CN110327879B - Is suitable for flue gas CO2Preparation method and product of adsorbed biomass porous carbon - Google Patents
Is suitable for flue gas CO2Preparation method and product of adsorbed biomass porous carbon Download PDFInfo
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- CN110327879B CN110327879B CN201910508935.3A CN201910508935A CN110327879B CN 110327879 B CN110327879 B CN 110327879B CN 201910508935 A CN201910508935 A CN 201910508935A CN 110327879 B CN110327879 B CN 110327879B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention belongs to the technical field related to flue gas pollutant control, and discloses a method suitable for flue gas CO2The preparation method of the adsorbed biomass porous carbon comprises the following steps: washing, drying, crushing and screening a crude biomass sample to obtain biomass powder, mixing and grinding the biomass powder and an activating agent KOH, heating under an inert atmosphere to perform a carbonization reaction, and naturally cooling to room temperature; grinding the generated carbonized product, and then modifying the carbonized powder by adopting low-temperature plasma in the air atmosphere. The invention also discloses a corresponding biomass porous carbon adsorbent product. The method can prepare the high-quality porous carbon adsorbent by using the biomass raw material, has simple preparation method, low cost and small influence on the environment, and is easy for industrial application.
Description
Technical Field
The invention belongs to the technical field related to flue gas pollutant control, and particularly relates to a flue gas CO control method2A preparation method of adsorbed biomass porous carbon and a product.
Background
Greenhouse gases emitted by human activities cause serious environmental problems such as global warming, climate deterioration and the like, harm natural ecosystem and bring huge economic loss to human society. CO22Is the most dominant greenhouse gas. Coal-fired power plants are the most dominant CO2Emission source, therefore CO of coal-fired power plant2Capture is a significant challenge facing human society.
At present, CO2The capture technology mainly comprises a pre-combustion capture method, a post-combustion capture method and an oxygen-enriched combustion method. Compared with other two methods, the post-combustion capture method has the advantages of low cost and good applicability, and has wide market potential. The post-combustion capture method includes an amine absorption method, a membrane separation method, an adsorption method, and the like. Among them, the amine absorption method is mature, but will corrode the equipment and cause environmental pollution. The cost of membrane separation is relatively high and is not conducive to large-scale utilization. The most promising technology at present is adsorption, which is centered on the development of efficient, inexpensive adsorbents. Among various adsorbents, porous carbon is receiving more and more attention due to its advantages of high porosity, good stability, low regeneration energy, and the like.
The renewable biomass can be used as a raw material of the porous carbon, so that the cost of the porous carbon is reduced, and the porous carbon has wide application prospect. Some preparation processes of biomass porous carbon adsorbents have been proposed in the prior art. For example, CN201510939918.7 discloses a porous carbon CO2The preparation method of the adsorbent discloses that straw can be taken as a biomass raw material, a precursor is obtained through hydrothermal reaction, and then KOH is used for chemical activation to improve the specific surface area and the micropore structure of the adsorbent. For another example, CN201810454278.4 discloses a biomass charcoal-based CO2The adsorbent and the preparation method thereof disclose that chitosan can be added into mixed molten salt for pyrolysis to obtain an intermediate product, then high-temperature calcination is carried out, and finally the mixed molten salt is removed by washing to obtain the adsorbent. In addition, cn201210252491.x discloses a biochar-based CO modified by metal ions2A process for preparing adsorbent is disclosed, in which raw material such as bamboo charcoal can be added in CO2High-temperature activation is carried out under the atmosphere, and then the biological carbon-based adsorbent is obtained by dipping and modifying in an aqueous solution of metal nitrate or metal chloride.
However, further studies have shown that the above prior art solutions still have the following drawbacks or shortcomings: the preparation process is complex, needs multi-step reaction and is difficult to realize large-scale production; more importantly, the preparation process of the porous carbon uses more active agents and modifiers, so that the cost is increased, and the environment is easily polluted. Accordingly, there is a need in the art for further research and improvement to better meet the CO requirement of modern coal-fired power plants2The need for capture.
