CN110935420A - Normal pressure CO2Preparation method of hierarchical pore activated carbon adsorbent - Google Patents
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Abstract
The invention relates to normal pressure CO2A preparation method of a hierarchical pore activated carbon adsorbent belongs to the technical field of activated carbon modification. Firstly, the waste fir, pine, cypress and camphor tree sawdust are used as carbon sources to be carbonized at a certain temperature. And then mixing the primary carbon and an activating agent according to a certain proportion, and activating at a certain temperature to construct a pore structure of the carbon, so as to obtain the activated carbon with a multistage pore structure. Finally adopting ultrasonic impregnation method to use modifier pairAnd (5) modifying by using activated carbon. Thermal gravimetric method for CO at normal temperature and pressure2The adsorption is carried out, and the balance adsorption capacity with the most excellent performance in the modified activated carbon can reach 6.20 mmol/g. The method has the characteristics of simple operation, cheap and easily obtained raw materials, high cost performance and the like.
Description
Technical Field
The invention relates to normal pressure CO2A preparation method of a hierarchical pore activated carbon adsorbent belongs to the technical field of activated carbon modification.
Background
The global warming caused by the aggravation of the greenhouse effect causes serious damage to our living environment, so that the reduction of greenhouse gases in the atmosphere is the key for reducing the greenhouse effect, and CO2Has the highest proportion in greenhouse gases, thereby reducing CO in the atmosphere2Is the key to reducing greenhouse gas emissions. CO discharged from coal-fired power plant2It occupies most of the space. Thereby reducing CO in flue gas of coal-fired power plant2The concentration of (2) is imperative.
The solid adsorbent is an adsorption material which is widely seen at present, and has the advantages of low corrosivity, low energy consumption, simple operation, large removal depth and the like. The solid adsorbents currently studied are mainly zeolites, organic polymers, metal organic frameworks, silica and activated carbon. Compared with the solid adsorbents, the activated carbon has the advantages of excellent hydrophobicity, developed pore structure, excellent cycling stability, low preparation cost, low regeneration energy consumption and the like, and is considered to be excellent CO2An adsorbent.
Activated carbon is prepared by using wood, coal, peat and the like as raw materials of a carbon precursor, carbonizing the raw materials at high temperature, and activating the carbonized materials. Activated carbon belongs to amorphous carbon, and during the activation process of the amorphous carbon, carbon-containing organic matters and disordered carbon among microcrystalline structures of the amorphous carbon are removed, so that pores of the activated carbon are formed. The shape, size and distribution of the pores of the activated carbon are different according to the raw materials, carbonization and activation processes. The activated carbon prepared by using biomass as a precursor mainly uses potassium hydroxide as an activating agent, and the activated carbon has good micropore and mesopore structures. Numerous studies have shown that the micropores and mesopores of the adsorbent are in CO2Plays an important role in the adsorption process of (A), and micropores play a role in CO2The mesoporous structure plays a main role in adsorption, and a large amount of CO can be absorbed by the mesoporous structure2The adsorption of carbon dioxide is promoted. Eyes of a userThe first most part of the activated carbon is in the presence of low concentration of CO2(CO in flue gas)2About 15%) had a poor adsorption effect at normal pressure. Therefore, macropores, mesopores and micropores are generated in the activated carbon, the macropores, the mesopores and the micropores in the activated carbon are fully utilized to be mutually cooperated, the modifier can reach the micropores more easily in the modification process, and the low-concentration carbon dioxide has excellent adsorption performance at normal pressure and normal temperature due to the unobstructed pore passage and the action of the modifier in the adsorption process.
Disclosure of Invention
Aiming at the problem that the adsorption effect of the existing activated carbon and modified activated carbon thereof on carbon dioxide under normal pressure is not ideal, the invention provides a preparation method of activated carbon prepared from fir, pine, cypress and camphor tree sawdust and modified by metal salt. The method has the characteristics of simple operation, cheap and easily obtained raw materials, high cost performance and the like.
The invention is realized by the following technical scheme:
normal pressure CO2The preparation method of the porous activated carbon adsorbent comprises the following steps:
(1) placing a certain amount of sawdust raw material in a tubular furnace, introducing nitrogen into the tubular furnace, wherein the flow rate of the nitrogen is 0.1-0.5L/min, heating the tubular furnace to 600-;
(2) mixing the primary carbon and an activating agent according to the mass ratio of the alkali to the carbon (0.2-10): 1, adding deionized water, stirring at room temperature for 30-60min, standing for 8-36h, and drying at 100-;
(3) and (3) placing the mixture in a tubular furnace, introducing nitrogen into the tubular furnace, activating at the temperature of 600-.
(4) Mixing an appropriate amount of activated carbon obtained in the step (3) with a modifier according to a mass ratio of (0.2-10): 1, adding an appropriate amount of deionized water, and heating at 70-100 DEG CAnd (3) performing ultrasonic treatment for 80-100 min after the water bath is carried out for 30min, and finally drying at the temperature of 100-. The modified activated carbon is used for CO thermal gravimetric method at normal temperature and normal pressure2And (4) carrying out adsorption.
