CN117247011A - Preparation method of active carbon with high benzene series adsorption rate and active carbon - Google Patents
Preparation method of active carbon with high benzene series adsorption rate and active carbon Download PDFInfo
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- CN117247011A CN117247011A CN202311525359.6A CN202311525359A CN117247011A CN 117247011 A CN117247011 A CN 117247011A CN 202311525359 A CN202311525359 A CN 202311525359A CN 117247011 A CN117247011 A CN 117247011A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 221
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 93
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 title abstract 6
- 238000002791 soaking Methods 0.000 claims abstract description 55
- 239000002243 precursor Substances 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 23
- 239000003929 acidic solution Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000012670 alkaline solution Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000003763 carbonization Methods 0.000 claims abstract description 13
- 230000004913 activation Effects 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 4
- 150000001555 benzenes Chemical class 0.000 claims description 83
- 238000000034 method Methods 0.000 claims description 21
- 239000011148 porous material Substances 0.000 claims description 21
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 20
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 20
- 241001330002 Bambuseae Species 0.000 claims description 20
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 20
- 239000011425 bamboo Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 10
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 10
- SJRJJKPEHAURKC-UHFFFAOYSA-N N-Methylmorpholine Chemical compound CN1CCOCC1 SJRJJKPEHAURKC-UHFFFAOYSA-N 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- -1 ethylenediamine, tetramethyl Chemical group 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 6
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 6
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 6
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 230000003213 activating effect Effects 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 6
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910052740 iodine Inorganic materials 0.000 claims description 6
- 239000011630 iodine Substances 0.000 claims description 6
- 238000004898 kneading Methods 0.000 claims description 6
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 6
- 239000002028 Biomass Substances 0.000 claims description 5
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 claims description 4
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 4
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- YPJUNDFVDDCYIH-UHFFFAOYSA-N perfluorobutyric acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)F YPJUNDFVDDCYIH-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims description 4
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 125000002619 bicyclic group Chemical group 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 3
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 3
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 13
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 12
- 230000006872 improvement Effects 0.000 description 9
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000003245 coal Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 241000282414 Homo sapiens Species 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 4
- 230000001788 irregular Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000011257 shell material Substances 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- 235000013162 Cocos nucifera Nutrition 0.000 description 3
- 244000060011 Cocos nucifera Species 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 150000007530 organic bases Chemical class 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000005539 carbonized material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
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Classifications
-
- 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
- C01B32/354—After-treatment
- C01B32/36—Reactivation or regeneration
-
- 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
-
- 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
-
- 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
- C01B32/354—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7027—Aromatic hydrocarbons
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of active carbon with high benzene series adsorption rate and the active carbon, belongs to the technical field of benzene series adsorption, and solves the technical problem of low benzene series adsorption rate in the prior art. The preparation method of the activated carbon with high benzene series adsorption rate comprises the following steps: obtaining active carbon prepared by carbonization and activation; soaking active carbon in a first acidic solution, and washing to neutrality after the soaking is completed to obtain a first precursor; soaking the first precursor in a second acidic solution, and washing to neutrality after the soaking is finished to obtain a second precursor; soaking the second precursor in an alkaline solution, and drying after the soaking is finished to obtain a third precursor; performing heat treatment on the third precursor to obtain the active carbon with high benzene series adsorption rate; wherein the first acidic solution contains organic strong acid; the second acidic solution contains a strong inorganic acid.
Description
Technical Field
The invention relates to the technical field of benzene series adsorption, in particular to a preparation method of active carbon with high benzene series adsorption rate and the active carbon.
Background
Benzene series is a general term of benzene derivatives, and refers to benzene-containing ring compounds which have certain distribution in the environment of human production and living and are harmful to human bodies in a narrow sense. Besides industrial fumes and waste water, benzene series are widely available in daily life, such as automobile exhaust, additives for organic solvents such as paint in building decoration materials, adhesives and artificial board furniture which are common in daily life, are pollution sources of benzene series compounds, and benzene series have been widely detected in human living and living environments.
