CN112897503A - Acid modification preparation method of biomass charcoal material with toluene adsorption effect - Google Patents

Acid modification preparation method of biomass charcoal material with toluene adsorption effect Download PDF

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CN112897503A
CN112897503A CN202110095678.2A CN202110095678A CN112897503A CN 112897503 A CN112897503 A CN 112897503A CN 202110095678 A CN202110095678 A CN 202110095678A CN 112897503 A CN112897503 A CN 112897503A
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biochar
acid
biomass charcoal
charcoal material
acid modification
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段方蕾
郑晓涵
孙尚
袁明
陈东辉
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Shanghai Institute of Technology
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    • 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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    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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Abstract

The invention relates to an acid modification preparation method of a biomass charcoal material with toluene adsorption, which is characterized by comprising the following steps: washing the surface of the rice hull by deionized water, and drying to finish pretreatment; placing the pretreated rice hulls in a tubular furnace, and carbonizing under the protection of inert gas; grinding and sieving the carbonized rice hulls to obtain biochar, putting the biochar in sulfuric acid, continuously stirring and soaking for 6-12 h to form a microporous structure with a specific size range in the biochar, and attaching oxygen-containing functional groups in the microporous structure to obtain an acid modified precursor; and washing, filtering and drying the acid modified precursor to obtain the acid modified rice hull biochar. Compared with the prior art, the invention can obtain the biochar material with rich micropores, improved surface oxygen-containing functional groups and good toluene adsorption performance by the specific acid modification preparation method and the adjustment of process parameters.