Disclosure of Invention
Aiming at the prior artIn view of the above-mentioned drawbacks or needs, the present invention provides a method for producing CO suitable for use in flue gas2The preparation method and the product of the adsorbed biomass porous carbon not only adopt the biomass as the preparation raw material of the porous carbon, but also further combine the requirements of specific application occasions of flue gas CO2 adsorption to research and design the preparation route, a plurality of key process conditions and the like again2The adsorbed heteroatom is doped into the porous carbon, so that the use of expensive and polluting modifiers is avoided, and meanwhile, the prepared porous carbon product has the characteristics of high specific surface area, rich pores, multiple active sites and the like, so that the porous carbon product is particularly suitable for CO in flue gas of a coal-fired power plant2Capture, and the like.
Accordingly, according to one aspect of the present invention, there is provided a method for CO-emission from flue gas2The preparation method of the adsorbed biomass porous carbon is characterized by comprising the following steps:
s1, selecting biomass as a charcoal source, washing the biomass with water, drying the biomass, and then crushing and screening the biomass to powder of 50-200 meshes;
s2, mixing and grinding the biomass powder and KOH serving as an activating agent according to the mass ratio of 1: 0.2-1: 1;
s3, transferring the mixture into a tube furnace, heating the mixture from room temperature to 600-1000 ℃ at the speed of 2-10 ℃/min under the inert gas atmosphere, and carbonizing the mixture for 0.5-4 hours; then, naturally cooling to room temperature under the atmosphere of inert gas, washing with 8-10 wt.% dilute hydrochloric acid to remove impurities, and drying after washing to obtain a carbonized product;
and S4, grinding and crushing the obtained carbonized product, and then modifying the ground and crushed carbonized product for 0.5-30 minutes by adopting low-temperature plasma with the working voltage of 20-60 KV in an air atmosphere, thereby obtaining the required porous carbon adsorbent product.
As a further preference, in step S1, the biomass is preferably one or a combination of the following: bark, leaves and wood chips.
More preferably, in step S1, the carbon source is pulverized and sieved to a powder of 80 to 150 mesh.
Further preferably, in step S2, the biomass powder and the activator are mixed and ground preferably at a mass ratio of 1:0.4 to 1: 0.8.
Further preferably, in step S3, the inert gas is preferably nitrogen, and the gas flow rate thereof is preferably set to 50 to 200 mL/min.
Further preferably, in step S3, the mixture is preferably heated from room temperature to 700 to 900 ℃ at a rate of 3 to 8 ℃/min under an inert gas atmosphere, and carbonized for 0.5 to 4 hours.
Further preferably, in step S4, the modification treatment is preferably performed by using low-temperature plasma of 30KV to 40KV operating voltage.
According to another aspect of the invention, a corresponding biomass porous carbon adsorbent product is also provided.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
1. the invention fully considers the influence of the aperture, the surface chemistry and the like on CO2The adsorption factor is researched and designed for porous carbon and the like, natural biomass is used as a carbon source, the cost is low, the source is wide, and the energy is saved and the cleanness is realized. Compared with the existing preparation process mode, the preparation method has the advantages that the preparation steps are simplified, the reaction conditions are mild, simple and reliable, the operation and the control are convenient, and the high-quality biomass porous carbon adsorbent can be realized;
2. the surface performance of the material is further improved by introducing the heteroatom into the surface of the material by adopting a low-temperature plasma modification method, the treatment conditions are air atmosphere, normal temperature and normal pressure, the treatment time is short, the efficiency is high, the cost is low, other properties of the material are not influenced, and the use of expensive and polluting modifiers is avoided;
3. on the whole, the invention utilizes the biomass as the raw material to directly prepare the high-quality porous carbon by a simplified methodThe adsorbent has low cost, simple and reliable preparation method and easy industrial application. The prepared porous carbon material has large specific surface area, developed pore structure and abundant surface active sites, and is favorable for realizing CO2High-efficiency adsorption, and is CO with great industrial application prospect2The material is captured.
