CN115770571A - Copper-based catalyst-loaded sludge activated carbon and preparation method and application thereof - Google Patents
Copper-based catalyst-loaded sludge activated carbon and preparation method and application thereof Download PDFInfo
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- CN115770571A CN115770571A CN202211405937.8A CN202211405937A CN115770571A CN 115770571 A CN115770571 A CN 115770571A CN 202211405937 A CN202211405937 A CN 202211405937A CN 115770571 A CN115770571 A CN 115770571A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 292
- 239000010802 sludge Substances 0.000 title claims abstract description 165
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 54
- 239000010949 copper Substances 0.000 title claims abstract description 54
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000003054 catalyst Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000002028 Biomass Substances 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 17
- 230000023556 desulfurization Effects 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 150000001879 copper Chemical class 0.000 claims abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 229910052799 carbon Inorganic materials 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- 230000010355 oscillation Effects 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 13
- 239000003546 flue gas Substances 0.000 claims description 13
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 7
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- 238000004898 kneading Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 2
- 229940116318 copper carbonate Drugs 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims 4
- 239000002910 solid waste Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000001994 activation Methods 0.000 description 41
- 230000004913 activation Effects 0.000 description 35
- 238000003763 carbonization Methods 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 15
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 239000011148 porous material Substances 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 9
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000005554 pickling Methods 0.000 description 7
- 238000000197 pyrolysis Methods 0.000 description 7
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- 230000003197 catalytic effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
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- 229910052757 nitrogen Inorganic materials 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 231100000719 pollutant Toxicity 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
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- 229940057838 polyethylene glycol 4000 Drugs 0.000 description 4
- 239000010801 sewage sludge Substances 0.000 description 4
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- 239000002699 waste material Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
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- 125000000524 functional group Chemical group 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
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- KVGZZAHHUNAVKZ-UHFFFAOYSA-N 1,4-Dioxin Chemical compound O1C=COC=C1 KVGZZAHHUNAVKZ-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 241001070941 Castanea Species 0.000 description 1
- 235000014036 Castanea Nutrition 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 235000009414 Elaeocarpus kirtonii Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 244000236151 Tabebuia pallida Species 0.000 description 1
- 235000013584 Tabebuia pallida Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- 235000012216 bentonite Nutrition 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000010852 non-hazardous waste Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
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- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- 239000011276 wood tar Substances 0.000 description 1
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Abstract
The invention discloses sludge activated carbon loaded with a copper-based catalyst, a preparation method and application thereof, wherein the sludge activated carbon is prepared by reacting sludge activated carbon with a copper salt; wherein the sludge activated carbon is prepared from the following components in percentage by mass (50-90): (10-50): (5-25) the sludge, the biomass material and the binder, and after the raw materials are mixed, the raw materials are carbonized and activated; the mass ratio of the metal copper salt to the sludge activated carbon is (0.01-0.25): 1. the method has the advantages that the sludge is cooperated with the biomass solid wastes as the raw materials, so that the quality of the activated carbon is improved, the denitration efficiency of the material loaded with the copper-based catalyst is improved, the preparation process of the material is simple, the operation is easy, the market competitiveness is strong, the integrated process target of desulfurization and denitration is achieved, and the environmental protection target of reduction, harmlessness and resource treatment of the municipal sludge is realized.
Description
Technical Field
The invention relates to the field of activated carbon preparation, the field of solid waste recycling and the field of catalyst research, in particular to sludge activated carbon loaded with a copper-based catalyst, a preparation method and application thereof in the field of flue gas desulfurization and denitrification.
Background
The solid content of the sewage sludge of the urban sewage treatment plant is about 1 to 3 percent, and the sewage sludge contains rich nitrogen, phosphorus, potassium, organic matters and other trace nutrient elements necessary for the growth of plants, and also contains organic pollutants, heavy metals and a small amount of pathogenic microorganisms, parasitic ova and the like which are difficult to degrade. The yield of dry sludge in the United states is about 600 million tons every year, the dry sludge produced in European Union is more than 1000 million tons every year, the dry sludge discharged by municipal sewage treatment plants in China is about 440 million tons every year, the annual growth rate is more than 10 percent, and the dry sludge accounts for 3.2 percent of the total solid waste in China. The problem of safe disposal of sewage sludge has received extensive attention from students in the environmental field all over the world. If the sludge is not treated safely in the true sense, secondary pollution can be caused to the surrounding environment.
