CN114887590A - Preparation method of porous biochar rich in alkaline sites and application of porous biochar in odor adsorption - Google Patents
Preparation method of porous biochar rich in alkaline sites and application of porous biochar in odor adsorption Download PDFInfo
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Abstract
The invention relates to the technical field of biomass resource utilization, in particular to a preparation method of porous biochar rich in alkaline sites and application of the porous biochar in odor adsorption. The method comprises the steps of uniformly mixing wood chips, a pore-forming agent and a nitrogen-containing template agent, then ball-milling the mixture into a solid mixture, and preparing the mixture into the porous biochar in protective gas by adopting a pyrolysis method. The preparation method can enrich the pore structure of the biochar, can form more defect sites on the surface, is beneficial to introducing alkaline nitrogen-containing functional groups, and improves the efficiency of adsorbing acidic gas components in odor. Meanwhile, the invention also discloses application of the porous biochar in odor adsorption, and the prepared biochar and the molecular sieve are combined to form a combined adsorbent, so that double adsorption of physical adsorption and chemical adsorption is realized, and the purpose of greatly improving odor adsorption efficiency is achieved.
Description
Technical Field
The invention relates to the technical field of biomass resource utilization, in particular to a preparation method of porous biochar rich in alkaline sites and application of the porous biochar in odor adsorption.
Background
In recent years, clean and safe disposal and energy utilization of a large amount of landfill gas in municipal landfill sites have become a current research hotspot. The anaerobic microbial digestion produces landfill gas containing components including methane, carbon dioxide, nitrogen, water and sulfur-containing harmful gases (SO) 2 、H 2 S) and the like, reasonably applies the renewable energy technology to treat the landfill gas, not only can greatly reduce the emission of atmospheric pollutants, but also can obtain biogas resources, and has environmental-friendly economic benefit.
The landfill gas generates odor (as H) 2 S is the main acid gas), under the environment that water and oxygen exist, the acid gas in the odor can corrode the equipment such as pipelines, valves, compressors, gas storage tanks and the like, the service life of the equipment is reduced, meanwhile, the leakage and the discharge of sulfides can seriously pollute the environment and influence the biological safety, and therefore, H is removed 2 The acid gases such as S are generated in the process of utilizing landfill gasThe key steps are as follows. To date, researchers at home and abroad have conducted extensive studies on odor adsorption, mainly including physical adsorption and chemical adsorption. The physical adsorption mainly adopts active media with large specific surface area, such as active carbon, molecular sieve and the like, and adsorbs gas molecules in a porous medium through Van der Waals force to achieve the purpose of removing odor. Although the physical adsorbent has a large adsorption amount to odor, physical adsorption has no selectivity, and the adsorption effect in a low-concentration odor environment is poor. The chemical adsorption is adsorption generated by chemical bonds formed among molecules, and is characterized by strong selectivity and good adsorption effect on low-concentration odor, but most of chemical adsorbents have small adsorption amount on odor. The most common chemical adsorbent is a load type adsorbent doped with alkaline compounds (such as KOH, NaOH and the like), rich alkaline functional groups can efficiently adsorb acidic components in odor, and the strong alkalinity can also corrode equipment to cause secondary pollution. Therefore, it is a challenge to prepare a chemical adsorbent that is both efficient and non-corrosive.