Drawings
Fig. 1 is an overall flow diagram of a method for preparing a biomass porous carbon adsorbent according to the present invention;
FIG. 2 is a sample prepared in example 1, and is used to show that the porous carbon adsorbent is at 30 deg.C for CO2CO under simulated flue gas with partial pressure of 15%2Schematic of the Capacity.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. 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.
Fig. 1 is a schematic overall flow diagram of a preparation method of a biomass porous carbon adsorbent according to the present invention. The preparation route, especially the key process conditions of a plurality of important steps, is researched and designed again, easily available natural biomass is used as a raw material, a simplified method is adopted to synthesize the porous carbon material, and the advantages of a low-temperature plasma modification technology are combined to directly prepare the high-quality porous carbon adsorbent. This will be explained in detail with reference to fig. 1.
First, the biomass screen is mixed with an activator.
For example, bark, leaves, wood chips and other naturally occurring biomass materials are selected as the char source, washed and dried. Crushing and screening the biomass into biomass powder of 50-200 meshes, preferably 80-150 meshes; then, the biomass powder and KOH are sufficiently mixed in a mass ratio of 1:0.2 to 1: 1. In a preferred embodiment, the biomass powder of 100 meshes and the activating agent KOH are fully mixed and ground in a mass ratio of 1: 0.4-1: 0.8.
Next, a carbonization step is performed.
And transferring the mixture to a tubular furnace, heating the mixture from room temperature to 600-1000 ℃ at the speed of 3-8 ℃/min under the inert gas atmosphere, carbonizing the mixture for 0.5-4 hours, washing the carbonized mixture with 10 wt.% of dilute hydrochloric acid to remove impurities, and drying the washed mixture to obtain the porous carbon material. In another preferred embodiment, the mixture is carbonized at 700 ℃ to 900 ℃ for 1 hour to 3 hours to obtain porous carbon.
Finally, the low-temperature plasma modification treatment step is carried out.
And grinding and crushing the porous carbon product obtained in the step, and then modifying the ground porous carbon product for 0.5-30 minutes in an air atmosphere by adopting low-temperature plasma with the working voltage of 20-60 KV, thereby obtaining the required porous carbon adsorbent product. In a preferred embodiment, the operating voltage of the low-temperature plasma is further designed to be 30KV to 50KV, and the processing time may be further designed to be 1 minute to 20 minutes.
Several examples are set forth below to more fully explain the detailed implementation of the present invention and the selection of key process parameters.
Example 1
Crushing the leaves in a crusher, sieving to 150 meshes, taking 3g of leaf powder, and fully mixing and grinding the leaf powder and an activating agent KOH according to the weight ratio of 1: 0.8.
And putting the ground mixture into a corundum boat, putting the corundum boat into a tubular furnace, and carbonizing the corundum boat for 1h at 700 ℃ in a nitrogen atmosphere. Naturally cooling to room temperature, washing with 10 wt.% dilute hydrochloric acid to remove impurities, washing, and drying.
And grinding the carbonized product, flatly paving the ground product on a lower-stage plate of a low-temperature plasma generator, and treating the product for 20min under the air atmosphere with the working voltage of 40KV to obtain the porous carbon adsorbent PC-1.
Example 2
The sawdust is put into a grinder to be ground, the sawdust is sieved to 150 meshes, 3g of sawdust powder is taken and fully mixed and ground with an activating agent KOH according to the weight ratio of 1: 0.6.
And putting the ground mixture into a corundum boat, putting the corundum boat into a tubular furnace, and carbonizing the corundum boat for 1h at 800 ℃ in a nitrogen atmosphere. Naturally cooling to room temperature, washing with 10 wt.% dilute hydrochloric acid to remove impurities, washing, and drying.
And grinding the carbonized product, flatly paving the ground product on a lower-stage plate of a low-temperature plasma generator, and treating the product for 10min under the air atmosphere with the working voltage of 40KV to obtain the porous carbon adsorbent PC-2.
Example 3
The sawdust is put into a grinder to be ground, the sawdust is sieved to 100 meshes, 3g of sawdust powder is taken and fully mixed and ground with an activating agent KOH according to the weight ratio of 1: 0.5.
