CN110327879A - One kind being suitable for flue gas CO2The biomass porous carbon preparation method and product of absorption - Google Patents

One kind being suitable for flue gas CO2The biomass porous carbon preparation method and product of absorption Download PDF

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CN110327879A
CN110327879A CN201910508935.3A CN201910508935A CN110327879A CN 110327879 A CN110327879 A CN 110327879A CN 201910508935 A CN201910508935 A CN 201910508935A CN 110327879 A CN110327879 A CN 110327879A
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biomass
porous carbon
flue gas
preparation
carbon preparation
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CN110327879B (en
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刘晶
吴大卫
沈锋华
董昱辰
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Huazhong University of Science and Technology
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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
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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 flue gas pollutants to control correlative technology field, and disclose a kind of suitable for flue gas CO2The biomass porous carbon preparation method of absorption, include: coarse biometric quality sample it is washed, it is dry, crush and obtain powdered biomass after sieving, by powdered biomass and activator KOH mixed grinding, heating executes carbonization reaction under an inert atmosphere, after naturally cool to room temperature；The carbonizing production generated is ground, processing is then modified to charing powder in air atmosphere using low temperature plasma.The invention also discloses corresponding biomass porous carbon adsorbent products.By means of the invention it is possible to produce the porous carbon adsorbent of high-quality using biomass material, preparation method is simple, low in cost, and effect on environment is small, is easy to industrial applications.

Description

One kind being suitable for flue gas CO2The biomass porous carbon preparation method and product of absorption
Technical field
The invention belongs to flue gas pollutants to control correlative technology field, be suitable for flue gas CO more particularly, to one kind2It inhales Attached biomass porous carbon preparation method and product.
Background technique
The greenhouse gases of mankind's activity discharge have caused the serious environmental problem such as global warming and climatic deterioration, compromise Natural ecosystems have brought tremendous economic losses to human society.CO2It is most important greenhouse gases.Coal-burning power plant is Most important CO2Emission source, therefore the CO of coal-burning power plant2Capture is the significant challenge that human society faces.
Currently, CO2Capture technique mainly includes capture and oxygen-rich combustion method after burning preceding capture, burning.It is captured after burning Compared with other two methods, with advantage at low cost, applicability is good, there is wide market potential.Catching method after burning Including amine absorption process, membrane separation process, absorption method etc..Wherein, amine absorption process technology is more mature, but can corrode equipment, to environment It pollutes.The cost is relatively high for membrane separation process, is unfavorable for utilizing on a large scale.Current most promising technology is absorption method, Its core is to develop efficient, cheap adsorbent.In a variety of adsorbents, porous charcoal is due to its high porosity, stability is good, Energy is low etc. that advantages receive more and more attention for regeneration.
Reproducible biomass can be used as the raw material of porous charcoal, reduce the cost of porous charcoal, make it have wide Application prospect.The preparation process of some biomass porous carbon adsorbents has been proposed in the prior art.For example, CN201510939918.7 discloses a kind of porous charcoal CO2The preparation method of adsorbent, which disclose can take stalk conduct Biomass material obtains presoma by hydro-thermal reaction, then carries out chemical activation with KOH to improve the specific surface area of adsorbent And microcellular structure.For another example, CN201810454278.4 discloses a kind of biomass carbon base CO2Adsorbent and preparation method thereof, In disclose and can take chitosan that fused salt mixt pyrolysis is added to obtain intermediate product, high-temperature calcination is then carried out, finally by washing It washs away fused salt mixt and obtains adsorbent.In addition, CN201210252491.X discloses a kind of metal ion-modified charcoal Base CO2The preparation method of adsorbent, which disclose can be by the raw material of bamboo charcoal etc in CO2High-temperature activation is carried out under atmosphere, so It impregnates and is modified in metal nitrate or metal chloride aqueous solution afterwards, thus to obtain biological carbon-supported catalyst.