Description

Acid modification preparation method of biomass charcoal material with toluene adsorption effect
Technical Field
The invention relates to a preparation method of an adsorption material, in particular to an acid modification preparation method of a biomass charcoal material with toluene adsorption.
Background
The biochar is a group of carbon materials formed by slowly pyrolyzing biomass in an inert atmosphere, is a highly aromatic carbon-rich solid product obtained by pyrolysis of a biomass raw material in a closed environment with limited oxygen supply at a high temperature, is rich in carbon-containing materials such as agricultural and forestry wastes, municipal sludge, fruit byproducts and the like, and can be used for biochar production. The biochar has the characteristics of multiple pores, large specific surface area, stable property and strong cation exchange capacity, and thus has a wide application prospect in the aspect of adsorption of organic pollutants in the air.
VOCs (volatile organic compounds) are a general term for volatile organic compounds discharged into the atmosphere by various human activities and biological metabolism, have the characteristics of low boiling point, strong reactivity and the like, are one of main reasons for forming haze weather, and greatly threaten human health and natural environment. VOCs are from many sources, and most of the VOCs come from the volatilization of organic solvents, such as automobile coating, home painting, printing and coating and the like. Certain chemicals such as benzene, toluene and halogenated carbon halogenated olefin contained in the natural gas not only can cause serious pollution to the atmospheric environment, but also can cause potential threats to human health due to the irritation and headache of eyes and respiratory tracts after a human body inhales the polluted gas.
The improper treatment of the biomass waste not only wastes resources, but also can pollute the environment, and the waste biomass is converted into the biochar to be applied to environment restoration and pollution treatment, so that the reasonable treatment and resource utilization of the biomass can be realized, and the aim of treating wastes with processes of wastes against one another can be fulfilled. Therefore, how to develop a biochar capable of efficiently adsorbing toluene in large-scale production is a technical problem which needs to be solved urgently.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an acid modification preparation method of a biomass charcoal material with toluene adsorption function, and the biomass charcoal material with rich micropores, improved surface oxygen-containing functional groups and good toluene adsorption performance can be obtained by the specific acid modification preparation method and the adjustment of process parameters.
The basis of the research and development of the invention is as follows: the biochar is combined with other materials, and is subjected to modification treatment by physical, chemical or biological methods, so that the physical, chemical and biological characteristics (specific surface area, porosity, cation exchange capacity, surface functional groups, pH and the like) can be improved, the adsorption capacity is greatly improved, and the chemical treatment usually comprises H2O2Or carrying out biochar modification on the acid and the alkali.
The biochar generated by carbonization in the invention is an unordered basic graphite microcrystal, has a basic pore structure, has an undeveloped pore structure, limits the adsorption capacity of the biochar on VOCs, and can greatly improve the physical and chemical properties of the biochar through physical or chemical modification. The specific surface area, chemical functional groups and pore structures of the VOCs adsorbent are adjusted by the modification technology, the adsorption performance of the VOCs adsorbent is improved, and the modified biochar can become a widely-applied adsorption material with low cost, convenient preparation method and high adsorption efficiency in an atmospheric pollution control project.
The purpose of the invention can be realized by the following technical scheme:
the acid modification preparation method of the biomass charcoal material with toluene adsorption function comprises the following steps:
s1: washing the surface of the rice hull by deionized water, and drying to finish pretreatment;
s2: placing the pretreated rice hulls in a tubular furnace, and carbonizing under the protection of inert gas;
s3: grinding and sieving the carbonized rice hulls to obtain biochar, putting the biochar in sulfuric acid, continuously stirring and soaking for 6-12 h to form a microporous structure with a specific size range in the biochar, and attaching oxygen-containing functional groups in the microporous structure to obtain an acid modified precursor;
s4: and washing, filtering and drying the acid modified precursor to obtain the acid modified rice hull biochar.
Further, the mass concentration of the biochar in the sulfuric acid in S3 is 10 g/L.
Further, the mass fraction of the sulfuric acid in the S3 is 20-90%.
Further, the microporous structure in S3 is a three-dimensional through-hole or pore structure having a pore size of 15 to 500nm, which is locally through or globally through.
Further, the drying process in S1 and S4 is carried out at the temperature of 80-105 ℃.
Further, the inert gas is firstly introduced into S2 for 15-20min, and then the temperature is raised for carbonization.
Further, the inert gas introduced in S2 is one or more of nitrogen, helium, neon, argon, krypton, or xenon.
Further, in the carbonization process in S2, the temperature rising speed is 2-10 ℃/min, the carbonization temperature is 500-700 ℃, and the heat preservation time is 1-3 h.
Further preferably, the carbonization temperature is 700 ℃.
Further, sieving in S3 to obtain 80-100 mesh biochar particles.
Further, the washing process in S4 is to soak with 1-5M NaOH and wash to neutrality.
Compared with the prior art, the invention has the following technical advantages:
1. the invention takes the biochar material as the carbon source, greatly reduces the preparation cost of the adsorbing material, does not cause secondary pollution at the same time, and plays a role in environmental protection.
2. The acid modified biochar can change the aperture, and the modified biochar has rich microporous structure and larger specific surface area (85-95 m)2·g-1) On one hand, the method is beneficial to physical adsorption, on the other hand, the contact sites of chemical adsorption are increased, and the adsorption capacity of the acid modified carbon for hydrophobic volatile organic compounds such as toluene and the like is obviously increased.
3. In the process of preparing the biochar, organic substances in the raw materials can generate rich oxygen-containing functional groups on the surface of the biochar, such as carboxyl, weak acid, phenolic hydroxyl and the like, and the oxygen-containing functional groups play an important role in the process of adsorbing the biochar.
4. The biological carbon modified by sulfuric acid can promote the surface of the biological carbon to form more oxygen-containing functional groups in the modification process, and the content of acid groups of the biological carbon is increased compared with that of the biological carbon which is not modified, so that the adsorption of toluene is influenced. The acid activates the surface of the biochar, increases the active sites of the biochar, and simultaneously, the sulfuric acid has high neutralization degree on basic groups in the material and oxidizes part of unstable functional groups.