Benzene compounds have a serious negative effect on the regional, in particular urban, atmospheric environment. Since most benzene compounds (such as benzene, toluene, etc.) have strong volatility, the benzene compounds are easily volatilized into gas under normal temperature to form volatile organic (Volatile Organic Compounds, i.e. VOCs) gas, which can cause the pollution of the VOCs gas. Meanwhile, in the pollution of wastewater, such as coking wastewater containing benzene series, the pollution is also very harmful to human beings. Benzene series can have strong harm to blood, nerves and reproductive systems of human bodies.
The benzene series is classified into two main types, namely, decomposition and recovery, depending on the purpose of control. Wherein, the recovery technology mainly uses physical control technology, and concretely comprises an adsorption method, a condensation concentration method, a membrane separation method and the like. Activated carbon adsorption is widely used because of low cost of raw materials and high adsorption rate. However, most of the existing active carbon materials in the market mainly comprise coal, fruit shells and coconut shells, wherein the coal is used as the main material; the coal resources are increasingly available and cost due to the increasingly heavy environmental awareness, limited total amount of the coal resources and the like, and the adsorption rate of the coal-based activated carbon is limited to increase, so that the market ratio of the coal-based activated carbon is increasingly reduced; activated carbon of the shell and coconut shell materials generally has high adsorption rate, but is limited by the reason that the materials are difficult to obtain, the price is always high, and the quality of the shell and coconut shell activated carbon is uneven at present.
The applicant of the present application has proposed in the prior application that bamboo is used as a biomass raw material, and the prepared activated carbon has developed pores and low raw material cost. Although the micropores of the activated carbon are developed, a certain amount of benzene series can be adsorbed, the mesoporous volume of the activated carbon is relatively low, and the diffusion of the benzene series to the micropores in the activated carbon is not facilitated, so that the adsorption of benzene series molecules is influenced.
Disclosure of Invention
The invention mainly aims to provide a preparation method of active carbon with developed micropores and proper mesopores and high benzene series adsorption rate, and the active carbon, so as to solve the technical problem of low benzene series adsorption rate in the prior art.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing activated carbon with high benzene series adsorption rate, which comprises the following steps.
The preparation method of the active carbon with high benzene series adsorption rate is characterized by comprising the following steps: the method comprises the following steps:
obtaining active carbon prepared by carbonization and activation;
soaking active carbon in a first acidic solution, and washing to neutrality after the soaking is completed to obtain a first precursor;
soaking the first precursor in a second acidic solution, and washing to neutrality after the soaking is finished to obtain a second precursor;
soaking the second precursor in an alkaline solution, and drying after the soaking is finished to obtain a third precursor;
performing heat treatment on the third precursor to obtain the active carbon with high benzene series adsorption rate;
wherein the first acidic solution contains organic strong acid; the second acidic solution contains a strong inorganic acid.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the organic strong acid is sulfonic acid or perhalogenated carboxylic acid; the sulfonic acid is any one of methanesulfonic acid, benzenesulfonic acid and dodecylbenzenesulfonic acid; the perhalogenated carboxylic acid is any one of trichloroacetic acid, perfluorobutyric acid and perfluorooctanoic acid; the inorganic strong acid is any one of hydrochloric acid, sulfuric acid and nitric acid.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the mass fraction of the first acidic solution is 2-4%, and the soaking time is 10-30 minutes.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the mass fraction of the second acid solution is 3-5%, and the soaking time is 20-40 minutes.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the alkaline solution contains organic alkali, wherein the organic alkali is any one of propylene diamine, ethylenediamine, tetramethyl ethylenediamine, triethylene diamine, pyridine diamine, 4-dimethylaminopyridine, N-methylmorpholine, tetramethyl guanidine, hexatomic bicyclic guanidine, triaza bicyclo and diazabicyclo.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the mass fraction of the alkaline solution is 4-6%, and the soaking time is 1-2 h; after the impregnation is finished, distilled water is adopted for washing for 2 to 4 times, and then standing is carried out for 2 to 10 hours, and then drying is carried out.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the step of obtaining the activated carbon prepared by carbonization and activation comprises the following steps:
carbonizing biomass raw materials to obtain carbon powder;
kneading carbon powder and an adhesive, and extruding and molding to obtain a blank;
and (3) performing activation treatment on the green body to obtain the activated carbon.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the biomass raw material is bamboo; the carbonization treatment is carbonization for 3-5 hours at 550-600 ℃; the activation treatment is to activate for 2-5 hours at 800-900 ℃, and the activating agent is water vapor.