However, further investigations have shown that, above-mentioned existing scheme still has defect or deficiency below: above-mentioned preparation Complex process needs to carry out multistep reaction, it is difficult to realize large-scale production；Importantly, in above-mentioned porous charcoal preparation process More activating agent and modifying agent have been used, cost is not only increased, and has been easy to pollute the environment.Correspondingly, this field It needs to make this further research and improve, preferably to meet modernization coal-burning power plant CO2The demand of capture.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides one kind to be suitable for flue gas CO2Absorption Biomass porous carbon preparation method and product, wherein the not raw material for preparing only with biomass as porous charcoal, and further Combine flue gas CO2 absorption certain applications demand come to its preparation route and multiple critical crafts etc. again into Gone research and design, accordingly compared with prior art, it is no longer necessary to use a large amount of activator, can sufficiently combine low temperature etc. from Sub- modification technology promotes CO2The Heteroatom doping of absorption is avoided into porous charcoal using valuableness and with the modification of pollution Agent, while obtained porous charcoal product has the features such as high-specific surface area, abundant hole, more active sites, thus it is especially suitable The CO in coal-fired plant flue gas2The application of capture etc.
Correspondingly, according to one aspect of the present invention, it provides a kind of suitable for flue gas CO2The biomass porous carbon of absorption Preparation method, which is characterized in that this method includes the following steps:
S1, biomass is chosen as charcoal source, drying, then crushes and screens to 50 mesh~200 mesh powders after being eluted with water；
S2, above-mentioned powdered biomass and the KOH as activator are carried out into mixed grinding with the mass ratio of 1:0.2~1:1；
S3, said mixture is transferred in tube furnace, with 2 DEG C/min~10 DEG C/min speed under atmosphere of inert gases Rate carbonizes 0.5 hour~4 hours from room temperature to 600 DEG C~1000 DEG C；Then, naturally cold under atmosphere of inert gases But to room temperature, removal impurity is washed with the dilute hydrochloric acid of 8wt.%~10wt.%, it is dry after cleaning, obtain carbonizing production；
S4, carbonizing production obtained is ground, then uses the low-temperature plasma of 20KV~60KV operating voltage Thus body obtains required more to carbonizing production modification 0.5 minute~30 minutes after grinding under air atmosphere Hole carbon adsorbent product.
As it is further preferred that in step sl, the biomass is preferably one of following substance or combination: tree Skin, leaf and sawdust.
As it is further preferred that in step sl, carbon source crushing is preferably sized to 80 mesh~150 mesh powders.
As it is further preferred that in step s 2, the powdered biomass and the activator are preferably with 1:0.4~1: 0.8 mass ratio carrys out mixed grinding.
As it is further preferred that in step s3, the inert gas is preferably nitrogen, and its gas flow rate is preferably set It is set to 50mL/min~200mL/min.
As it is further preferred that in step s3, the mixture preferably under atmosphere of inert gases with 3 DEG C/min~ The rate of 8 DEG C/min carbonizes 0.5 hour~4 hours from room temperature to 700 DEG C~900 DEG C.
As it is further preferred that in step s 4, it is preferred to use the low temperature plasma of 30KV~40KV operating voltage Carry out the modification.
It is another aspect of this invention to provide that additionally providing corresponding biomass porous carbon adsorbent product.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below Technological merit:
1, the present invention has fully considered that aperture and surface chemistry etc. influence CO2The factor of absorption carries out porous charcoal etc. Research and design, use natural biomass for charcoal source, low in cost, from a wealth of sources, energy-saving clean.With existing preparation process Mode is compared, this invention simplifies preparation step, reaction condition is mild, it is simple and reliable, convenient for manipulation, high-quality may be implemented Biomass porous carbon adsorbent；
2, hetero atom is introduced into material surface by using low-temperature plasma modified method, further improves material table Face performance, treatment conditions be air atmosphere, normal temperature and pressure, short processing time, it is high-efficient, at low cost and do not influence material other Property is avoided using valuableness and with the modifying agent of pollution；
3, on the whole, the present invention directly produces the more of high-quality by simplified method using biomass as raw material Hole carbon adsorbent, low in cost, preparation method is simple and reliable, is easy to industrial applications.Prepared porous carbon material has big Specific surface area, flourishing pore structure and Adsorption abundant, be conducive to realize CO2Efficient absorption, because being a kind of great The CO of prospects for commercial application2Capture material.
