CN117019128A - Activated carbon-based catalyst and preparation method and application thereof - Google Patents
Activated carbon-based catalyst and preparation method and application thereof Download PDFInfo
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- CN117019128A CN117019128A CN202311294006.XA CN202311294006A CN117019128A CN 117019128 A CN117019128 A CN 117019128A CN 202311294006 A CN202311294006 A CN 202311294006A CN 117019128 A CN117019128 A CN 117019128A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000003054 catalyst Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 96
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 96
- 241001330002 Bambuseae Species 0.000 claims abstract description 96
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 96
- 239000011425 bamboo Substances 0.000 claims abstract description 96
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 84
- 238000001035 drying Methods 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 32
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 28
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 25
- 238000010000 carbonizing Methods 0.000 claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000006477 desulfuration reaction Methods 0.000 claims description 41
- 230000023556 desulfurization Effects 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 8
- 238000003763 carbonization Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 abstract 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 17
- 229910052717 sulfur Inorganic materials 0.000 description 17
- 239000011593 sulfur Substances 0.000 description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 238000001179 sorption measurement Methods 0.000 description 9
- 239000005539 carbonized material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 229910052725 zinc Inorganic materials 0.000 description 6
- 229960000892 attapulgite Drugs 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 125000001741 organic sulfur group Chemical group 0.000 description 4
- 229910052625 palygorskite Inorganic materials 0.000 description 4
- 230000000149 penetrating effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000001994 activation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000003009 desulfurizing effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 150000004763 sulfides Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 244000018633 Prunus armeniaca Species 0.000 description 1
- 235000009827 Prunus armeniaca Nutrition 0.000 description 1
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical class O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- 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
- B01D53/04—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 with stationary adsorbents
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- B01D—SEPARATION
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/485—Sulfur compounds containing only one sulfur compound other than sulfur oxides or hydrogen sulfide
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
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- B01D53/508—Sulfur oxides by treating the gases with solids
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8603—Removing sulfur compounds
- B01D53/8606—Removing sulfur compounds only one sulfur compound other than sulfur oxides or hydrogen sulfide
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/8609—Sulfur oxides
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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- B01J37/0201—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2257/306—Organic sulfur compounds, e.g. mercaptans
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/308—Carbonoxysulfide COS
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Abstract
The invention discloses an active carbon-based catalyst, a preparation method and application thereof; the preparation method comprises the following steps: s1, preparing bamboo powder; s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 to obtain bamboo-based carbide; s3, mixing the bamboo-based carbide obtained in the step S2 with rectorite according to a mass ratio of 1: 0.4-0.7 of the solid separation agent is added into sodium hydroxide solution, and the solid separation agent is obtained after stirring; then the solid separated matter is dried firstly and then treated for 0.5 to 4 hours at the temperature of 780 to 795 ℃; washing, drying, grinding and sieving to obtain a carrier; s4, adding the carrier obtained in the step S3 into ferric nitrate solution, oscillating and impregnating, and then drying and roasting to obtain a material a; s5, adding the material a obtained in the step S4 into zinc nitrate solution, oscillating for impregnation, and then drying and roasting.
Description
Technical Field
The invention belongs to the technical field of desulfurization catalysts, and particularly relates to an active carbon-based catalyst, a preparation method and application thereof.
Background
The combustion of coal fuel and the emission of a large amount of sulfur-containing pollutants in the industrial production process; wherein about 90% of sulfur dioxide compounds in China are all from flue gas generated by coal combustion. The sulfur-containing compounds can form acid rain through complex physical and chemical actions after being discharged into the atmosphere, thereby threatening the health of people. Currently, the desulfurization methods industrially practiced include wet desulfurization (i.e., liquid absorption), dry desulfurization (i.e., powder absorbent or catalyst, etc.), and semi-dry desulfurization; desulfurization, in accordance with the object of desulfurization, includes removal of organic sulfur and removal of inorganic sulfur. In the prior art, the dry desulfurization is widely applied; wherein, the dry desulfurization comprises chemical reaction desulfurization and physical adsorption desulfurization. The chemical reaction method is to remove sulfide through chemical reaction, and the desulfurization has the characteristics of high desulfurization precision, large sulfur capacity and the like; the physical adsorption desulfurization is mainly carried out by adsorbing sulfides by the polarity of the adsorbent, and the polarity adsorption desulfurization has certain requirements on the polarity of the sulfides, so that the sulfides with low polarity can not be adsorbed and removed.
