CN113233460A - Method for hydrothermal-assisted production of lignin activated carbon with high specific surface area - Google Patents
Method for hydrothermal-assisted production of lignin activated carbon with high specific surface area Download PDFInfo
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- CN113233460A CN113233460A CN202110350966.8A CN202110350966A CN113233460A CN 113233460 A CN113233460 A CN 113233460A CN 202110350966 A CN202110350966 A CN 202110350966A CN 113233460 A CN113233460 A CN 113233460A
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- surface area
- specific surface
- lignin
- activated carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
Abstract
The invention discloses a method for hydrothermal auxiliary production of lignin activated carbon with a high specific surface area, which comprises the following steps: putting lignin and deionized water into a reaction kettle; the reaction kettle is arranged in a muffle furnace and is insulated for a certain time; placing the mixture subjected to hydrothermal assistance in a nickel ark, adding KOH with certain mass, and slowly stirring; putting the nickel ark with the stirred mixture into a high-temperature tube furnace to activate for a certain time; and cooling, acid washing and water washing the activated product, and drying the product in an oven to constant weight to obtain the lignin activated carbon with high specific surface area. Compared with lignin pyrolytic carbon (without hydrothermal assistance and KOH), the specific surface area is obviously improved, and the improvement rate reaches 265.82-374.90%; compared with the lignin activated carbon activated by KOH (without hydrothermal assistance), the specific surface area is also obviously improved, and the improvement rate reaches 48.93-93.34%. The process is simple to operate, low in production cost and remarkable in economic benefit.
Description
Technical Field
The invention belongs to the field of activated carbon production, and particularly relates to a method for hydrothermal-assisted production of lignin activated carbon with a high specific surface area.
Background
The activated carbon with high specific surface area has a developed pore structure and extremely strong adsorption capacity, is a carbon material with excellent performance, and is widely applied to the fields of military industry, fermentation, bio-pharmaceuticals, synthetic chemical industry, environmental protection, electrode materials and the like. However, the specific surface area of the commercially available activated carbon (500- & lt 1200 & gt m)2The/g) is generally low. Therefore, activated carbon with high specific surface area has been favored. In order to produce activated carbon with high specific surface area, multiple activating agents are often adopted for composite activation. However, the activation process is complicated, the production time is long, and the chemical reagent is used for many times, so that the production cost is extremely high.
In addition, in the papermaking industry, a large amount of lignin is discharged along with waste liquid, so that resource waste is caused, the environment is polluted, meanwhile, most of the development of the lignin is concentrated on the research of lignin adhesives, and the range of lignin increment is limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for hydrothermal auxiliary production of lignin activated carbon with high specific surface area aiming at the defects of the prior art, and the method for hydrothermal auxiliary production of lignin activated carbon with high specific surface area realizes the aims of increasing the value of lignin and greatly increasing the specific surface area of activated carbon, thereby achieving the win-win effect of further improving the economic benefit and the quality of activated carbon.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a method for hydrothermal-assisted production of lignin activated carbon with high specific surface area comprises the following steps:
(1) putting a certain mass of lignin and a certain volume of deionized water into a reaction kettle;
(2) the reaction kettle is arranged in a muffle furnace and is insulated for a certain time;
(3) placing the mixture subjected to hydrothermal assistance in a nickel ark, adding KOH with certain mass, and slowly stirring;
(4) putting the nickel ark with the stirred mixture into a high-temperature tube furnace to activate for a certain time;
(5) and cooling, acid washing and water washing the activated product, and drying the product in an oven to constant weight to obtain the lignin activated carbon with high specific surface area.
As a further improved technical scheme of the invention, the mass of the lignin in the step (1) is 5 g, and the volume of the deionized water is 60 mL.
As a further improved technical scheme of the invention, the temperature of the muffle furnace in the step (2) is 100-250 ℃, and the heat preservation time is 2 h.
As a further improvement of the invention, the mass of KOH in the step (3) is 10 g.
As a further improved technical scheme of the invention, in the step (4), under the nitrogen atmosphere, the temperature of the tubular furnace is increased from room temperature to 900 ℃ at the heating rate of 10 ℃/min, and the temperature is maintained at 900 ℃ for 80 min.
As a further improved technical scheme of the invention, the flow rate of the nitrogen is 200 mL/min.
As a further improved technical scheme of the present invention, the step (5) of drying in an oven to a constant weight specifically comprises: drying in 105 deg.C oven to constant weight.
The invention has the beneficial effects that:
(1) the invention realizes the increment of lignin and obviously improves the specific surface area of the lignin activated carbon.
(2) The invention has simple process operation, lower production cost and obvious economic benefit.
Drawings
FIG. 1 is a flow chart of a method for hydrothermally assisted production of high specific surface area lignin activated carbon.
FIG. 2 is a nitrogen adsorption and desorption curve of apricot hull lignin pyrolytic carbon and activated carbon.