Biochar is a material widely used in chemical adsorption at present, has the advantages of sufficient source, low cost and reproducibility, and is highly concerned by the industry. The biochar material is obtained by directly carbonizing a biomass raw material, has a small pore structure and a small specific surface area, and can be added with a pore-forming agent in the carbonization process in order to improve the characteristics of pore channels and the specific surface area of the biochar, so that the pore structure is enriched, and the specific surface area is increased. The Chinese patent application CN110935280A discloses a nitrogen-doped mesoporous bamboo-based biochar and application thereof, wherein the mesoporous bamboo-based biochar is prepared by taking waste disposable bamboo chopsticks as precursors through the steps of pretreatment, carbonization, air oxidation, urea nitrogen doping and the like, but the activated carbon has poor pore structure, limited specific surface area and no alkaline sites. Chinese patent application CN113231013A discloses vinasse-based biochar for adsorbing multi-component organic pollutants and a preparation method thereof, the vinasse-based biochar with rich microporous structures and large specific surface area is prepared, alkaline chemicals such as KOH and NaOH are used as activating agents, and strong alkalinity can corrode equipment. However, the existing biochar materials still have the problems of small pore structure, limited specific surface area and corrosiveness, so that the development of modified biochar materials with rich microporous structures, large specific surface areas and no corrosiveness is needed.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of porous biochar rich in alkaline sites and application of the porous biochar in odor adsorption.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of porous biochar rich in alkaline sites, which comprises the following steps:
s1, uniformly mixing the wood chips, the pore-forming agent and the nitrogen-containing template agent, and then crushing into a uniform solid mixture;
s2, carrying out pyrolysis reaction on the solid mixture under inert atmosphere;
and S3, adding boiling water into the obtained solid product, uniformly stirring to remove impurities, filtering, and drying filter residues to obtain the microporous biochar rich in the alkaline sites.
Preferably, in step 1, the wood chips comprise bamboo chips and fir wood chips; the pore-forming agent comprises potassium chloride and sodium chloride; the nitrogen-containing template agent comprises melamine, ammonium chloride and urea phosphate. Furthermore, the wood dust is bamboo dust, the pore-forming agent is sodium chloride, and the nitrogen-containing template agent is melamine.
Preferably, in the step 1, the mixing mass ratio of the wood dust, the pore-forming agent and the nitrogen-containing template is (2-3): (1-2): 0.5-1.
Preferably, in step 1, the particle size of the solid mixture is less than 30 mesh.
Preferably, in the step 2, the detailed step of the pyrolysis reaction is to heat the mixture to 300-350 ℃ at a heating rate of 3-5 ℃/min for reaction for 1-2 h; then, the temperature is raised to 750-850 ℃ at the rate of 1-3 ℃/min for reaction for 2-3 h. Further, the detailed steps of the pyrolysis reaction are that the temperature is increased to 300 ℃ at the rate of 3 ℃/min for reaction for 1 h; then the temperature is raised to 750 ℃ at the rate of 1 ℃/min for reaction for 2 h.
Preferably, in step 2, the inert gas is nitrogen.
The invention also provides the porous biochar rich in the alkaline sites, which is prepared by the preparation method and is applied to odor chemical adsorption. The prepared porous biochar and the molecular sieve are combined to form a combined adsorbent which is applied to odor physical and chemical adsorption.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of porous biochar rich in alkaline sites and application of the porous biochar in odor adsorption. The pyrolysis method and the pore-forming agent are utilized to enrich the pore structure of the biochar, more defect sites are formed on the surface, the nitrogen-containing template agent provides basic functional groups and forms basic sites, and the efficiency of adsorbing acidic gas components in odor is improved. The biochar prepared by the invention has the advantages of rich microporous structure, large specific surface area and no corrosiveness, can be applied to odor chemical adsorption, can realize dual adsorption of odor physics and chemistry by combining with the application of a molecular sieve, and greatly improves the odor adsorption efficiency.
Drawings
FIGS. 1 a-d are electron microscope scans of biochar, wherein (a) and (b) are biochar C and (C) and (d) are NMC-1;
fig. 2 is a schematic diagram of four packed small adsorption columns of biochar-coupled molecular sieves, where (a) is the molecular sieve: biochar: a small adsorption tower filled with a molecular sieve in a packing ratio of 1:1: 1; (b) is a molecular sieve: biochar: a small adsorption tower filled with a molecular sieve in a packing ratio of 1:4: 1; (c) is a molecular sieve: the biological carbon is a small adsorption tower with the filler proportion of 1:1 which is uniformly mixed; (d) is a molecular sieve: biochar: a small adsorption tower filled with a molecular sieve in a packing ratio of 3:1: 2.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The experimental procedures in the following examples were carried out by conventional methods unless otherwise specified, and the test materials used in the following examples were commercially available by conventional methods unless otherwise specified.