As a further improvement of the preparation method of the high benzene series adsorption rate active carbon, the following steps are adopted: the heat treatment is an anaerobic heat treatment for 1.5 to 2 hours at the temperature of 400 to 500 ℃.
In order to achieve the above object, according to a second aspect of the present invention, there is also provided activated carbon, which has the following technical scheme:
the activated carbon is prepared by the preparation method of the high benzene series adsorption rate activated carbon; the micropore volume of the activated carbon is 0.5-0.6 mL/g, the mesoporous volume is 0.09-0.11mL/g, the average pore diameter is 0.9-1 nm, and the specific surface area is 1300-1400 m 2 The iodine adsorption value per gram is 1100-1200 mg/g, and the adsorption rate of benzene series is more than or equal to 50%.
Therefore, the preparation method of the activated carbon with high benzene series adsorption rate has the following advantages:
firstly, on the basis of the traditional inorganic strong acid, the invention also adopts the organic strong acid to pretreat the activated carbon, thereby producing the following beneficial effects: (1) The impurities in the activated carbon are removed more thoroughly, so that on one hand, the impurities are prevented from affecting the adsorption of benzene series, and on the other hand, the impurities are prevented from obstructing the subsequent pore-forming process. (2) The depth removal of impurities in the activated carbon enables the specific surface area of the activated carbon to be obviously improved, and further enables the pore-forming action area of subsequent alkaline substances to be obviously improved, so that the pore-forming effect is improved. (3) Through the deep removal of impurities, a certain number of mesopores and macropores are formed in the activated carbon, so that the diffusion of benzene series molecules to micropores is facilitated, and the adsorption capacity to benzene series is improved. (4) The organic strong acid is used before the inorganic strong acid, so that the number of acid groups on the surface of the second precursor can be reduced as much as possible, and the influence of the acid groups on the adsorption of benzene series is reduced. (5) The traditional bamboo activated carbon needs to be carbonized twice, but in the invention, the two-stage strong acid acidification process can achieve a certain carbonization effect, so that the second carbonization can be omitted, thereby saving energy consumption to a certain extent.
Secondly, the invention does not use traditional inorganic strong alkali such as sodium hydroxide and potassium hydroxide to carry out pore formation, but adopts weak alkaline or medium-strong alkaline organic alkali to carry out pore formation, and the pore formation reaction intensity is proper, so that on one hand, the micropore volume can be increased, meanwhile, the proper number of mesopores can be increased, the uniformity of pore size distribution is improved, and on the other hand, alkaline groups can be introduced on the surface of the activated carbon, thereby being beneficial to the adsorption of benzene series.
Therefore, the preparation method of the high benzene series adsorption rate active carbon has the advantages of simple process, low raw material cost and easy control, the obtained active carbon has high specific surface area, total pore volume and micropore volume, moderate increase of mesoporous quantity and high benzene series adsorption rate, effectively solves the technical problem of low benzene series adsorption rate of the bamboo active carbon in the prior art, and has extremely strong practicability.
Examples of the invention provided in this specification are further described below with reference to the accompanying drawings and detailed description. Additional aspects and advantages of embodiments of the invention provided in the specification will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of embodiments of the invention provided in the specification.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain, without undue limitation, the embodiments of the invention.
FIG. 1 is a low-magnification SEM photograph of a high benzene series adsorption rate active carbon of example 1 of the present invention.
FIG. 2 is a high-magnification SEM photograph of the high benzene series adsorption rate active carbon of example 1 of the present invention.
FIG. 3 is a graph showing N of the high benzene series adsorption rate activated carbon and the blank activated carbon of example 1 of the present invention 2 Adsorption and desorption curves are compared with the graph.
FIG. 4 is a graph showing the comparison of pore size distribution of the high benzene series adsorption rate activated carbon and the blank activated carbon according to example 1 of the present invention.
Detailed Description
The following provides a clear and complete description of the inventive embodiments provided in this specification in connection with the accompanying drawings. Those skilled in the art will be able to implement the embodiments of the invention provided herein based on these descriptions. Before describing embodiments of the invention provided in this specification with reference to the drawings, it should be noted in particular that:
in the embodiments of the invention provided in the present specification, the technical solutions and technical features provided in the respective sections including the following description may be combined with each other without conflict.