Detailed Description
The present invention is further illustrated by the following specific examples. The experimental procedures in the following examples are conventional unless otherwise specified.
Raw materials: lignin (production factory: Tokyo chemical industry plant type club house, particle size 100-
The main device comprises: a reaction kettle, a muffle furnace, a high-temperature tube furnace, an oven and an Autosorb-iQ type full-automatic gas adsorption analyzer.
Example 1:
the nickel ark containing 5 g of lignin is placed in a high-temperature tube furnace, and is heated to 900 ℃ from room temperature at the heating rate of 10 ℃/min in the nitrogen atmosphere of 200 mL/min, and is kept at the temperature for 80 min. The tube furnace was cooled to room temperature and the sample was removed, washed with water to neutrality and then dried in an oven at 105 ℃ to constant weight. Thus obtaining the lignin pyrolytic carbon (named AAC-1). According to the nitrogen adsorption-desorption curve test (analysis is carried out by adopting an Autosorb-iQ type full-automatic gas adsorption analyzer, the same is applied below) shown in FIG. 2, the specific surface area of AAC-1 is 669.27 m2/g。
Example 2:
placing 5 g of lignin in a nickel ark, adding 10 g of KOH and 10 mL of deionized water, and slowly stirring until the lignin is uniformly mixed. Then the nickel ark with the mixture is placed in a high-temperature tube furnace, and the temperature is raised from room temperature to 900 ℃ at the temperature raising rate of 10 ℃/min in the nitrogen atmosphere of 200 mL/min, and the temperature is kept for 80 min at the temperature. The tube furnace was cooled to room temperature and the sample was removed, acid washed, water washed to neutral and then dried in an oven at 105 ℃ to constant weight. Thus obtaining the lignin activated carbon (named AAC-2) with higher specific surface area. The specific surface area of AAC-2 is 1643.93 m by the test of a nitrogen adsorption and desorption curve2/g。
Example 3:
as shown in FIG. 1, 5 g of lignin and 60 mL of deionized water were placed in a reaction kettle and mixed well, and then the reaction kettle was placed in a muffle furnace at 100 ℃ for 2 hours. The reaction kettle is cooled to room temperature, the mixture subjected to the hydrothermal auxiliary treatment is poured out to be put into a nickel ark, 10 g of KOH is added, and the mixture is slowly stirred until the mixture is uniformly mixed. The nickel ark with the mixture (mixed well) was then placed in a high temperature tube furnace, warmed from room temperature to 900 ℃ at a ramp rate of 10 ℃/min in a nitrogen atmosphere of 200 mL/min, and held at that temperature for 80 min. The tube furnace was cooled to room temperature and the sample was removed, acid washed, water washed to neutral and then dried in an oven at 105 ℃ to constant weight. Thus obtaining the lignin activated carbon (named AAC-3) with high specific surface area. The specific surface area of AAC-3 is 2448.35 m by the test of a nitrogen adsorption and desorption curve2(ii) in terms of/g. The specific surface area of AAC-3 is increased by 265.82% and 48.93% respectively compared with the specific surface area of AAC-1 and AAC-2.
Example 4:
as shown in FIG. 1, 5 g of lignin and 60 mL of deionized water were placed in a reaction kettle and mixed well, and then the reaction kettle was placed in a muffle furnace at 150 ℃ for 2 hours. The reaction kettle is cooled to room temperature, the mixture subjected to the hydrothermal auxiliary treatment is poured out to be put into a nickel ark, 10 g of KOH is added, and the mixture is slowly stirred until the mixture is uniformly mixed. The nickel ark with the mixture (mixed well) was then placed in a high temperature tube furnace, warmed from room temperature to 900 ℃ at a ramp rate of 10 ℃/min in a nitrogen atmosphere of 200 mL/min, and held at that temperature for 80 min. The tube furnace was cooled to room temperature and the sample was removed, acid washed, water washed to neutral and then dried in an oven at 105 ℃ to constant weight. Thus obtaining the lignin activated carbon (named AAC-4) with high specific surface area. The specific surface area of AAC-4 is 3033.88 m by the test of a nitrogen adsorption and desorption curve2(ii) in terms of/g. The specific surface area of AAC-4 is increased by 353.31% and 84.55% respectively compared with the specific surface area of AAC-1 and AAC-2.
Example 5:
as shown in FIG. 1, 5 g of lignin and 60 mL of deionized water were placed in a reaction kettle and mixed well, and then the reaction kettle was placed at 200 deg.CThe temperature in the muffle furnace was maintained for 2 hours. The reaction kettle is cooled to room temperature, the mixture subjected to the hydrothermal auxiliary treatment is poured out to be put into a nickel ark, 10 g of KOH is added, and the mixture is slowly stirred until the mixture is uniformly mixed. The nickel ark with the mixture (mixed well) was then placed in a high temperature tube furnace, warmed from room temperature to 900 ℃ at a ramp rate of 10 ℃/min in a nitrogen atmosphere of 200 mL/min, and held at that temperature for 80 min. The tube furnace was cooled to room temperature and the sample was removed, acid washed, water washed to neutral and then dried in an oven at 105 ℃ to constant weight. Thus obtaining the lignin activated carbon (named AAC-5) with high specific surface area. The specific surface area of AAC-5 is 3178.36 m by the test of a nitrogen adsorption and desorption curve2(ii) in terms of/g. The specific surface area of AAC-5 is increased by 374.90% and 93.34% compared with the specific surface area of AAC-1 and AAC-2, respectively.