5. The modified biochar is used for adsorbing VOCs, so that the application range of the biochar material is expanded, the utilization rate of the biochar is improved, and the adsorption rate of the VOCs is enhanced on the original basis. The preparation of the biochar with high adsorption capacity and stable property has important significance in the field of VOCs gas adsorption and the field of environmental remediation.
6. The biomass material prepared by the invention has potential application value in the fields of adsorption, electrode materials, separation, sensing, gas storage, catalyst carriers and the like, has great market significance for the application of biochar, and improves the application of environment-friendly materials in the field of environmental engineering.
Drawings
FIG. 1 is a penetration curve of acid-modified biochar material for dynamic adsorption of toluene;
fig. 2 is an electron micrograph of the resulting acid-modified biochar material.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1:
(1) washing the high rice hulls with deionized water, drying the high rice hulls in an oven at 80 ℃ for 12 hours, then putting the rice hulls into a crucible, sending the rice hulls into a tube furnace, introducing high-purity nitrogen, setting the nitrogen flow rate to be 100mL/min, continuing for 15-20min, exhausting air in the tube furnace, finally setting the program temperature rise to 500 ℃, setting the temperature rise rate to be 1-5 ℃/min, preserving heat for 1-3 hours, performing pyrolysis carbonization, and naturally cooling to room temperature. Grinding the carbonized rice hull with a mortar grinding rod, then sieving, and taking 80-100 meshes as 500DK for later use.
(2) The temperature was programmed to 600 ℃ as in step (1), and recorded as 600DK for future use.
(3) The temperature was programmed to 700 ℃ as in step (1), and recorded as 700DK for future use.
The experimental gas source is generated by adopting a dynamic gas distribution method, namely toluene gas is prepared by a bubbling method. And high-purity nitrogen is used as carrier gas, wherein one path of high-purity nitrogen passes through a bubbler filled with toluene liquid, the other path of high-purity nitrogen is used as diluent gas and directly introduced into a mixing tank, and finally, the two paths of gases are uniformly mixed in the mixing tank. The bubbler is placed in a constant-temperature ice-water bath, a 3mm stainless steel pipe is adopted as a gas circulation pipeline of the whole system, and the temperature is kept at 60 ℃. The initial concentration of toluene was controlled by controlling the gas flow rate into the bubbler and the gas flow rate of the dilution gas by adjusting a gas mass flow Meter (MFC). The mixed gas passes through a U-shaped pipe filled with an adsorbent to achieve the purpose of carrying out an adsorption experiment, finally, the gas after adsorption directly enters a Gas Chromatography (GC) for analysis and detection, the concentration of toluene is 4mg/L, 3 groups of experiments are carried out on the material, the average of 3 groups of the absorption penetration time and the absorption saturation time is taken, and the measured results are shown in table 1.
TABLE 1
Figure BDA0002913818390000041
Experimental data show that the rice hull biochar adsorption effect at 700 ℃ is good, probably because the specific surface area of the biochar is increased due to the increase of the pyrolysis temperature, meanwhile, the aromaticity of the biochar is improved through high-temperature pyrolysis, and the adsorption of the biochar to VOCs is promoted.
700DK was found to be the best acid modified material to adsorb toluene in conjunction with the overall experimental system.
(1) H with the mass concentration fraction of 98%2SO4(density 1.84) diluting with distilled water to obtain H with mass concentration fractions of 20%, 40%, 70% and 90%2SO4A solution;
(2) modifying 700DK obtained in the step (3) with sulfuric acid with different concentrations for 6H, and mixing 700DK with H2SO4Mixing and soaking, wherein the mass concentration of the biochar is 10g/L, and mechanically stirring the beaker on a magnetic stirrer at the rotating speed of 30 r/min.
(3) And soaking the biochar obtained after acidification in 1-5M NaOH, washing until the biochar is neutral, performing suction filtration, and drying at 80 ℃ for 12h to obtain acid modified biomass carbon, wherein the acid modified biomass carbon is respectively marked as 700DK2006, 700DK4006, 700DK7006 and 700DK 9006. 700DK2006 shows that 700 degree rice hull biological carbon material passes through 20% H2SO4Acidifying for 6h to obtain the biochar acid modified material.
(4) And (4) placing 0.05g of the adsorbing material obtained in the step (3) in a U-shaped tube for an adsorption experiment to obtain a biochar dynamic adsorption toluene penetration curve as shown in the attached figure 1. It can be seen from FIG. 1 that H is added to the biochar material as it is acidified2SO4The concentration is increased, the adsorption penetration time of the acidified biochar to toluene is obviously prolonged, the adsorption penetration time reflects the effect of the adsorbing material to a certain extent, the longer the penetration time is, the better the adsorption effect is, the oxygen functional group introduced by acid enhances chemical adsorption, and the adsorption rate of the adsorbent is improved. The 700DK7006 adsorption material is prepared under the optimal condition in consideration of production cost and adsorption efficiency. Fig. 2 is an electron microscope photograph of the acid-modified biochar material, and it is seen from fig. 2 that the biochar has a rough surface and a poor porosity, and after acid modification, the biochar has been broken and collapsed on the surface layer to different degrees, and the collapse of the acid-modified biochar is observed to be half-penetrated to penetrated, and is not uniformly distributed, and is accompanied by collapse of a larger area. This shows that acid modification has an influence on the structure of the biochar, and the original physicochemical properties of the biochar are influenced to a certain extent.
Example 2:
(1) same as in step (1) in example 1;
(2) 700DK obtained in example 1 was modified with sulfuric acid at different concentrations for 12H, and 700DK and H were added2SO4Mixing and soaking, wherein the mass concentration of the biochar is 10g/L, and mechanically stirring the beaker on a magnetic stirrer at the rotating speed of 30 r/min.
(3) And soaking the biochar obtained after acidification in 1-5M NaOH, washing until the biochar is neutral, performing suction filtration, and drying at 80 ℃ for 12 hours to obtain acid modified biomass carbon, wherein the acid modified biomass carbon is respectively marked as 700DK2012, 700DK4012, 700DK7012 and 700DK 9012. 700DK2006 shows that 700 degree rice hull biological carbon material passes through 20% H2SO4Acidifying for 12h to obtain the biochar acid modified material.
(4) And (3) placing 0.05g of the adsorbing material obtained in the step (3) in a U-shaped pipe for an adsorption experiment, and finding that the adsorption efficiency of the acid-modified biochar material for toluene after 12 hours is obviously lower than that of the acid-modified biochar material after 6 hours.
(5) Performing characterization analysis on the adsorbing material obtained in the step (3) by a Scanning Electron Microscope (SEM), and finding that obvious channels appear on the 700DK7006 surface, which shows that H is a defect2SO4The modification plays a favorable role in preparing the biomass charcoal material with the adsorption effect on the toluene.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (10)