Moreover, the embodiments of the invention provided in the present specification referred to in the following description are generally only some, but not all, embodiments of the invention provided in the present specification, and therefore, all other embodiments obtained by a person having ordinary skill in the art based on the embodiments of the invention provided in the present specification without making any inventive effort shall fall within the scope of protection of the embodiments of the invention provided in the present specification.
Terms and units in the examples of the invention provided in the present specification: the terms "comprising," "including," "having," and any variations thereof, in the description and claims of embodiments of the invention and in the relevant parts, are intended to cover a non-exclusive inclusion. In addition, other related terms and units in the embodiments of the invention provided in the present specification can be reasonably interpreted based on the related contents of the embodiments of the invention provided in the present specification.
The specific implementation mode of the preparation method of the high benzene series adsorption rate active carbon comprises the following steps:
(1) Obtaining active carbon prepared by carbonization and activation;
and (3) bamboo wood treatment: processing fresh bamboo or waste bamboo into bamboo blocks with arbitrary side length not exceeding 30mm, and oven drying the bamboo blocks at 150deg.C for more than 24 hr.
Carbonizing: carbonizing the dried bamboo blocks at 550-600 ℃ for 3-5 h, controlling the heating rate to be 4-6 ℃/min, crushing the bamboo blocks into irregular blocks with the particle size smaller than 3 meshes in a crusher, and grinding the irregular blocks into carbon powder with the particle size larger than 90% and passing through a 230-mesh test sieve in a pulverizer.
Kneading: putting the carbon powder and the adhesive into a kneader, wherein the adhesive is tar and water, the mass ratio of the carbon powder to the tar to the water is 100 (45-50) (35-40), kneading for 5-10 min, and extruding into a cylindrical green body with the diameter of 4.5-5 mm and the length of 6-8 mm.
Activating: the mass ratio of the carbonized material to distilled water is (3-4) 1, the heating rate is controlled to be 8-10 ℃/min, and the activated carbon is obtained after the activated carbon is activated for 2-5 hours at 800-900 ℃.
(2) Soaking active carbon in a first acidic solution, and washing to neutrality after the soaking is completed to obtain a first precursor, wherein the method comprises the following steps of:
the first acidic solution contains organic strong acid; the organic strong acid is sulfonic acid or perhalogenated carboxylic acid; the sulfonic acid is any one of methanesulfonic acid, benzenesulfonic acid and dodecylbenzenesulfonic acid; the perhalogenated carboxylic acid is any one of trichloroacetic acid, perfluorobutyric acid and perfluorooctanoic acid; the mass fraction of the first acidic solution is 2-4%, and the soaking time is 10-30 minutes.
(3) Soaking the first precursor in a second acidic solution, and washing to neutrality after the soaking is finished to obtain a second precursor, wherein the method comprises the following steps of:
a strong inorganic acid in the second acidic solution; the inorganic strong acid is any one of hydrochloric acid, sulfuric acid and nitric acid; the mass fraction of the second acid solution is 3-5%, and the soaking time is 20-40 minutes.
(4) Soaking the second precursor in an alkaline solution, and drying after the soaking is finished to obtain a third precursor, wherein the method comprises the following steps of:
the alkaline solution contains organic alkali, wherein the organic alkali is any one of propylene diamine, ethylenediamine, tetramethyl ethylenediamine, triethylene diamine, pyridine diamine, 4-dimethylaminopyridine, N-methylmorpholine, tetramethyl guanidine, hexatomic bicyclic guanidine, triaza bicyclo and diazabicyclo; the mass fraction of the alkaline solution is 4-6%, and the soaking time is 1-2 h; after the impregnation is finished, distilled water is adopted for washing for 2 to 4 times, and then standing is carried out for 2 to 10 hours, and then drying is carried out.
In order to improve the pore-forming effect, the alkaline solution is put into an oscillator to be oscillated and soaked at the speed of 180-200 r/min, so that the alkaline solution is fully soaked in the pores inside and on the surface of the activated carbon.
(5) And carrying out heat treatment on the third precursor, wherein the heat treatment is anaerobic heat treatment for 1.5-2 hours at 400-500 ℃ to obtain the active carbon with high benzene series adsorption rate.