Activated carbon is a material widely used in the desulfurization field. According to different raw materials, the activated carbon can be divided into coal activated carbon, wood activated carbon, synthetic material activated carbon and other activated carbon types; wherein, the preparation sources of the wood activated carbon comprise coconut shells, apricot shells, fruit shells, bamboo and the like; in the prior art, as in patent document CN106732751B, a desulfurization and denitrification agent for carrying iron and vanadium by a carrier composed of attapulgite clay, a molecular sieve and active carbon is provided, wherein the active carbon used in the desulfurization and denitrification agent is rice husk, and the carrier has various types. The bamboo forest resources in China are rich, the growth of the bamboo has the characteristics of short period, high yield and the like, and the reasonable utilization of the rich bamboo resources is greatly helpful for the environmental protection, energy conservation and emission reduction in China. In the prior art, some reports of desulfurization by utilizing bamboo exist, for example, patent document CN103693643B reports that a bamboo-based activated carbon applied to flue gas desulfurization has an activation temperature of 900-1000 ℃ in the preparation process and a high temperature, and the achieved desulfurization is mainly physical adsorption, so that the desulfurization effect needs to be further improved; patent document CN106824068A reports a high-selectivity adsorption desulfurizing agent for bamboo-source porous biomass charcoal-based fuel oil, and similarly, desulfurization achieved by the desulfurizing agent is mainly physical adsorption.
The preparation of efficient desulfurization catalysts around the utilization of bamboo is still worth studying. Based on the above considerations, the present invention has been made.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide an active carbon-based catalyst, a preparation method and application thereof, wherein bamboo and rectorite are taken as main raw materials of a carrier, active components are relatively common, the raw materials are common, the cost is controllable, and the desulfurization effect is good.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: crushing bamboo raw materials, and then drying to obtain bamboo powder for later use;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 to obtain bamboo-based carbide;
s3, mixing the bamboo-based carbide obtained in the step S2 with rectorite according to a mass ratio of 1: 0.4-0.7 of the solid separation agent is added into sodium hydroxide solution, and the solid separation agent is obtained after stirring; drying the obtained solid separation material, and then treating the solid separation material at 780-795 ℃ for 0.5-4 hours; washing, drying, grinding and sieving to obtain a carrier;
s4, adding the carrier obtained in the step S3 into ferric nitrate solution, oscillating and impregnating, and then drying and roasting to obtain a material a;
s5, adding the material a obtained in the step S4 into zinc nitrate solution, oscillating and impregnating, and then drying and roasting to obtain the active carbon-based catalyst.
Further, in the step S1, the powder is crushed to 120-200 meshes, the drying temperature is 105-115 ℃, and the drying time is 12-36 hours.
Further, in the step S2, the carbonization treatment temperature is 495-525 ℃ and the carbonization treatment time is 0.5-2 h.
Further, in the step S3, the concentration of the sodium hydroxide solution is 25-40wt%; the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g: 10-20 mL; the number of the ground screening meshes is 200-300 meshes.
Further, in the step S4, the concentration of the ferric nitrate solution is 0.8-1.2 mol/L, and the mass ratio of the carrier to the ferric nitrate solution is 1: 5-9.
In step S4, the calcination treatment temperature is 520-550 ℃ and the treatment time is 0.5-4 h.
Further, in the step S5, the concentration of the zinc nitrate solution is 0.4-0.8 mol/L; the mass ratio of the material a to the zinc nitrate solution is 1: 4-7.
In step S5, the calcination treatment temperature is 520-550 ℃ and the treatment time is 0.5-4 h.
In addition, the invention also aims to protect the activated carbon-based catalyst prepared by the method.
And, it is also desirable to protect the use of the activated carbon-based catalyst prepared as described above in desulfurization.
Compared with the prior art, the invention has the following beneficial effects:
the active carbon-based catalyst takes the bamboo-based active carbon and the rectorite as the composite carrier, and the active components of iron and zinc are impregnated and loaded step by step, so that the good simultaneous removal of organic sulfur and inorganic sulfur can be realized, the raw materials are common, the cost is controllable, the preparation method is simple, and the operation is easy.