Wherein the sawdust raw material is selected from any one of waste fir, pine, cypress and camphor tree sawdust.
Further, the activating agent is KOH or NH3·H2O、NaOH、Ca(OH)2Any one of them.
Further, the modifier is KCl, NaCl, MgCl2·6H2O、Mg(NO3)2·6H2O、NaNO3、KNO3Any one of the above.
The invention has the following remarkable advantages:
the method has the advantages of easily obtained raw materials, simple operation and low requirements on experimental equipment, and the active carbon prepared by the method can be seen from the attached drawing to have macropores, mesopores and micropores (SEM analysis in figure 1 can show that macropores exist on the surface of the activated active carbon, and pore size distribution in figure 2 shows that micropores and mesopores exist in the activated active carbon) and higher specific surface area of about 1200m2The pores are in multiple grades and have excellent adsorption performance on carbon dioxide at normal pressure and normal temperature, the highest adsorption performance can reach 6.20mmol/g, and the carbon dioxide can be prepared and recycled on a large scale.
Drawings
FIG. 1 scanning electron microscopy characterization of activated carbon after activation;
figure 2 pore size distribution of activated carbon after activation.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. The scope of the present invention includes, but is not limited to, the following embodiments, and any modifications made in the details and form of the technical solution of the present invention are within the scope of the present invention without departing from the spirit and scope of the present application.
Example 1:
putting a certain amount of sawdust raw material into a tubular furnace, introducing nitrogen into the tubular furnace, wherein the flow rate of the nitrogen is 0.1L/min, and the tubular furnace is used for producing sawdustHeating the furnace to 700 ℃ at the speed of 10 ℃/min, carbonizing for 60min, and cooling to room temperature to obtain a primary carbon material; mixing an activating agent and primary carbon according to the mass ratio of 2:1, adding deionized water, stirring at room temperature for 30min, standing for 20h, and drying at 115 ℃. And (3) placing the fully mixed alkali-carbon mixture in a tubular furnace, introducing nitrogen into the tubular furnace, activating at 700 ℃ for 60min, cooling to room temperature, taking out, washing with deionized water to be neutral, and drying for later use. Mixing the activated carbon and a modifier according to the mass ratio of 0.5:1, adding deionized water, carrying out water bath at 80 ℃ for 30min, carrying out ultrasonic treatment for 80min, and finally drying at 100 ℃ to obtain the modified activated carbon. The modified activated carbon is used for CO thermal gravimetric method at normal temperature and normal pressure2(15vol.%) and the equilibrium adsorption amount can reach 4.06 mmol/g.
Example 2:
putting a certain amount of sawdust raw materials into a tubular furnace, introducing nitrogen into the tubular furnace, heating the tubular furnace to 600 ℃ at the speed of 10 ℃/min, carbonizing the sawdust raw materials for 65min, and cooling the sawdust raw materials to room temperature to obtain a primary carbon material, wherein the flow rate of the nitrogen is 0.2L/min; mixing an activating agent and primary carbon according to the mass ratio of 3.5:1, adding deionized water, stirring at room temperature for 30min, standing for 12h, and drying at 100 ℃. And (3) placing the fully mixed alkali-carbon mixture in a tubular furnace, introducing nitrogen into the tubular furnace, activating at 750 ℃ for 65min, cooling to room temperature, taking out, washing with deionized water to be neutral, and drying for later use. Mixing activated carbon and a modifier according to the mass ratio of 1.5:1, adding deionized water, carrying out water bath at 80 ℃ for 30min, carrying out ultrasonic treatment for 80min, and finally drying at 100 ℃ to obtain the modified activated carbon. The modified activated carbon is used for CO thermal gravimetric method at normal temperature and normal pressure2(15vol.%) and the equilibrium adsorption can reach 4.69 mmol/g. .
Example 3:
putting a certain amount of sawdust raw materials into a tubular furnace, introducing nitrogen into the tubular furnace, heating the tubular furnace to 700 ℃ at the speed of 10 ℃/min, carbonizing the sawdust raw materials for 65min, and cooling the sawdust raw materials to room temperature to obtain a primary carbon material, wherein the flow rate of the nitrogen is 0.3L/min; mixing an activating agent and primary carbon according to the mass ratio of the alkali to the carbon of 4.5:1, adding deionized water, stirring at room temperature for 30min, standing for 12h, and drying at 100 ℃. Mixing the aboveAnd (3) fully mixing the alkali-carbon mixture, placing the mixture in a tubular furnace, introducing nitrogen into the tubular furnace, activating the mixture for 70min at the temperature of 790 ℃, taking the mixture out after cooling the mixture to the room temperature, washing the mixture to be neutral by using deionized water, and drying the mixture for later use. Mixing activated carbon and a modifier according to the mass ratio of 3:1, adding deionized water, carrying out water bath at 80 ℃ for 30min, carrying out ultrasonic treatment for 80min, and finally drying at 100 ℃ to obtain the modified activated carbon. The modified activated carbon is used for CO thermal gravimetric method at normal temperature and normal pressure2(15vol.%) and the equilibrium adsorption can reach 5.82 mmol/g.