And putting the ground mixture into a corundum boat, putting the corundum boat into a tubular furnace, and carbonizing the corundum boat for 1h at 800 ℃ in a nitrogen atmosphere. Naturally cooling to room temperature, washing with 8 wt.% dilute hydrochloric acid to remove impurities, washing, and drying.
And grinding the carbonized product, flatly paving the ground product on a lower-stage plate of a low-temperature plasma generator, and treating for 5min under the air atmosphere with the working voltage of 50KV to obtain the porous carbon adsorbent PC-3.
Example 4
Crushing the leaves in a crusher, sieving to 100 meshes, taking 3g of leaf powder, and fully mixing and grinding the leaf powder and an activating agent KOH according to the weight ratio of 1: 0.4.
And putting the ground mixture into a corundum boat, putting the corundum boat into a tubular furnace, and carbonizing the corundum boat for 3 hours at 700 ℃ in a nitrogen atmosphere. Naturally cooling to room temperature, washing with 10 wt.% dilute hydrochloric acid to remove impurities, washing, and drying.
And grinding the carbonized product, flatly paving the ground product on a lower-stage plate of a low-temperature plasma generator, and treating for 3min under the air atmosphere with the working voltage of 40KV to obtain the porous carbon adsorbent PC-4.
Example 5
Crushing bark in a crusher, sieving to 100 mesh, mixing 3g of bark powder with activating agent KOH at a weight ratio of 1:0.5, and grinding.
And putting the ground mixture into a corundum boat, putting the corundum boat into a tubular furnace, and carbonizing the corundum boat for 2 hours at 700 ℃ in a nitrogen atmosphere. Naturally cooling to room temperature, washing with 9 wt.% dilute hydrochloric acid to remove impurities, washing, and drying.
And grinding the carbonized product, flatly paving the ground product on a lower-stage plate of a low-temperature plasma generator, and treating for 3min under the air atmosphere with the working voltage of 30KV to obtain the porous carbon adsorbent PC-5.
Example 6
The sawdust is put into a grinder to be ground, the sawdust is sieved to 80 meshes, 3g of sawdust powder is taken and fully mixed and ground with an activating agent KOH according to the weight ratio of 1: 0.6.
And putting the ground mixture into a corundum boat, putting the corundum boat into a tubular furnace, and carbonizing the corundum boat for 1h at 800 ℃ in a nitrogen atmosphere. Naturally cooling to room temperature, washing with 10 wt.% dilute hydrochloric acid to remove impurities, washing, and drying.
And grinding the carbonized product, flatly paving the ground product on a lower-stage plate of a low-temperature plasma generator, and treating the product for 1min under the air atmosphere with the working voltage of 50KV to obtain the porous carbon adsorbent PC-6.
Example 7
Crushing bark in a crusher, sieving to 100 mesh, mixing 3g of bark powder with activating agent KOH at a weight ratio of 1:0.6, and grinding.
And putting the ground mixture into a corundum boat, putting the corundum boat into a tubular furnace, and carbonizing the corundum boat for 1h at 700 ℃ in a nitrogen atmosphere. Naturally cooling to room temperature, washing with 8.5 wt.% dilute hydrochloric acid to remove impurities, washing, and drying.
And grinding the carbonized product, flatly paving the ground product on a lower-stage plate of a low-temperature plasma generator, and treating for 5min under the air atmosphere with the working voltage of 40KV to obtain the porous carbon adsorbent PC-7.
The sample prepared in example 1 is used as an example, and the porous carbon adsorbent is shown in FIG. 2 at 30 deg.C for CO2CO under simulated flue gas with partial pressure of 15%2A capture capability.
Referring to fig. 2, it can be clearly seen that: the porous carbon prepared by the simplified steps has good CO under simulated smoke conditions2Adsorption property, and canTo realize CO2Rapid adsorption of 90% CO2The adsorption is completed within 10min, and the method has good application prospect.