Example 6:
as shown in FIG. 1, 5 g of lignin and 60 mL of deionized water were placed in a reaction kettle and mixed well, and then the reaction kettle was placed in a muffle furnace at 250 ℃ for 2 hours. The reaction kettle is cooled to room temperature, the mixture subjected to hydrothermal auxiliary treatment is poured out to be put into a nickel ark, 10 g of KOH is added, and the mixture is slowly stirred until the mixture is uniformly mixed. The nickel ark with the mixture (mixed well) was then placed in a high temperature tube furnace, warmed from room temperature to 900 ℃ at a ramp rate of 10 ℃/min in a nitrogen atmosphere of 200 mL/min, and held at that temperature for 80 min. The tube furnace was cooled to room temperature and the sample was removed, acid washed, water washed to neutral and then dried in an oven at 105 ℃ to constant weight. Thus obtaining the lignin activated carbon (named AAC-6) with high specific surface area. The specific surface area of AAC-6 is 2697.79 m by the test of a nitrogen adsorption and desorption curve2(ii) in terms of/g. The specific surface area of AAC-6 is increased by 303.09% and 64.11% compared with the specific surface area of AAC-1 and AAC-2, respectively.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (7)
1. A method for producing lignin activated carbon with high specific surface area by hydrothermal auxiliary production is characterized in that: the method comprises the following steps:
(1) putting a certain mass of lignin and a certain volume of deionized water into a reaction kettle;
(2) the reaction kettle is arranged in a muffle furnace and is insulated for a certain time;
(3) placing the mixture subjected to hydrothermal assistance in a nickel ark, adding KOH with certain mass, and slowly stirring;
(4) putting the nickel ark with the stirred mixture into a high-temperature tube furnace to activate for a certain time;
(5) and cooling, acid washing and water washing the activated product, and drying the product in an oven to constant weight to obtain the lignin activated carbon with high specific surface area.
2. The method for hydrothermally assisted production of high specific surface area lignin activated carbon according to claim 1, characterized in that: the mass of the lignin in the step (1) is 5 g, and the volume of the deionized water is 60 mL.
3. The method for hydrothermally assisted production of high specific surface area lignin activated carbon according to claim 1, characterized in that: the temperature of the muffle furnace in the step (2) is 100-250 ℃, and the heat preservation time is 2 h.
4. The method for hydrothermally assisted production of high specific surface area lignin activated carbon according to claim 1, characterized in that: the mass of KOH in the step (3) is 10 g.
5. The method for hydrothermally assisted production of high specific surface area lignin activated carbon according to claim 1, characterized in that: in the step (4), in the nitrogen atmosphere, the temperature of the tube furnace is increased from room temperature to 900 ℃ at the heating rate of 10 ℃/min, and the temperature is maintained at 900 ℃ for 80 min.
6. The method for hydrothermally assisted production of high specific surface area lignin activated carbon according to claim 5, characterized in that: the flow rate of the nitrogen is 200 mL/min.
7. The method for hydrothermally assisted production of high specific surface area lignin activated carbon according to claim 1, characterized in that: the step (5) of drying in an oven to constant weight specifically comprises the following steps: drying in 105 deg.C oven to constant weight.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534690A (en) * | 2022-03-18 | 2022-05-27 | 南京林业大学 | Biomass activated carbon for removing tetracycline and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127695A (en) * | 2018-11-22 | 2019-08-16 | 南京林业大学 | A kind of preparation method of supercapacitor wood sawdust base porous charcoal |
| CN110862077A (en) * | 2019-11-19 | 2020-03-06 | 东华大学 | Preparation method of hierarchical porous carbon material rich in mesopores for supercapacitor |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127695A (en) * | 2018-11-22 | 2019-08-16 | 南京林业大学 | A kind of preparation method of supercapacitor wood sawdust base porous charcoal |
| CN110862077A (en) * | 2019-11-19 | 2020-03-06 | 东华大学 | Preparation method of hierarchical porous carbon material rich in mesopores for supercapacitor |
Non-Patent Citations (1)
| Title |
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| CATALINA RODRÍGUEZ CORREA等: "Influence of the Carbonization Process on Activated Carbon Properties from Lignin and Lignin-Rich Biomasses" * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534690A (en) * | 2022-03-18 | 2022-05-27 | 南京林业大学 | Biomass activated carbon for removing tetracycline and preparation method thereof |
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