The specific implementation mode of the activated carbon is prepared by the preparation method of the activated carbon with high benzene series adsorption rate; the micropore volume of the activated carbon is 0.5-0.6 mL/g, the mesoporous volume is 0.09-0.11mL/g, the average pore diameter is 0.9-1 nm, and the specific surface area is 1300-1400 m 2 The iodine adsorption value per gram is 1100-1200 mg/g, and the adsorption rate of benzene series is more than or equal to 50%.
The advantageous effects of the present invention are described below by way of specific examples.
Example 1: the preparation method of the high benzene series adsorption rate activated carbon comprises the following steps:
(1) Obtaining active carbon prepared by carbonization and activation;
and (3) bamboo wood treatment: processing fresh bamboo or waste bamboo into bamboo blocks with arbitrary side length not exceeding 30mm, and oven drying the bamboo blocks at 150deg.C for more than 24 hr.
Carbonizing: carbonizing the dried bamboo blocks for 4 hours at 550 ℃, controlling the heating rate to be 4 ℃/min, crushing the bamboo blocks into irregular blocks with the particle size smaller than 3 meshes in a crusher, and grinding the irregular blocks into carbon powder with the particle size larger than 90% and passing through a 230-mesh test sieve in a pulverizer.
Kneading: putting the carbon powder and the adhesive into a kneader, wherein the adhesive is tar and water, the mass ratio of the carbon powder to the tar to the water is 100:48:38, kneading for 5-10 min, and extruding into a cylindrical green body with the diameter of 5mm and the length of 7 mm.
Activating: and (3) using steam as an activating agent, controlling the mass ratio of the carbonized material to distilled water to be 4:1, controlling the heating rate to be 8 ℃/min, and activating for 4 hours at 900 ℃ to obtain the activated carbon.
(2) And (3) soaking the activated carbon in a benzenesulfonic acid solution, wherein the mass fraction of the benzenesulfonic acid solution is 3%, the soaking time is 20 minutes, and washing to neutrality after the soaking is completed to obtain a first precursor.
(3) And soaking the first precursor in a hydrochloric acid solution, wherein the mass fraction of the hydrochloric acid solution is 4%, the soaking time is 30 minutes, and washing to neutrality after the soaking is completed to obtain a second precursor.
(4) Soaking the second precursor in an ethylenediamine solution, wherein the mass fraction of the ethylenediamine solution is 5%, and the soaking time is 1.5h; after the impregnation is completed, washing the mixture for 3 times by using distilled water, standing the mixture for 5 hours, and drying the mixture to obtain a third precursor.
(5) And carrying out heat treatment on the third precursor, wherein the heat treatment is to carry out anaerobic heat treatment for 2 hours at 450 ℃ to obtain the active carbon with high benzene series adsorption rate.
Example 2: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: the organic strong acid is dodecylbenzene sulfonic acid; the organic base is pyridine diamine.
Example 3: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: the organic strong acid is trichloroacetic acid; the organic base is tetramethyl guanidine.
Example 4: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: the organic strong acid is perfluorobutyric acid; the organic base is a triazabicyclo.
Comparative example 1: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: (2) The mass fraction of the benzenesulfonic acid solution is 4%, and the soaking time is 40 minutes.
Comparative example 2: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: (2) The mass fraction of the benzenesulfonic acid solution is 2%, and the soaking time is 6 minutes.
Comparative example 3: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: the activated carbon is directly soaked in the second acidic solution without the first acidic solution.
Comparative example 4: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: (4) The mass fraction of the ethylenediamine solution is 6%, and the soaking time is 2.5 hours.
Comparative example 5: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: and (3) exchanging the sequence of the step (2) and the step (3), namely firstly soaking the activated carbon in a hydrochloric acid solution to obtain a first precursor, and then soaking the first precursor in a benzenesulfonic acid solution to obtain a second precursor.
Comparative example 6: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: (4) The mass fraction of the ethylenediamine solution is 4%, and the soaking time is 0.5h.
Comparative example 7: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: the second precursor is directly subjected to heat treatment without soaking in an alkaline solution.
Comparative example 8: the method for producing the activated carbon with a high benzene series adsorption rate of the present example is different from that of example 1 in that: the alkaline solution is sodium hydroxide solution with the mass fraction of 5% and the soaking time of 1.5h.