In the preparation process of the catalyst, the bamboo-based activated carbon and a small amount of rectorite are treated by sodium hydroxide solution at the same time and then calcined at high temperature, so that the reason is that: on the one hand, from the high temperature treatment, the bamboo-based activated carbon can remove impurities and dredge pore channels under the high temperature treatment of sodium hydroxide, and enrich the pore channel structures; the rectorite can strengthen ion exchange under the high-temperature treatment of sodium hydroxide, so that the structure of the rectorite is amorphized, the pore canal distribution is enriched, the high-temperature sodium hydroxide treatment is beneficial to the enrichment of the pore canal structures of the rectorite and the porous canal distribution, and the subsequent loading of active components is beneficial; on the other hand, from the selection of carrier types, the rectorite has better acid and alkali resistance, rich lamellar structure and surface functional groups, can play a role in modifying bamboo-based activated carbon, and the two are matched for use to enhance the adaptability of the catalyst to sulfur-containing environment and synergistically improve the desulfurization effect; compared with other biomass activated carbon, the bamboo-based activated carbon has better specific surface area and pore volume, has excellent sulfide physical adsorption performance, and simultaneously, the characteristic is favorable for the adsorption of subsequent active components of zinc and iron, so that the desulfurization effect is further improved; the applicant repeatedly screens to determine that the effect of the composite use of the rectorite Dan Hezhu-based activated carbon is optimal (compared with the activated carbon and the attapulgite) because the rectorite Dan Hezhu-based activated carbon has the difference of pore size distribution, and meanwhile, the surface of the bamboo-based activated carbon treated by sodium hydroxide has rich oxygen-containing functional groups such as carboxyl, phenolic hydroxyl and the like, so that the cation ionization exchange of the rectorite can be further promoted, and the adsorptivity of the rectorite can be improved; the functional groups such as hydroxyl groups of the rectorite can have hydrogen bond action with the oxygen-containing functional groups such as carboxyl groups and phenolic hydroxyl groups of the bamboo-based activated carbon, so that the stability, strength, adsorptivity and other performances of the composite carrier are improved, the adsorption of zinc and iron active components is further improved, and the better desulfurization effect and recycling performance are ensured.
In the invention, the active components are simple combinations of iron and zinc, and a better desulfurization effect can be realized without additional auxiliary active components; the iron can realize the removal of organic sulfur (such as carbonyl sulfur) and inorganic sulfur in the environment containing hydrogen or water vapor, and the zinc can directly remove the inorganic sulfur; the two are matched together, so that the simultaneous removal of organic sulfur and inorganic sulfur can be realized, the desulfurization precision and the sulfur capacity are high, and the recycling performance is good.
In the invention, the rectorite is directly added for treatment in the activation process of the bamboo, so that the step-by-step treatment of the rectorite is avoided. In addition, the carbonization temperature, the activation temperature, the concentration of sodium hydroxide and other process conditions in the invention are obtained through repeated researches, so that the desulfurization performance of the obtained active carbon-based catalyst is ensured.
In a word, the invention solves the problems of poor dispersion and insufficient loading of zinc oxide and ferric oxide by optimizing the types of carriers, and the prepared catalyst has good desulfurization performance at low temperature (200 ℃), can fully utilize bamboo resources, and has a certain application prospect.
Detailed Description
The following detailed description of embodiments of the invention, all of which are exemplary and intended to be illustrative of the invention and not to be construed as limiting the invention.
In each embodiment of the invention, the bamboo raw material is from the Jiangsu Li-yang area, and the growth period is about 4 years; rectorite was purchased from the company rectorite limited, ming's current, hubei.
The other parts not described, such as washing, drying and other treatment process means, are conventional technical means for those skilled in the art; the rest chemical raw materials are all purchased in the market.