EXAMPLE 1 preparation of NMC-1 and sorbent combination
(1) Uniformly stirring 3g of bamboo chips, 2g of potassium chloride and 1.5g of melamine, placing the mixture and zirconia balls with the diameters of 1mm and 5mm respectively in a 100mL polytetrafluoroethylene ball milling tank, carrying out ball milling for 12 hours at the rotating speed of 270rpm by using a planetary ball mill, separating the materials, and filtering by using a 30-mesh sieve to obtain a uniform powdery solid mixture;
(2) transferring the powdery solid mixture into a tubular furnace, pyrolyzing the powdery solid mixture in the atmosphere of nitrogen, heating to 300 ℃ at the heating rate of 3 ℃/min, reacting for 1h, heating to 750 ℃ at the heating rate of 1 ℃/min, reacting for 2h, and cooling to room temperature to obtain a solid product;
(3) adding the obtained solid product into 500mL of boiling water, stirring uniformly, and performing suction filtration; performing suction filtration washing on the filter residue by using 2L of deionized water for 5 times until the filtrate is neutral, and finally drying the filter residue in a 60-DEG C oven for 12 hours to obtain porous biochar rich in alkaline sites, which is marked as NMC-1;
(4) preparation of NMC-1 combined with molecular sieves adsorbent:
1. filling 0.1g of 13X molecular sieve, 0.1g of NMC-1 and 0.1g of 13X molecular sieve into a small adsorption tower according to the packing ratio of 1:1:1, arranging the packing in sequence according to the weighing serial number from bottom to top, marking as MIX1, and filling the adsorbent in a manner shown in figure 2 (a);
2. filling 0.05g of 13X molecular sieve, 0.2g of NMC-1 and 0.05g of 13X molecular sieve into a small adsorption tower according to the packing ratio of 1:4:1, arranging the packing in sequence according to the weighing serial number from bottom to top, marking as MIX2, and filling the adsorbent in a manner shown in figure 2 (b);
3. uniformly mixing 0.15g of 13X molecular sieve and 0.15g of NMC-1 according to a filler ratio of 1:1, and filling the mixture into a small adsorption tower, wherein the mixture is marked as MIX3, and the adsorbent is filled in a manner shown in a figure 2 (c);
4. filling 0.15g of 13X molecular sieve, 0.05g of NMC-1 and 0.1g of 13X molecular sieve into a small adsorption tower according to the packing ratio of 3:1:2, arranging the packing in sequence according to the weighing serial number from bottom to top, marking as MIX4, and filling the adsorbent in a manner shown in figure 2 (d).
EXAMPLE 2 preparation of NMC-2 and sorbent combination
The preparation method is the same as example 1, and is different from example 1 in that the used wood chips are fir wood chips, and the microporous wood-based charcoal containing the alkaline sites is prepared and recorded as NMC-2;
preparation of NMC-2 combined with molecular sieves adsorbent:
1. filling 0.1g of 13X molecular sieve, 0.1g of NMC-2 and 0.1g of 13X molecular sieve into a small adsorption tower according to the packing ratio of 1:1:1, arranging the packing in sequence according to the weighing serial number from bottom to top, marking as MIX5, and filling the adsorbent in a manner shown in figure 2 (a);
2. filling 0.05g of 13X molecular sieve, 0.2g of NMC-2 and 0.05g of 13X molecular sieve into a small adsorption tower according to the packing ratio of 1:4:1, arranging the packing in sequence according to the weighing serial number from bottom to top, marking as MIX6, and filling the adsorbent in a manner shown in figure 2 (b);
3. uniformly mixing 0.15g of 13X molecular sieve and 0.15g of NMC-2 according to a filler ratio of 1:1, and filling the mixture into a small adsorption tower, wherein the mixture is marked as MIX7, and the adsorbent is filled in a manner shown in a figure 2 (c);
4. filling 0.15g of 13X molecular sieve, 0.05g of NMC-2 and 0.1g of 13X molecular sieve into a small adsorption tower according to the packing ratio of 3:1:2, arranging the packing in sequence according to the weighing serial number from bottom to top, marking as MIX8, and filling the adsorbent in a manner shown in figure 2 (d).
