar has a good adsorption effect on arsenic, particularly trivalent arsenic, and is well suitable for remediation of soil arsenic pollution.
In order to achieve the above purpose, the first aspect of the invention provides a preparation method of shaddock peel biochar for adsorbing arsenic, which comprises the steps of sequentially carrying out pretreatment, solid-phase carbonization and grinding on shaddock peel.
According to the technical scheme, the shaddock peel biochar can be obtained by carbonizing and grinding the shaddock peel in a solid phase mode, a large number of particles are attached to the surface of a biochar body obtained by carbonizing in the solid phase mode, the particles can be formed by carbonizing a white pulp structure of the shaddock peel in the solid phase mode, and the particles are small in nano size and high in adsorption performance. In addition, the shaddock peel biochar has high content of metals such as potassium, calcium and the like, can generate electrostatic adsorption on trivalent arsenic, has a good adsorption and fixation effect, and can be applied to remediation of arsenic pollution in water and soil environments. The method utilizes agricultural waste shaddock peel to prepare the charcoal adsorbent with particles on the surface by a simple and rapid solid-phase carbonization method, fully utilizes resources, reduces environmental pollution, has good economic benefit and is beneficial to industrial production.
Preferably, the pre-treatment comprises naturally air-drying and crushing the shaddock peel.
Preferably, the granularity of the crushed shaddock peel by the belt screen crusher is 60 meshes.
Preferably, the temperature of the solid-phase carbonization is 300-700 ℃, and the time is 1-3 h.
Preferably, the solid-phase carbonization is carried out in a muffle furnace, and the temperature rise rate is 8-15 ℃/min.
The pomelo peel biochar comprises a biochar body and particulate matters attached to the surface of the biochar body, wherein the particle size of the biochar body is 800-2700 nm, and the particle size of the particulate matters is 200-400 nm. The nano-size of the particles obtained by the method has stronger adsorption capacity on arsenic, and more importantly, the particles have better adsorption effect on trivalent arsenic.
The third aspect of the invention provides application of the shaddock peel biochar, wherein the shaddock peel biochar is added into arsenic-containing soil or water sample to be mixed and subjected to adsorption treatment. The invention can repair arsenic pollution in water and soil by using the shaddock peel biochar with particles on the surface.
Preferably, the ratio of the weight/g of the arsenic-containing soil to the weight/g of the shaddock peel biochar is 100: 1-3.
Preferably, the arsenic in the arsenic-containing soil is trivalent arsenic.
Drawings
FIG. 1 is an SEM photograph of the biochar from the shaddock peel in example 1.
FIG. 2 is the result of particle size distribution of the shaddock peel biochar in example 1 measured using a Zeta instrument.
FIG. 3 shows the results of NMR measurement of the shaddock peel charcoal in example 1.
FIG. 4 is the adsorption isotherm of the biochar from shaddock peel for arsenic adsorption in example 2.
FIG. 5 shows the result of arsenic adsorption by the shaddock peel biochar in example 3.
Detailed Description
The shaddock peel biochar can be used for arsenic adsorption in arsenic-containing soil or water samples, and is particularly suitable for adsorption of trivalent arsenic. And when the adsorption is carried out, the shaddock peel biochar is added into the arsenic-containing soil or water sample for adsorption treatment. Wherein the ratio of the weight/g of the arsenic-containing soil to the weight/g of the shaddock peel biochar is 100: 1-3, and more preferably, the ratio of the weight/g of the arsenic-containing soil to the weight/g of the shaddock peel biochar is 100: 3.
The preparation method of the shaddock peel biochar comprises the steps of sequentially carrying out pretreatment, solid-phase carbonization and grinding on shaddock peel.
Wherein the pretreatment comprises naturally air drying and pulverizing pericarpium Citri Grandis, and in the specific operation, the pericarpium Citri Grandis can be naturally air dried and then pulverized, or pulverized and then naturally air dried. The temperature of natural air drying is 25-40 ℃, namely, the air drying is carried out at room temperature, the drying time is 5-7 d, preferably, the natural air drying is carried out at 25 ℃, and the drying time is 7 d. The granularity of the crushed shaddock peel by a crusher with a screen is 60 meshes.
And (3) carrying out solid-phase carbonization in a muffle furnace, wherein the temperature rise rate is 8-15 ℃/min, and preferably 10 ℃/min. The temperature of the solid-phase carbonization is 300-700 ℃, and the time is 1-3 h. Preferably 500 ℃ and 2 h. During the solid-phase carbonization process, the shaddock peel is firstly placed in a closed ceramic tank and then placed in a muffle furnace for carbonization.