Example 1
A method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: pulverizing bamboo material to 150 mesh, and drying at 110deg.C for 24 hr to obtain bamboo powder;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 at 505 ℃ for 45min to obtain bamboo-based carbonized materials;
s3, mixing the bamboo-based carbide obtained in the step S2 with rectorite according to a mass ratio of 1:0.5 is added into 38wt% sodium hydroxide solution (the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g:15 mL), and the mixture is stirred and separated to obtain a solid separation product; subsequently, the solid isolate obtained is dried first (95 ℃) and treated for a further 2 hours at 785 ℃; after the treatment is finished, washing, drying, grinding and sieving by 200 meshes to obtain a carrier;
s4, according to the mass ratio of 1:7, adding the carrier obtained in the step 3 into 1mol/L ferric nitrate solution, oscillating and impregnating, and then drying and roasting (520 ℃ C. For 1.5 h) to obtain a material a;
s5, according to the mass ratio of 1: and 5, adding the material a obtained in the step S4 into a 0.6mol/L zinc nitrate solution, oscillating and impregnating, and then drying and roasting (525 ℃ C., 1.5 h) to obtain the active carbon-based catalyst.
Example 2
A method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: pulverizing bamboo material to 150 mesh, and drying at 105deg.C for 32 hr to obtain bamboo powder;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 at 500 ℃ for 60min to obtain bamboo-based carbonized materials;
s3, mixing the bamboo-based carbide obtained in the step S2 with rectorite according to a mass ratio of 1:0.45 is added into 36wt% sodium hydroxide solution (the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g to 16 mL), and the mixture is stirred and separated to obtain a solid separation product; subsequently, the solid isolate obtained is dried first (95 ℃) and treated at 790℃for a further 1.5h; after the treatment is finished, washing, drying, grinding and sieving by 200 meshes to obtain a carrier;
s4, according to the mass ratio of 1:7.5, adding the carrier obtained in the step S3 into 1mol/L ferric nitrate solution, oscillating and impregnating, and then drying and roasting (525 ℃ for 2 hours) to obtain a material a;
s5, according to the mass ratio of 1:4.5, adding the material a obtained in the step S4 into 0.6mol/L zinc nitrate solution, oscillating and impregnating, and then drying and roasting (520 ℃ C. For 1.5 h) to obtain the active carbon-based catalyst.
Example 3
A method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: pulverizing bamboo material to 150 mesh, and drying at 105deg.C for 36 hr to obtain bamboo powder;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 at 510 ℃ for 30min to obtain bamboo-based carbonized materials;
s3, mixing the bamboo-based carbide obtained in the step S2 with rectorite according to a mass ratio of 1:0.55 is added into 37wt% sodium hydroxide solution (the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g:15 mL), and the mixture is stirred and separated to obtain a solid separation product; subsequently, the solid isolate obtained is dried first (95 ℃) and treated at 795℃for a further 1.5h; after the treatment is finished, washing, drying, grinding and sieving by 200 meshes to obtain a carrier;
s4, according to the mass ratio of 1:6.5, adding the carrier obtained in the step S3 into 1mol/L ferric nitrate solution, oscillating and impregnating, and then drying and roasting (525 ℃ for 2 hours) to obtain a material a;
s5, according to the mass ratio of 1:5.5, adding the material a obtained in the step S4 into 0.6mol/L zinc nitrate solution, oscillating and impregnating, and then drying and roasting (520 ℃ C. For 1.5 h) to obtain the active carbon-based catalyst.
Comparative example 1
A method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: pulverizing bamboo material to 150 mesh, and drying at 110deg.C for 24 hr to obtain bamboo powder;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 at 505 ℃ for 45min to obtain bamboo-based carbonized materials;
s3, adding the bamboo-based carbide obtained in the step S2 into a 38wt% sodium hydroxide solution (the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g:15 mL), and separating after stirring to obtain a solid separation product; subsequently, the solid isolate obtained is dried first (95 ℃) and treated for a further 2 hours at 785 ℃; after the treatment is finished, washing, drying, grinding and sieving by 200 meshes to obtain a carrier;
s4, according to the mass ratio of 1:7, adding the carrier obtained in the step 3 into 1mol/L ferric nitrate solution, oscillating and impregnating, and then drying and roasting (520 ℃ C. For 1.5 h) to obtain a material a;
s5, according to the mass ratio of 1: and 5, adding the material a obtained in the step S4 into a 0.6mol/L zinc nitrate solution, oscillating and impregnating, and then drying and roasting (525 ℃ C., 1.5 h) to obtain the active carbon-based catalyst.