Comparative example 1 preparation of biochar C and Combined adsorbent thereof
The preparation method is the same as that of the example 1, and is different from the example 1 in that the biochar C is prepared without adding potassium chloride and melamine;
preparation of the adsorbent combining biochar C and molecular sieve: weighing (i) 0.1g of 13X molecular sieve, (ii) 0.1g of biochar C and (iii) 0.1g of 13X molecular sieve, and filling the materials into a small adsorption tower according to a filler ratio of 1:1:1, wherein the fillers are sequentially arranged from bottom to top according to the weighing serial numbers and are marked as MIX9, and the adsorbent filling mode is shown in figure 2 (a).
Comparative example 2 molecular sieve adsorbent
The odor adsorption experiment is carried out by adopting molecular sieves, and 0.3g of 13X molecular sieves are weighed and completely filled in a small adsorption tower and recorded as MIX 10.
Example 1 structural characterization of biochar and adsorption Capacity testing of the combination adsorbent
(1) Structural characterization
NMC-1 and biochar C are subjected to scanning analysis by an electron microscope, the scanning image is shown in figure 1, the biochar C is observed from figures 1a-b to have relatively flat and non-porous surface morphology, and the specific surface area and the pore volume are very small; from FIGS. 1c-d, it is observed that the surface of NMC-1 biochar has a rich pore structure.
The specific surface area, the pore volume and the pore size distribution of the activated carbon are measured by adopting a full-automatic specific surface area and pore size analyzer for NMC-1, NMC-2 and biochar C, and the specific surface areas and the pore characteristics of different biochars are shown in a table 1:
TABLE 1 characterization results of specific surface area and pore characteristics of different biochar
From table 1, it is found that the specific surface area and pore volume of the biochar can be greatly increased by using the pore-forming agent sodium chloride, the pore structures (such as micropores and mesopores) of the biochar are enriched, more defect sites are formed on the surface, and the introduction of basic sites containing nitrogen functional groups is facilitated.
(2) Adsorption Capacity testing of the Combined adsorbents
MIX1-10 was subjected to a fixed bed adsorption breakthrough experiment at room temperature. The adsorbents were packed in quartz tubes each having an inner diameter of 10mm, with an inlet hydrogen sulfide concentration of 500ppm and an inlet gas flow rate of 100 mL/min. The breakthrough adsorption capacity is the mass of gas molecules that can be adsorbed by a unit mass of adsorbent when the concentration of outlet gas reaches a certain concentration of outlet gas, which is used as a judgment index. In this experiment, it was considered that the breakthrough was initiated when the outlet hydrogen sulfide concentration was 1ppm, and the breakthrough sulfur capacity A was calculated according to the following formula C ，
In the formula:
A C : the mass of hydrogen sulfide adsorbed at the beginning of breakthrough of a unit mass of adsorbent, mg/g;
v: inlet gas flow rate, mL/min;
t: time, min; defining a breakthrough time for an outlet hydrogen sulfide concentration of 1 ppm;
cin: inlet hydrogen sulfide concentration, ppm;
cout: outlet hydrogen sulfide concentration, ppm;
m: molecular weight of hydrogen sulfide, 34 g/mol;
vmol: molar volume, 22.45mol/L (25 ℃, 1 atm);
m: mass of adsorbent, g;
each combined adsorbent penetrated the sulfur capacity A C The results are shown in table 2:
TABLE 2 breakthrough sulfur capacity of different combinations of sorbents
As shown in Table 2, the penetrating sulfur capacity of MIX1-8 is greatly increased compared with that of single charcoal, which indicates that a large number of defect sites are formed on the surface through the pore-forming agent, so that the basic sites containing a large number of nitrogen functional groups are introduced, the contact and adsorption of the basic sites and acidic gases can be greatly increased, and the odor chemical adsorption efficiency is improved.