Detailed description of the invention
Fig. 1 is the overall flow schematic diagram of biomass porous carbon sorbent preparation method according to the invention；
For Fig. 2 is the sample obtained by the embodiment 1, for show the porous carbon adsorbent at 30 DEG C, CO2Partial pressure is CO under 15% simulated flue gas2The schematic diagram of capture ability.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below Not constituting a conflict with each other can be combined with each other.
Fig. 1 is the overall flow schematic diagram of biomass porous carbon sorbent preparation method according to the invention.Wherein pass through Research and design have been re-started to the critical craft etc. of the especially multiple important steps of its preparation route, used what is be easy to get The advantages of natural biomass is raw material, synthesizes porous carbon material using simplified method, and combines low-temperature plasma modification technology, Directly produce the porous carbon adsorbent of high-quality.Specific explanations explanation is carried out to it below in conjunction with Fig. 1.
Firstly, being biomass screening and activator mixed process.
For example the naturally occurring biological material such as selection bark, leaf and sawdust is dry after washing as charcoal source.And it will Biomass crushes and screens as 50 mesh~200 mesh, further preferably 80 mesh~150 mesh powdered biomass；Then, by the biology Matter powder and KOH are sufficiently mixed with the mass ratio of 1:0.2~1:1.In one preferred embodiment, the biomass of 100 mesh Powder is sufficiently mixed grinding with activator KOH with the mass ratio of 1:0.4~1:0.8.
It then, is carbonization.
The mixture is transferred in tube furnace, under atmosphere of inert gases with 3 DEG C/min~8 DEG C/min rate from Room temperature carbonizes 0.5 hour~4 hours to 600 DEG C~1000 DEG C, washs removal impurity with the dilute hydrochloric acid of 10wt.%, washes It is dry after net, thus to obtain porous carbon material.In another preferred embodiment, mixture is carbonized in 700 DEG C~900 DEG C Obtain porous charcoal within 1 hour~3 hours.
Finally, being low-temperature plasma modifying processing step.
Above step porous product char obtained is ground, the low temperature of 20KV~60KV operating voltage is then used Plasma is modified processing 0.5 minute~30 minutes to the porous product char after grinding under air atmosphere, thus obtains Required porous carbon adsorbent product.In one preferred embodiment, the operating voltage of low temperature plasma is also further It is designed as 30KV~50KV, the processing time can be further designed to 1 minute~20 minutes.
Multiple embodiments are shown below, so that specific implementation process and its crucial work of the invention is more fully explained The selection of skill parameter.
Embodiment 1
It takes leaf to be put into pulverizer to crush, is sized to 150 mesh, take 3g leaf powder, with activator KOH with 1:0.8's Weight ratio is sufficiently mixed grinding.
Mixture after grinding is put into corundum boat, is placed in tube furnace, in a nitrogen atmosphere 700 DEG C of charing 1h.From It is so cooled to room temperature, washs removal impurity with the dilute hydrochloric acid of 10wt.%, it is dry after cleaning.
By the product grinding after charing, tiling is placed on the lower step of low-temperature plasma generator, in operating voltage 20min is handled under 40KV air atmosphere, obtains porous carbon adsorbent PC-1.
Embodiment 2
It takes sawdust to be put into pulverizer to crush, is sized to 150 mesh, take 3g sawdust powder, with activator KOH with 1:0.6's Weight ratio is sufficiently mixed grinding.