This comparative example 1 differs from example 1 in that rectorite was not used.
Comparative example 2
A method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: pulverizing bamboo material to 150 mesh, and drying at 110deg.C for 24 hr to obtain bamboo powder;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 at 505 ℃ for 45min to obtain bamboo-based carbonized materials;
s3, the bamboo-based carbide obtained in the step S2 and attapulgite are mixed according to the mass ratio of 1:0.5 is added into 38wt% sodium hydroxide solution (the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g:15 mL), and the mixture is stirred and separated to obtain a solid separation product; subsequently, the solid isolate obtained is dried first (95 ℃) and treated for a further 2 hours at 785 ℃; after the treatment is finished, washing, drying, grinding and sieving by 200 meshes to obtain a carrier;
s4, according to the mass ratio of 1:7, adding the carrier obtained in the step 3 into 1mol/L ferric nitrate solution, oscillating and impregnating, and then drying and roasting (520 ℃ C. For 1.5 h) to obtain a material a;
s5, according to the mass ratio of 1: and 5, adding the material a obtained in the step S4 into a 0.6mol/L zinc nitrate solution, oscillating and impregnating, and then drying and roasting (525 ℃ C., 1.5 h) to obtain the active carbon-based catalyst.
This comparative example 2 differs from example 1 in that the rectorite was replaced with attapulgite.
Comparative example 3
A method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: pulverizing bamboo material to 150 mesh, and drying at 110deg.C for 24 hr to obtain bamboo powder;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 at 505 ℃ for 45min to obtain bamboo-based carbonized materials;
s3, adding the bamboo-based carbide obtained in the step S2 into a 38wt% sodium hydroxide solution (the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g:15 mL), and separating after stirring to obtain a solid separation product; then the obtained solid separation is firstly dried (95 ℃) and then is uniformly mixed with the dried rectorite (the mass ratio of the bamboo-based carbide to the rectorite is 1:0.5) and then is treated for 2 hours at 785 ℃; after the treatment is finished, washing, drying, grinding and sieving by 200 meshes to obtain a carrier;
s4, according to the mass ratio of 1:7, adding the carrier obtained in the step 3 into 1mol/L ferric nitrate solution, oscillating and impregnating, and then drying and roasting (520 ℃ C. For 1.5 h) to obtain a material a;
s5, according to the mass ratio of 1: and 5, adding the material a obtained in the step S4 into a 0.6mol/L zinc nitrate solution, oscillating and impregnating, and then drying and roasting (525 ℃ C., 1.5 h) to obtain the active carbon-based catalyst.
This comparative example 3 differs from example 1 in that the rectorite is not impregnated with sodium hydroxide solution.
Comparative example 4
A method for preparing an activated carbon-based catalyst, comprising the steps of:
s1, preparing bamboo powder: pulverizing bamboo material to 150 mesh, and drying at 110deg.C for 24 hr to obtain bamboo powder;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 at 505 ℃ for 45min to obtain bamboo-based carbonized materials;
s3, mixing the bamboo-based carbide obtained in the step S2 with rectorite according to a mass ratio of 1:0.5 is added into 38wt% sodium hydroxide solution (the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g:15 mL), and the mixture is stirred and separated to obtain a solid separation product; subsequently, the solid isolate obtained is dried first (95 ℃) and treated for a further 2 hours at 785 ℃; after the treatment is finished, washing, drying, grinding and sieving by 200 meshes to obtain a carrier;
s4, according to the mass ratio of 1: and 7, adding the carrier obtained in the step 3 into a 1mol/L ferric nitrate solution, oscillating and impregnating, and then drying and roasting (520 ℃ C. For 1.5 h) to obtain the active carbon-based catalyst.
This comparative example 4 differs from example 1 in that zinc was not loaded.