In conclusion, the porous biochar formed by pyrolyzing the wood chips, the pore-forming agent and the nitrogen-containing template agent has abundant pore structures (such as micropores and mesopores) of the biochar, has a large specific surface area, forms a large number of basic sites containing nitrogen functional groups on the surface, and greatly increases the contact and adsorption of the basic sites and acidic gas, thereby improving the efficiency of odor chemical adsorption, having no corrosivity and reducing the damage to equipment; the porous biochar and the molecular sieve are combined into the combined adsorbent, so that the dual adsorption of physical adsorption and chemical adsorption is realized, and the purpose of greatly improving the odor adsorption efficiency is achieved.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (8)
1. A preparation method of porous biochar rich in alkaline sites is characterized by comprising the following steps:
s1, uniformly mixing the wood chips, the pore-forming agent and the nitrogen-containing template agent, and then crushing into a uniform solid mixture;
s2, carrying out pyrolysis reaction on the solid mixture under inert atmosphere;
and S3, adding boiling water into the obtained solid product, uniformly stirring to remove impurities, filtering, and drying filter residues to obtain the microporous biochar rich in the alkaline sites.
2. The method for preparing the porous biochar rich in alkaline sites according to claim 1, wherein in the step 1, the wood chips comprise bamboo chips and fir wood chips; the pore-forming agent comprises potassium chloride and sodium chloride; the nitrogen-containing template agent comprises melamine, ammonium chloride and urea phosphate.
3. The method for preparing the porous biochar rich in the alkaline sites according to claim 1, wherein in the step 1, the mixing mass ratio of the wood chips, the pore-forming agent and the nitrogen-containing template is (2-3): (1-2): 0.5-1.
4. The method for preparing a porous biochar rich in basic sites according to claim 1, wherein in step 1, the particle size of the solid mixture is less than 0.6 mm.
5. The preparation method of the porous biochar rich in the alkaline sites according to claim 1, wherein in the step 2, the detailed steps of the pyrolysis reaction are that the temperature is increased to 300-350 ℃ at a temperature increasing rate of 3-5 ℃/min for reaction for 1-2 hours; then, the temperature is raised to 750-850 ℃ at the rate of 1-3 ℃/min for reaction for 2-3 h.
6. The method for preparing porous biochar rich in basic sites according to claim 1, wherein in step 2, the inert gas is nitrogen.
7. The porous biochar rich in alkaline sites prepared by the preparation method of any one of claims 1 to 6.
8. The use of the basic site-enriched porous biochar of claim 7 for odor adsorption.
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| WO2022036878A1 (en) * | 2020-08-20 | 2022-02-24 | 浙江大学 | High-nitrogen biochar composite material, preparation method therefor, and application thereof |
| CN114433163A (en) * | 2022-01-24 | 2022-05-06 | 广东工业大学 | In-situ modified and pore-controllable biochar-supported ruthenium catalyst, preparation method thereof and application thereof in lignin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108163853A (en) * | 2018-02-07 | 2018-06-15 | 华中科技大学 | Method, product and its application of high nitrogenous porous carbon material are prepared using biomass |
| WO2022036878A1 (en) * | 2020-08-20 | 2022-02-24 | 浙江大学 | High-nitrogen biochar composite material, preparation method therefor, and application thereof |
| CN113603087A (en) * | 2021-09-03 | 2021-11-05 | 四川大学 | Nitrogen-rich biomass-based activated carbon with hierarchical pore microchannel structure and application thereof |
| CN114433163A (en) * | 2022-01-24 | 2022-05-06 | 广东工业大学 | In-situ modified and pore-controllable biochar-supported ruthenium catalyst, preparation method thereof and application thereof in lignin |
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