With the increasing improvement of the environmental protection requirements of China, the control variety of atmospheric pollutants is more and more, the emission standard is stricter, and the treatment requirement of various pollutants in industrial flue gas is more urgent. The sintering flue gas is a main source for the emission of atmospheric pollutants of iron and steel enterprises, and mainly comprises sulfur dioxide, nitrogen oxides, particulate matters, dioxin, heavy metals (lead, arsenic, chromium, mercury and the like), fluorides, volatile Organic Compounds (VOCs) and other various pollutants. The activated carbon flue gas treatment technology can realize the deep treatment of flue gas, thereby gradually becoming the optimal technical scheme for atmospheric treatment. The activated carbon is widely applied to SO in coal-fired flue gas as an adsorbent 2 And NOx can be removed, and the desulfurization and denitrification activity of the activated carbon can be effectively improved after the catalyst is loaded. The most studied supported catalysts are metal catalysts, including Fe 2 O 3 And ZnO, etc., the corresponding active carbon supported catalyst has Fe 2 O 3 and/AC and ZnO/AC, etc. The catalyst can promote NOx and NH in Selective Catalytic Reduction (SCR) reaction of NOx 4 Reaction to form N 2 And H 2 And O, improving the denitration rate.
CN112371085A discloses a steel pickling sludge modified sludge activated carbon for rainwater treatment, which is prepared by drying steel pickling sludge and sludge activated carbon to make the water content of the steel pickling sludge and the sludge activated carbon 30-60 wt%, grinding the dried steel pickling sludge and the sludge activated carbon to be 0.1mm, mixing the steel pickling sludge and the sludge activated carbon according to the mass ratio of 1: 4-1: 8, and roasting the mixture at 600-900 ℃ in a nitrogen atmosphere. The invention uses the steel pickling sludge and the sludge activated carbon to prepare the adsorbing material for the first time, solves the problem of recycling the pickling sludge and the sewage sludge, but the activated carbon has poor adsorption effect and less applicable fields.
CN101543763B discloses a gamma-type aluminum oxide film and vanadium pentoxide modified sludge activated carbon for flue gas desulfurization and denitration, and the raw material components of the gamma-type aluminum oxide film and the vanadium pentoxide modified sludge activated carbon are AlCl 3 ·6H 2 O、V 2 O 5 And sludge of sewage treatment plants; the preparation steps are as follows: (1) preparation of Al (OH) 3 Sol; (2) preparing sludge activated carbon; (3) preparing gamma type aluminum oxide film modified sludge activated carbon; (4) preparing a gamma-type aluminum oxide film and vanadium pentoxide modified sludge activated carbon. The gamma-type aluminum oxide film and vanadium pentoxide are firstly used for preparing the modified sludge activated carbon, so that the desulfurization and denitrification efficiency of the sludge activated carbon is effectively improved, the existing use requirements are met, but the performance of the material prepared by the method is poor, and the material can only be used for removing pollutants with lower concentration.
Disclosure of Invention
In order to solve the problems of low denitration efficiency and poor using effect of the existing activated carbon, the invention provides the sludge activated carbon loaded with the copper-based catalyst and the preparation method and application thereof. In addition, the invention also provides a preparation method and application of the sludge activated carbon loaded with the copper-based catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a copper-based catalyst-loaded sludge activated carbon, which is prepared by reacting sludge activated carbon with a metal copper salt;
wherein the sludge activated carbon is prepared from the following components in percentage by mass (50-90): (10-50): (5-25) the sludge, the biomass material and the binder, and after the raw materials are mixed, the raw materials are carbonized and activated;
the carbonization treatment is carried out in an inert gas environment, the carbonization temperature is 400-700 ℃, the carbonization time is 0.5-3 h, and the carbonization temperature rise is 10-30 ℃/min;
in the activation treatment process, the activation temperature is 600-1000 ℃, the activation time is 0.5-3 h, and the activation temperature rise is 10-30 ℃/min.