CO of examples 1 to 7 above2The adsorption performance test method is as follows: place the sample in a thermogravimetric analyzer at N2Increasing the temperature from room temperature to 105 deg.C at a rate of 10 deg.C/min under atmosphere, degassing for 30min, cooling to 30 deg.C after degassing, and introducing 15 vol% CO2Testing porous carbon in CO2CO under simulated flue gas with partial pressure of 15%2The adsorption capacity, the change of the weight in the period is CO2The amount of adsorption.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. Is suitable for flue gas CO2The preparation method of the adsorbed biomass porous carbon is characterized by comprising the following steps:
s1, selecting biomass as a charcoal source, washing the biomass with water, drying the biomass, and then crushing and screening the biomass into powder of 50-200 meshes;
s2, mixing and grinding the biomass powder and KOH serving as an activating agent according to the mass ratio of 1: 0.2-1: 1;
s3, transferring the mixture into a tube furnace, heating the mixture from room temperature to 600-1000 ℃ at the speed of 2-10 ℃/min in the nitrogen atmosphere, and carbonizing the mixture for 0.5-4 hours; then, naturally cooling to room temperature in a nitrogen atmosphere, washing with 8-10 wt.% dilute hydrochloric acid to remove impurities, and drying after washing to obtain a carbonized product;
s4, grinding and crushing the obtained carbonized product, and then modifying the ground and crushed carbonized product for 0.5-30 minutes in air atmosphere by adopting low-temperature plasma with 20-60 KV working voltage, thereby obtaining the required porous carbon adsorbent product for flue gas CO2And (4) adsorbing.
2. The method for preparing the biomass porous carbon according to claim 1, wherein in the step S1, the biomass is one or a combination of the following substances: bark, leaves and wood chips.
3. The method for preparing porous biomass charcoal according to claim 1, wherein in step S1, the carbon source is pulverized and sieved to powder of 80-150 mesh.
4. The method for preparing the biomass porous carbon according to claim 1, wherein in step S2, the biomass powder and the activator are mixed and ground at a mass ratio of 1:0.4 to 1: 0.8.
5. The method for producing biomass porous carbon according to claim 1, wherein in step S3, the gas flow rate of nitrogen is set to 50mL/min to 200 mL/min.
6. The method for preparing biomass porous carbon according to claim 1, wherein in step S3, the mixture is heated from room temperature to 700-900 ℃ at a rate of 3-8 ℃/min under nitrogen atmosphere, and carbonized for 0.5-4 hours.
7. The method for preparing porous biomass carbon according to any one of claims 1 to 6, wherein in step S4, the modification treatment is performed by using low-temperature plasma at an operating voltage of 30KV to 40 KV.
8. A biomass porous carbon adsorbent product prepared by the method of any one of claims 1 to 7 and used for flue gas CO of coal-fired power plant2In the case of capture.
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| CN110745808B (en) * | 2019-12-04 | 2023-01-24 | 西安科技大学 | Method for preparing foam carbon based on heavy tar generated by pyrolysis of rich coal |
| CN110935420A (en) * | 2019-12-11 | 2020-03-31 | 福州大学 | Normal pressure CO2Preparation method of hierarchical pore activated carbon adsorbent |
| CN113648966A (en) * | 2021-08-10 | 2021-11-16 | 南京航空航天大学 | Biomass porous carbon material and preparation method and application thereof |
| CN114988404A (en) * | 2022-06-07 | 2022-09-02 | 北京石大油源科技开发有限公司 | Preparation method of efficient solid adsorption carbon capture material |
| CN115140737A (en) * | 2022-06-30 | 2022-10-04 | 潍坊学院 | Process for preparing peanut shell-based activated carbon by one-step activation method and CO 2 Application of trapping |
| CN117623302A (en) * | 2023-12-01 | 2024-03-01 | 浙江大学 | Preparation method and application of heteroatom doped biochar |
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| CN104549153A (en) * | 2015-01-14 | 2015-04-29 | 福建紫荆环境工程技术有限公司 | Device and method for modifying activated carbon adsorbent by using rotating low-temperature plasma |
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| CN106031860A (en) * | 2016-03-24 | 2016-10-19 | 华东理工大学 | Nano-porous material pore channel inner surface plasma modification treatment method and application |
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