Example 4:
putting a certain amount of sawdust raw materials into a tubular furnace, introducing nitrogen into the tubular furnace, heating the tubular furnace to 800 ℃ at the speed of 10 ℃/min, carbonizing the sawdust raw materials for 70min, and cooling the sawdust raw materials to room temperature to obtain a primary carbon material, wherein the flow rate of the nitrogen is 0.4L/min; mixing an activating agent and primary carbon according to the mass ratio of 5:1, adding deionized water, stirring at room temperature for 30min, standing for 12h, and drying at 100 ℃. And (3) placing the fully mixed alkali-carbon mixture in a tubular furnace, introducing nitrogen into the tubular furnace, activating at 650 ℃ for 75min, cooling to room temperature, taking out, washing with deionized water to be neutral, and drying for later use. Mixing activated carbon and a modifier according to a mass ratio of 4:1, adding deionized water, carrying out water bath at 90 ℃ for 30min, carrying out ultrasonic treatment for 100min, and finally drying at 100 ℃ to obtain the modified activated carbon. The modified activated carbon is used for CO thermal gravimetric method at normal temperature and normal pressure2(15vol.%) and the equilibrium adsorption can reach 6.20 mmol/g.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. Normal pressure CO2The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: the method comprises the following steps:
(1) placing a certain amount of sawdust raw material in a tubular furnace, introducing nitrogen into the tubular furnace, wherein the flow rate of the nitrogen is 0.1-0.5L/min, heating the tubular furnace to 600-;
(2) mixing the primary carbon and an activating agent, adding deionized water, stirring at room temperature for 30-60min, standing for 8-36h, and drying at 100-115 ℃;
(3) placing the mixture in a tubular furnace, introducing nitrogen into the tubular furnace, activating, cooling to room temperature, taking out, washing with deionized water to be neutral, and drying for later use;
(4) mixing the activated carbon obtained in the step (3) with a modifier, adding deionized water, performing ultrasonic treatment after water bath, and finally drying at the temperature of 100-115 ℃ to obtain the modified activated carbon.
2. The atmospheric CO of claim 12The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: wherein the sawdust raw material is selected from any one of waste fir, pine, cypress and camphor tree sawdust.
3. The atmospheric CO of claim 12The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: the activating agent is KOH or NH3·H2O、NaOH、Ca(OH)2Any one of them.
4. The atmospheric CO of claim 12The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: and (3) mixing the primary carbon and the activating agent in the step (2) according to the mass ratio of the alkali to the carbon (0.2-10) to 1.
5. The atmospheric CO of claim 12The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: the modifier is KCl, NaCl, MgCl2·6H2O、Mg(NO3)2·6H2O、NaNO3、KNO3Any one of them.
6. The atmospheric CO of claim 12The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: the activation in the step (3) is specifically in 600-Activating at 800 deg.C for 60-100 min.
7. The atmospheric CO of claim 12The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: and (4) mixing the activated carbon and the modifier according to a mass ratio of (0.2-10) to 1.
8. The atmospheric CO of claim 12The preparation method of the hierarchical pore activated carbon adsorbent is characterized by comprising the following steps: the post-water bath ultrasound in the step (4) is specifically as follows: carrying out water bath at 70-100 ℃ for 30min, and then carrying out ultrasonic treatment for 80-100 min.
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Cited By (4)
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| CN111659046A (en) * | 2020-06-15 | 2020-09-15 | 北京东瑞科技有限公司 | Protective mask |
| CN113041999A (en) * | 2021-03-23 | 2021-06-29 | 福州大学 | Preparation of atmospheric CO from nutshells2Method for producing adsorbent |
| CN113101894A (en) * | 2021-04-30 | 2021-07-13 | 广东国华人防科技有限公司 | Modified activated carbon, preparation method thereof and civil air defense filter absorber using modified activated carbon |
| CN117585673A (en) * | 2024-01-19 | 2024-02-23 | 成都达奇科技股份有限公司 | Preparation method of biomembrane carrier activated carbon for sewage treatment and sewage treatment method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113101894A (en) * | 2021-04-30 | 2021-07-13 | 广东国华人防科技有限公司 | Modified activated carbon, preparation method thereof and civil air defense filter absorber using modified activated carbon |
| CN117585673A (en) * | 2024-01-19 | 2024-02-23 | 成都达奇科技股份有限公司 | Preparation method of biomembrane carrier activated carbon for sewage treatment and sewage treatment method |
| CN117585673B (en) * | 2024-01-19 | 2024-04-30 | 成都达奇科技股份有限公司 | Preparation method of biomembrane carrier activated carbon for sewage treatment and sewage treatment method |
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