Mixture after grinding is put into corundum boat, is placed in tube furnace, in a nitrogen atmosphere 800 DEG C of charing 1h.From It is so cooled to room temperature, is washed with the dilute hydrochloric acid of 10wt.% and remove impurity, it is dry after cleaning.
By the product grinding after charing, tiling is placed on the lower step of low-temperature plasma generator, in operating voltage 10min is handled under 40KV air atmosphere, obtains porous carbon adsorbent PC-2.
Embodiment 3
It takes sawdust to be put into pulverizer to crush, is sized to 100 mesh, take 3g sawdust powder, with activator KOH with 1:0.5's Weight ratio is sufficiently mixed grinding.
Mixture after grinding is put into corundum boat, is placed in tube furnace, in a nitrogen atmosphere 800 DEG C of charing 1h.From It is so cooled to room temperature, is washed with the dilute hydrochloric acid of 8wt.% and remove impurity, it is dry after cleaning.
By the product grinding after charing, tiling is placed on the lower step of low-temperature plasma generator, in operating voltage 5min is handled under 50KV air atmosphere, obtains porous carbon adsorbent PC-3.
Embodiment 4
It takes leaf to be put into pulverizer to crush, is sized to 100 mesh, take 3g leaf powder, with activator KOH with 1:0.4's Weight ratio is sufficiently mixed grinding.
Mixture after grinding is put into corundum boat, is placed in tube furnace, in a nitrogen atmosphere 700 DEG C of charing 3h.From It is so cooled to room temperature, is washed with the dilute hydrochloric acid of 10wt.% and remove impurity, it is dry after cleaning.
By the product grinding after charing, tiling is placed on the lower step of low-temperature plasma generator, in operating voltage 3min is handled under 40KV air atmosphere, obtains porous carbon adsorbent PC-4.
Embodiment 5
It takes bark to be put into pulverizer to crush, is sized to 100 mesh, take 3g bark fines, with activator KOH with 1:0.5's Weight ratio is sufficiently mixed grinding.
Mixture after grinding is put into corundum boat, is placed in tube furnace, in a nitrogen atmosphere 700 DEG C of charing 2h.From It is so cooled to room temperature, is washed with the dilute hydrochloric acid of 9wt.% and remove impurity, it is dry after cleaning.
By the product grinding after charing, tiling is placed on the lower step of low-temperature plasma generator, in operating voltage 3min is handled under 30KV air atmosphere, obtains porous carbon adsorbent PC-5.
Embodiment 6
It takes sawdust to be put into pulverizer to crush, is sized to 80 mesh, take 3g sawdust powder, with activator KOH with the weight of 1:0.6 Amount ratio is sufficiently mixed grinding.
Mixture after grinding is put into corundum boat, is placed in tube furnace, in a nitrogen atmosphere 800 DEG C of charing 1h.From It is so cooled to room temperature, is washed with the dilute hydrochloric acid of 10wt.% and remove impurity, it is dry after cleaning.
By the product grinding after charing, tiling is placed on the lower step of low-temperature plasma generator, in operating voltage 1min is handled under 50KV air atmosphere, obtains porous carbon adsorbent PC-6.
Embodiment 7
It takes bark to be put into pulverizer to crush, is sized to 100 mesh, take 3g bark fines, with activator KOH with 1:0.6's Weight ratio is sufficiently mixed grinding.
Mixture after grinding is put into corundum boat, is placed in tube furnace, in a nitrogen atmosphere 700 DEG C of charing 1h.From It is so cooled to room temperature, is washed with the dilute hydrochloric acid of 8.5wt.% and remove impurity, it is dry after cleaning.
By the product grinding after charing, tiling is placed on the lower step of low-temperature plasma generator, in operating voltage 5min is handled under 40KV air atmosphere, obtains porous carbon adsorbent PC-7.