Grinding the shaddock peel after solid-phase carbonization, and sieving by a 2mm sieve. The shaddock peel biochar obtained after grinding comprises a biochar body and particles attached to the surface of the biochar body, the particle size of the biochar body is 800-2700 nm, and the particle size of the particles is 200-400 nm.
To better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples. It should be noted that the following implementation of the method is a further explanation of the present invention, and should not be taken as a limitation of the present invention.
Example 1 preparation of shaddock peel biochar
Naturally air drying pericarpium Citri Grandis at 25 deg.C for 7d, pulverizing to 60 mesh with a sieve pulverizer, and placing in a sealed ceramic jar. And (3) placing the ceramic pot in a muffle furnace, heating the muffle furnace to 500 ℃ at a speed of 10 ℃/min, and carrying out solid-phase carbonization reaction on the shaddock peel for 2 h. After the carbonization reaction, grinding and crushing the mixture until the mixture passes through a sieve of 2mm to obtain the shaddock peel biochar. SEM and Zeta appearance test are carried out to shaddock peel biochar, and its result is shown respectively in FIG. 1 and FIG. 2, and the particle size distribution of biochar body is 800 ~ 2700nm, and its surface adheres to there is the particulate matter, and the particle size distribution of particulate matter is 200 ~ 400 nm. The results of NMR test and elemental analysis of the shaddock peel biochar are shown in fig. 3 and table 1, respectively, and the shaddock peel biochar mainly contains carbon, oxygen, potassium, calcium and other elements on the surface, has functional groups such as hydroxyl, carboxyl, carbonyl and the like, and can adsorb trivalent arsenic through electrostatic adsorption, hydrogen bond formation and other actions. In addition, metal cations such as potassium and calcium are favorable for forming a complex compound with particles on the surface of the shaddock peel biochar and trivalent arsenic, and the trivalent arsenic is further adsorbed.
TABLE 1 elemental analysis of shaddock peel biochar
Example 2 adsorption of shaddock peel biochar on arsenic in aerobic water sample
And (2) soaking part of the shaddock peel biochar obtained in the example 1 in deionized water for 24 hours, stirring at regular time, filtering, drying the solid component obtained by filtering at 60 ℃ for 48 hours to obtain the shaddock peel biochar with surface particles removed.
Firstly, water samples of As (III) and As (V) with certain concentrations are prepared respectively. 0.05g of the shaddock peel Biochar (BC) obtained in example 1 and 0.05g of the shaddock peel biochar (SCBC) with surface particles removed are weighed into 50mL centrifuge tubes respectively, 25mL of As (III) and As (V) water samples are accurately weighed into the centrifuge tubes respectively, a water bath oscillator is placed into the centrifuge tubes after a cover is covered, the water bath oscillator is vibrated for 24h at the water temperature of 25 ℃ and 180r/min, and the filtration is carried out.
The concentrations of the obtained filtrate and the prepared As (III) and As (V) water sample solutions were measured by an Atomic Fluorescence Spectrometer (AFS), and the adsorption amount was calculated from the difference between the arsenic concentrations before and after adsorption, and the results are shown in Table 2.
As can be seen from the results, the adsorption capacity of the shaddock peel biochar to the As (III) water sample is 1365 mug/g, and the adsorption capacity to the As (V) water sample is only 54 mug/g. The adsorption capacity of the shaddock peel biochar after surface particles are removed to an As (III) water sample is 491 mug/g, and the adsorption capacity to an As (V) water sample is only 55 mug/g. The comparison of the two results shows that the shaddock peel biochar prepared by the invention has good arsenic adsorption performance, especially good trivalent arsenic adsorption performance, and probably because the particle size of particles on the surface of the biochar body is small, the nano-size effect is achieved, the shaddock peel is ground after solid-phase carbonization without being cleaned and filtered, and the obtained shaddock peel biochar has high adsorption performance on As (III), which is related to the fact that the shaddock peel biochar has more particles on the surface. The adsorption of As (III) by the shaddock peel biochar conforms to the Langmuir adsorption mode, and the result is shown in FIG. 4, and the adsorption is presumed to be monomolecular adsorption according to FIG. 4.
TABLE 2 adsorption results of arsenic in water samples
| 25ml water sample | As(III) | As(V) |
| 0.05g of adsorption amount after BC treatment | 1365μg/g | 54μg/g |
| 0.05g of the adsorption amount after SCBC treatment | 491μg/g | 55μg/g |
(Note: μ g/g is arsenic adsorbed per g of particulate matter)
Example 3 adsorption of shaddock peel biochar on arsenic in anaerobic soil
The influence of shaddock peel biochar on the adsorption of arsenic in anaerobic soil is researched by simulating the microenvironment of flooded rice field soil.