1. An acid modification preparation method of a biomass charcoal material with toluene adsorption function is characterized by comprising the following steps:
s1: washing the surface of the rice hull by deionized water, and drying to finish pretreatment;
s2: placing the pretreated rice hulls in a tubular furnace, and carbonizing under the protection of inert gas;
s3: grinding and sieving the carbonized rice hulls to obtain biochar, putting the biochar in sulfuric acid, continuously stirring and soaking for 6-12 h to form a microporous structure with a specific size range in the biochar, and attaching oxygen-containing functional groups in the microporous structure to obtain an acid modified precursor;
s4: and washing, filtering and drying the acid modified precursor to obtain the acid modified rice hull biochar.
2. The acid modification preparation method of biomass charcoal material with toluene adsorption function according to claim 1, wherein the mass concentration of biochar in sulfuric acid in S3 is 10 g/L.
3. The acid modification preparation method of biomass charcoal material with toluene adsorption function according to claim 2, wherein the mass fraction of sulfuric acid in S3 is 20% -90%.
4. The acid modification preparation method of biomass charcoal material with toluene adsorption function according to claim 1, wherein the microporous structure in S3 is a three-dimensional through hole or pore structure with a pore size of 15-500nm, which is locally or globally through.
5. The acid modification preparation method of the biomass charcoal material with the toluene adsorbing effect according to claim 1, wherein the drying process temperature in S1 and S4 is 80-105 ℃.
6. The acid modification preparation method of biomass charcoal material with toluene adsorption function according to claim 1, wherein the inert gas is introduced into S2 for 15-20min, and then the temperature is raised for carbonization.
7. The acid modification preparation method of biomass charcoal material with toluene adsorption function according to claim 1, wherein in the carbonization process in S2, the temperature rise speed is 2-10 ℃/min, the carbonization temperature is 500-700 ℃, and the heat preservation time is 1-3 h.
8. The method for preparing the biomass charcoal material with the adsorption effect on toluene according to claim 7, wherein the carbonization temperature is 700 ℃.
9. The acid modification preparation method of biomass charcoal material with toluene adsorption function according to claim 1, wherein 80-100 mesh biochar particles are screened in S3.
10. The acid modification preparation method of biomass charcoal material with toluene adsorption function according to claim 1, wherein the washing process in S4 is soaking with 1-5M NaOH and washing to neutrality.
CN202110095678.2A 2021-01-25 2021-01-25 Acid modification preparation method of biomass charcoal material with toluene adsorption effect Pending CN112897503A (en)

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CN113307262A (en) * 2021-06-16 2021-08-27 哈尔滨工业大学（深圳） Preparation method and application of highly graphitized biochar-based material
CN115945182A (en) * 2022-12-20 2023-04-11 安徽工业大学 Adsorbent for treating VOCs and dioxin in organic coating pyrolysis flue gas and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113307262A (en) * 2021-06-16 2021-08-27 哈尔滨工业大学（深圳） Preparation method and application of highly graphitized biochar-based material
CN115945182A (en) * 2022-12-20 2023-04-11 安徽工业大学 Adsorbent for treating VOCs and dioxin in organic coating pyrolysis flue gas and preparation method thereof
CN115945182B (en) * 2022-12-20 2024-04-16 安徽工业大学 Adsorbent for treating VOCs and dioxins in organic coating pyrolysis flue gas and preparation method thereof

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Application publication date: 20210604