Below by for the sample obtained by the embodiment 1, in conjunction with Fig. 2 show the porous carbon adsorbent at 30 DEG C, CO2Point Pressure is the CO under 15% simulated flue gas2Capture ability.
Referring to Fig. 2, it is apparent that: the porous charcoal by simplifying step preparation has to be had under the conditions of simulated flue gas There is good CO2Absorption property, and CO may be implemented2Quick adsorption, 90% CO2The time for being adsorbed on 10min completes, It has a good application prospect.
The CO of above embodiments 1~72Absorption property test method is as described below: sample is put in thermogravimetric analyzer, N2105 DEG C and the 30min that deaerates are risen to from room temperature with the rate of 10 DEG C/min under atmosphere, temperature is cooled to 30 after the completion of degassing DEG C, it is subsequently passed the CO of volume fraction 15%2, porous charcoal is tested in CO2Partial pressure is the CO under 15% simulated flue gas2Adsorption energy Power, during which weight change amount is CO2Adsorbance.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include Within protection scope of the present invention.

Claims (8)

1. one kind is suitable for flue gas CO2The biomass porous carbon preparation method of absorption, which is characterized in that this method includes following step It is rapid:
S1, biomass is chosen as charcoal source, drying, then crushes and screens to 50 mesh~200 mesh powders after being eluted with water；
S2, above-mentioned powdered biomass and the KOH as activator are carried out into mixed grinding with the mass ratio of 1:0.2~1:1；
S3, said mixture is transferred in tube furnace, under atmosphere of inert gases with 2 DEG C/min~10 DEG C/min rate from Room temperature carbonizes 0.5 hour~4 hours to 600 DEG C~1000 DEG C；Then, it is naturally cooled under atmosphere of inert gases Room temperature washs removal impurity with the dilute hydrochloric acid of 8wt.%~10wt.%, dry after cleaning, and obtains carbonizing production；
S4, carbonizing production obtained is ground, then uses the low temperature plasma of 20KV~60KV operating voltage, in To carbonizing production modification 0.5 minute~30 minutes after grinding under air atmosphere, required porous charcoal is thus obtained Adsorbent product.
2. biomass porous carbon preparation method as described in claim 1, which is characterized in that in step sl, the biomass One of preferably following substance or combination: bark, leaf and sawdust.
3. biomass porous carbon preparation method as claimed in claim 1 or 2, which is characterized in that in step sl, preferably by carbon Source is crushed and screened to 80 mesh~150 mesh powders.
4. biomass porous carbon preparation method as claimed in any one of claims 1-3, which is characterized in that in step s 2, The powdered biomass and the activator preferably carry out mixed grinding with the mass ratio of 1:0.4~1:0.8.
5. the biomass porous carbon preparation method as described in claim 1-4 any one, which is characterized in that in step s3, The inert gas is preferably nitrogen, and its gas flow rate is preferably set to 50mL/min~200mL/min.
6. the biomass porous carbon preparation method as described in claim 1-5 any one, which is characterized in that in step s3, The mixture is preferably under atmosphere of inert gases with 3 DEG C/min~8 DEG C/min rate from room temperature to 700 DEG C~900 DEG C, and carbonize 0.5 hour~4 hours.
7. biomass porous carbon preparation method as claimed in any one of claims 1 to 6, which is characterized in that in step s 4, It is preferred that the low temperature plasma using 30KV~40KV operating voltage carries out the modification.
8. a kind of biomass porous carbon adsorbent product uses the method as described in claim 1-7 any one and is made, And it is used for coal-fired plant flue gas CO2The occasion of capture.
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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
CN114713188A (en) * 2022-03-04 2022-07-08 浙江工业大学 Carbon dioxide adsorbing material and preparation method thereof
CN114713188B (en) * 2022-03-04 2024-04-30 浙江工业大学 Carbon dioxide adsorption material and preparation method 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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