The specific operation can be as follows: 7.0g each of arsenic contaminated paddy field soil was weighed into two 100mL penicillin bottles. Then, 0.21g of the grapefruit peel charcoal of example 1 was added to one vial, and the other vial was used as a blank. 70mL of PIPES buffer solution were added to each of the solutions to a final concentration of 30mM and pH 7.3. Finally, lactic acid is respectively added as a carbon source for the growth and the propagation of the microorganisms, and the final concentration of the lactic acid is 10 mM. And (3) filling nitrogen into each penicillin bottle, covering the penicillin bottle with a cover, and performing anaerobic dark culture at the temperature of 30 ℃. Taking supernatant of each penicillin bottle reaction solution by using a disposable syringe, filtering by using a filter head with the diameter of 0.45 mu m, and placing in a centrifuge tube to be added with nitric acid for preservation. The form of arsenic in the solution was measured by AFS to determine the effect of the shaddock peel biochar on the adsorption of arsenic in the paddy soil, and the results are shown in FIG. 5. As shown in FIG. 5, the concentration of As (III) in the aqueous solution was reduced by 21.5 to 22.2% in the cases of the treatment with the addition of the shaddock peel biochar at 16 th and 20 th days of anaerobic culture, as compared with the blank control without the addition of the shaddock peel biochar.
The raw material of the invention is shaddock peel, and the preparation process is simple. At present, the annual output of the grapefruits in China is about 2000 million tons, and the grapefruit peel is utilized, so that the waste treatment cost can be reduced. The shaddock peel is used as a raw material for preparing the biochar, is applied to arsenic remediation of polluted water and soil, changes waste into valuable, is economical and feasible, is beneficial to industrial production, and has important environmental significance and application value.
Finally, it should be noted that the above examples are only for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, the present invention is not limited to the examples, and those skilled in the art should understand that the technical solutions of the present invention, such as the preparation process parameters of the shaddock peel biochar, etc., can be modified or equivalently replaced without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of shaddock peel biochar for adsorbing arsenic is characterized by comprising the steps of sequentially carrying out pretreatment, solid-phase carbonization and grinding on shaddock peel.
2. The method for preparing pomelo peel biochar for adsorbing arsenic as recited in claim 1, wherein the pre-treatment comprises natural air drying and crushing of the pomelo peel.
3. The preparation method of the shaddock peel biochar for adsorbing arsenic as recited in claim 2, wherein the granularity of the shaddock peel after being crushed by a crusher with a sieve is 60 meshes.
4. The preparation method of the shaddock peel biochar for adsorbing arsenic as recited in claim 1, wherein the temperature of the solid-phase carbonization is 300-700 ℃ and the time is 1-3 h.
5. The preparation method of the shaddock peel biochar for adsorbing arsenic as claimed in claim 1, wherein the solid-phase carbonization is carried out in a muffle furnace, and the temperature rise rate is 8-15 ℃/min.
6. The method for preparing the shaddock peel biochar for adsorbing arsenic as recited in claim 1, wherein the shaddock peel after being carbonized in a solid phase can be sieved by a 2mm sieve after being ground.
7. The shaddock peel biochar prepared by the preparation method for the shaddock peel biochar for adsorbing arsenic as claimed in any one of claims 1 to 6, wherein the biochar comprises a biochar body and particles attached to the surface of the biochar body, the particle size of the biochar body is 800-2700 nm, and the particle size of the particles is 200-400 nm.
8. The use of the shaddock peel biochar as recited in claim 7, wherein the shaddock peel biochar is added to arsenic-containing soil or a water sample to be mixed and subjected to adsorption treatment.
9. The application of the shaddock peel biochar as recited in claim 8, wherein the ratio of the weight/g of the arsenic-containing soil to the weight/g of the shaddock peel biochar is 100: 1-3.
10. The use of the shaddock peel biochar as recited in claim 8, wherein the arsenic in the arsenic-bearing soil is trivalent arsenic.
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Cited By (3)
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| CN115475603A (en) * | 2022-09-14 | 2022-12-16 | 桂林理工大学 | Preparation method and application of shaddock peel biochar/MgFe-LDH composite material |
| CN115925210A (en) * | 2022-12-26 | 2023-04-07 | 华中科技大学 | Method for preparing sludge-based biochar and reducing heavy metal toxicity |
| CN116237014A (en) * | 2023-02-13 | 2023-06-09 | 广州大学 | Regulating and controlling method and evaluating method for toxicity of arsenic and copper based on acidified biochar |
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| CN115925210A (en) * | 2022-12-26 | 2023-04-07 | 华中科技大学 | Method for preparing sludge-based biochar and reducing heavy metal toxicity |
| CN116237014A (en) * | 2023-02-13 | 2023-06-09 | 广州大学 | Regulating and controlling method and evaluating method for toxicity of arsenic and copper based on acidified biochar |
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