The results of performance tests of the high benzene series adsorption rate activated carbon of the above examples and comparative examples are shown in table 1, wherein the blank activated carbon is the activated carbon prepared only by the step (1). In table 1: v (V) 1 Represents the mesoporous volume, V 2 The total volume of the micropores is shown, and the benzene series is a mixture of benzene steam, toluene steam, xylene steam and ethylbenzene steam in a volume ratio of 1:1:1:1.
TABLE 1
In comparative example 1, since more acidic groups are attached to the surface of the activated carbon due to a longer soaking time, the subsequent ethylenediamine may be affected, and thus, various performance indexes in comparative example 1 are considerably deteriorated. In comparative example 2, the time of soaking in the benzenesulfonic acid solution is short, so that the impurities on the surface of the activated carbon are not thorough, and the number of mesopores is reduced, which is unfavorable for the diffusion and adsorption of toluene. In comparative example 3, since only hydrochloric acid treatment was used, each performance index was further deteriorated. As is clear from comparison of comparative example 5 with example 1, the preferred acid treatment procedure is to first conduct benzenesulfonic acid soaking and then conduct hydrochloric acid soaking.
The soaking time of ethylenediamine in comparative example 4 was too long compared with example 1, resulting in a decrease in the partial mesoporous plug volume, and eventually a slight decrease in the toluene adsorption amount. The immersion time of ethylenediamine in comparative example 6 was too short, which resulted in not only unsatisfactory pore structure but also a decrease in the amount of basic groups on the activated carbon, and thus, the amount of toluene adsorption was further decreased. In comparative example 7, since ethylenediamine was not used for soaking, the improvement degree of the pore structure was small. In comparative example 8, the inorganic strong base was used, so that not only the pore size distribution was unreasonable, but also the basic groups on the activated carbon were small, and thus the toluene adsorption effect was poor.
FIG. 1 is a low-magnification SEM photograph of a high benzene series adsorption rate active carbon of example 1 of the present invention. FIG. 2 is a high-magnification SEM photograph of the high benzene series adsorption rate active carbon of example 1 of the present invention. FIG. 3 is a high benzene series of example 1 of the present inventionAdsorption rate of N of activated carbon and blank activated carbon 2 Adsorption and desorption curves are compared with the graph. FIG. 4 is a graph showing the comparison of pore size distribution of the high benzene series adsorption rate activated carbon and the blank activated carbon according to example 1 of the present invention.
As shown in fig. 1-2, regular round holes and a plurality of pores are distributed on the surface of the activated carbon, and the round holes are communicated with the pores, so that the diffusion resistance of toluene in the activated carbon is remarkably reduced.
As shown in FIGS. 3 to 4, N of the activated carbon was obtained by the preparation method described in example 1 2 The hysteresis loop in the adsorption and desorption curves is changed compared with that of blank activated carbon, which shows that the material of the embodiment 1 has a certain number of mesopores, and the pore distribution of the activated carbon larger than 2nm is improved, so that the diffusion resistance of toluene in the activated carbon is obviously reduced.
As is clear from the above, the preparation method of the high benzene series adsorption rate active carbon has simple process and low production cost, the micropore volume of the obtained active carbon is 0.5-0.6 mL/g, the mesoporous volume is 0.09-0.11mL/g, the average pore diameter is 0.9-1 nm, and the specific surface area is 1300-1400 m 2 The iodine adsorption value per gram is 1100-1200 mg/g, and the adsorption rate of the benzene series is more than or equal to 50%, which shows that the invention can improve the pore size distribution of the traditional bamboo activated carbon, and increase the mesoporous volume and the micropore volume at the same time, so that the adsorption rate of the benzene series is obviously improved.
Among the above performance parameters and structural parameters:
the benzene series adsorption rate test adopts: referring to a testing instrument and a flow prescribed in Chinese national standard GB/T12496.5-1999 (determination of carbon tetrachloride adsorption rate (activity) of a wood activated carbon test method), a carbon tetrachloride steam generating bottle is changed into 4 organic gas steam generating bottles which are connected in parallel, the benzene steam generating bottle, the toluene steam generating bottle, the xylene steam generating bottle and the ethylbenzene steam generating bottle are respectively, the flow prescribed in the standard is equally divided into 4 parts, each part respectively passes through 1 organic steam generating bottle, and pipelines after the 4 organic steam generating bottles are subjected to gas mixing in a summarizing way, and other parts and steps are kept consistent with the standard.