The desulfurization performance test is carried out on the activated carbon-based catalysts prepared in the example 1 and the comparative examples 1-4, and the specific method is as follows: in the fixed bed, 3.5g of each of the activated carbon-based catalysts obtained in example 1 and comparative examples 1 to 4 was charged, and the temperature was raised to 200℃under normal pressure, according to 2800 h -1 The mixture (1500 ppm of hydrogen sulfide, 220ppm of carbonyl sulfide, 25% of hydrogen, 8% of water vapor and the balance of nitrogen) was introduced into the reactor for desulfurization. Activated carbon based for penetrative deactivationWashing and regenerating the catalyst, then carrying out ultrasonic oscillation in deionized water for 15min, and drying for later use; after recycling for 20 times, the desulfurization performance was tested again. The test results are shown in tables 1 and 2. The desulfurization precision refers to the sulfur content of the desulfurization tail gas before the sulfur content penetrates in the desulfurization process; the penetrating sulfur capacity refers to the capacity of sulfur absorbed by a unit volume of desulfurizing agent when ensuring the process purification index; the sulfur content of the desulfurized mixed gas is detected according to GB/T28727-2012.
As can be seen from tables 1 and 2, the active carbon-based catalyst obtained in the examples of the present invention has higher desulfurization precision, higher penetrating sulfur capacity and higher penetrating sulfur capacity retention rate after 20 cycles compared with comparative examples 1 to 4.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for preparing an activated carbon-based catalyst, which is characterized by comprising the following steps:
s1, preparing bamboo powder: crushing bamboo raw materials, and then drying to obtain bamboo powder for later use;
s2, carbonizing bamboo powder: carbonizing the bamboo powder obtained in the step S1 to obtain bamboo-based carbide;
s3, mixing the bamboo-based carbide obtained in the step S2 with rectorite according to a mass ratio of 1: 0.4-0.7 of the solid separation agent is added into sodium hydroxide solution, and the solid separation agent is obtained after stirring; drying the obtained solid separation material, and then treating the solid separation material at 780-795 ℃ for 0.5-4 hours; washing, drying, grinding and sieving to obtain a carrier;
s4, adding the carrier obtained in the step S3 into ferric nitrate solution, oscillating and impregnating, and then drying and roasting to obtain a material a;
s5, adding the material a obtained in the step S4 into zinc nitrate solution, oscillating and impregnating, and then drying and roasting to obtain the active carbon-based catalyst.
2. The method for preparing an activated carbon-based catalyst according to claim 1, wherein in the step S1, the activated carbon-based catalyst is crushed to 120-200 meshes, the drying temperature is 105-115 ℃, and the drying time is 12-36 hours.
3. The method for preparing an activated carbon-based catalyst according to claim 1, wherein in the step S2, the carbonization treatment temperature is 495-525 ℃ and the carbonization treatment time is 0.5-2 h.
4. The method for preparing an activated carbon-based catalyst according to claim 1, wherein in the step S3, the concentration of the sodium hydroxide solution is 25-40 wt%; the dosage ratio of the bamboo-based carbide to the sodium hydroxide solution is 1g: 10-20 mL; the number of the ground screening meshes is 200-300 meshes.
5. The method for preparing an activated carbon-based catalyst according to claim 1, wherein in the step S4, the concentration of the ferric nitrate solution is 0.8-1.2 mol/L, and the mass ratio of the carrier to the ferric nitrate solution is 1: 5-9.
6. The method for preparing an activated carbon-based catalyst according to claim 1, wherein in the step S4, the calcination treatment temperature is 520-550 ℃ and the treatment time is 0.5-4 hours.
7. The method for preparing an activated carbon-based catalyst according to claim 1, wherein in the step S5, the concentration of the zinc nitrate solution is 0.4-0.8 mol/L; the mass ratio of the material a to the zinc nitrate solution is 1: 4-7.
8. The method for preparing an activated carbon-based catalyst according to claim 1, wherein in the step S5, the calcination treatment temperature is 520-550 ℃ and the treatment time is 0.5-4 hours.
9. The activated carbon-based catalyst prepared by the method of any one of claims 1 to 8.
10. Use of the activated carbon-based catalyst of claim 9 for desulfurization.
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| CN104667872A (en) * | 2015-02-12 | 2015-06-03 | 江苏竹海活性炭有限公司 | High-efficiency deep desulfurization active carbon and preparation method thereof |
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| CN111135793A (en) * | 2020-01-07 | 2020-05-12 | 江苏竹海活性炭有限公司 | Renewable efficient deep desulfurization activated carbon and preparation method and application thereof |
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