The iodine adsorption value test adopts: GB/T12496.8-1999 (determination of iodine adsorption value by woody activated carbon test method).
Specific surface area, average pore size, mesoporous volume and microporous volume were obtained using BET test using Bei Shide BSD-PM.
The above description has been made of the contents of the embodiments of the invention provided in the present specification. Those skilled in the art will be able to implement the embodiments of the invention provided herein based on these descriptions. Based on the foregoing of the inventive embodiments provided herein, all other preferred embodiments and examples, which a person of ordinary skill in the art would obtain without making any inventive effort, shall fall within the scope of the inventive embodiments provided herein.
Claims (10)
1. The preparation method of the active carbon with high benzene series adsorption rate is characterized by comprising the following steps: the method comprises the following steps:
obtaining active carbon prepared by carbonization and activation;
soaking active carbon in a first acidic solution, and washing to neutrality after the soaking is completed to obtain a first precursor;
soaking the first precursor in a second acidic solution, and washing to neutrality after the soaking is finished to obtain a second precursor;
soaking the second precursor in an alkaline solution, and drying after the soaking is finished to obtain a third precursor;
performing heat treatment on the third precursor to obtain the active carbon with high benzene series adsorption rate;
wherein the first acidic solution contains organic strong acid; the second acidic solution contains a strong inorganic acid.
2. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 1, which is characterized in that: the organic strong acid is sulfonic acid or perhalogenated carboxylic acid; the sulfonic acid is any one of methanesulfonic acid, benzenesulfonic acid and dodecylbenzenesulfonic acid; the perhalogenated carboxylic acid is any one of trichloroacetic acid, perfluorobutyric acid and perfluorooctanoic acid; the inorganic strong acid is any one of hydrochloric acid, sulfuric acid and nitric acid.
3. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 2, which is characterized in that: the mass fraction of the first acidic solution is 2-4%, and the soaking time is 10-30 minutes.
4. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 2, which is characterized in that: the mass fraction of the second acid solution is 3-5%, and the soaking time is 20-40 minutes.
5. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 1, which is characterized in that: the alkaline solution contains organic alkali, wherein the organic alkali is any one of propylene diamine, ethylenediamine, tetramethyl ethylenediamine, triethylene diamine, pyridine diamine, 4-dimethylaminopyridine, N-methylmorpholine, tetramethyl guanidine, hexatomic bicyclic guanidine, triaza bicyclo and diazabicyclo.
6. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 5, which is characterized in that: the mass fraction of the alkaline solution is 4-6%, and the soaking time is 1-2 h; after the impregnation is finished, distilled water is adopted for washing for 2 to 4 times, and then standing is carried out for 2 to 10 hours, and then drying is carried out.
7. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 1, which is characterized in that: the step of obtaining the activated carbon prepared by carbonization and activation comprises the following steps:
carbonizing biomass raw materials to obtain carbon powder;
kneading carbon powder and an adhesive, and extruding and molding to obtain a blank;
and (3) performing activation treatment on the green body to obtain the activated carbon.
8. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 7, which is characterized in that: the biomass raw material is bamboo; the carbonization treatment is carbonization for 3-5 hours at 550-600 ℃; the activation treatment is to activate for 2-5 hours at 800-900 ℃, and the activating agent is water vapor.
9. The method for preparing the activated carbon with high benzene series adsorption rate according to claim 1, which is characterized in that: the heat treatment is an anaerobic heat treatment for 1.5 to 2 hours at the temperature of 400 to 500 ℃.
10. Activated carbon, its characterized in that: is prepared by the preparation method of the high benzene series adsorption rate active carbon according to any one of claims 1 to 9; the micropore volume of the activated carbon is 0.5-0.6 mL/g, the mesoporous volume is 0.09-0.11mL/g, the average pore diameter is 0.9-1 nm, and the specific surface area is 1300-1400 m 2 The iodine adsorption value per gram is 1100-1200 mg/g, and the adsorption rate of benzene series is more than or equal to 50%.
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