Specifically, the sludge is non-hazardous waste sludge and is one or more of municipal sludge, industrial sludge and oily sludge.
Specifically, the biomass material is one or more of corn stalk, bamboo chip, chestnut shell, rice bran, coconut shell, nut, pine tree, white wood, poplar, and cottonseed shell.
Preferably, the biomass material is coconut shell, which has a relatively high carbon content.
Because the carbon content in the sludge is low, the biomass material is added into the formula as a carburant, and the carbon content is an important index for screening the biomass material. The highest content of C in the constituent elements in the biomass material is about 38-76%, so that the biomass material can be used as an excellent synergistic raw material in the preparation process of the activated carbon.
Specifically, the binder is one or more of coal tar, wood tar, phenolic resin, carboxymethyl cellulose, water glass, sepiolite, bentonite, starch, polyvinyl alcohol and polyethylene glycol.
Specifically, in the activation treatment process, the activation mode is one or more of chemical activation, physical activation and physical-chemical activation.
Preferably, the activation treatment mode is physical activation, and the adopted activating agent is one or more of air, water vapor and CO 2. The activating agent is preferably steam, and the ratio of the steam to the mixed material to be carbonized (which also becomes the water-carbon ratio) is (0.5-3): 1.
in the application, the carbonization and activation process steps adopt a carbonization and activation integrated furnace, and through a large number of experiments, the performance indexes such as strength, desulfurization and denitrification performance and the like of the finally prepared activated carbon material are comprehensively considered, so that the optimal carbonization temperature, carbonization time, carbonization temperature rise rate, activation temperature, activation time and activation temperature rise are finally determined.
The combustible gas generated in the processes of pyrolysis carbonization and high-temperature activation can be used as a heat source in the processes of carbonization and activation and can also be used as a heat source for drying and dehydrating raw materials.
The main function of pyrolysis and carbonization is that volatile matters in the material are decomposed and escaped under the condition of oxygen-free high temperature to form a complex porous pore structure, wherein carbon atoms of partial carbonization products are combined into an irregular aromatic ring sheet structure to cause partial cracks, and the cracks can further form a more developed microporous structure in the subsequent high-temperature activation process to improve the adsorption performance.
The activation treatment process in the application selects a physical activation mode and selects water vapor as an activation medium. In the high-temperature activation process, oxidation-reduction reaction is carried out between the activated material and the carbonized material, so that the purpose of expanding old holes and opening new holes is achieved. After the carbon surface of the material adsorbs water vapor, the adsorbed water vapor releases hydrogen, and the adsorbed oxygen falls off from the carbon surface in a CO form; CO production by reaction of the CO produced with adsorbed oxygen on the carbon surface 2 (ii) a The carbon surface continues to react with water vapor. The reaction not only enlarges the complex and porous pore structure of the active carbon and improves the performance index of the pores, but also can remove pyrolysis tar and pyrolysis products which do not escape and are accumulated in the pore structure in the carbonization process, enlarge the pore structure, improve the volume and the specific surface area of the pores, increase complex surface functional groups and obtain the active carbon material with the optimal performance.
In order to improve the specific surface area of the finally prepared catalyst and the dispersion degree of the loaded active component, the mass ratio of the active component (copper salt) to the carrier (sludge activated carbon) needs to be controlled, and the mass ratio of the copper salt to the sludge activated carbon is (0.01-0.25): 1, preferably, the mass ratio of the metal copper salt to the sludge activated carbon is (0.05-0.13): 1.
specifically, before the sludge activated carbon reacts with the metal copper salt, modification treatment is carried out, heavy metals contained in raw materials can be reduced, redundant ash can be removed, dust in the surface layer and pores of the materials is reduced, and subsequent loading of active components is facilitated.
The modification treatment process comprises hydrochloric acid dipping treatment, ethanol cleaning and hot water washing.
In the hydrochloric acid dipping treatment process, the concentration of a hydrochloric acid solution is 2-7 mol/L, the dipping time is 1-4 h, and the dipping temperature is 40-150 ℃; in the ethanol cleaning treatment process, the pretreated sludge activated carbon is placed in an ethanol solution for oscillation treatment, the oscillation temperature is 20-60 ℃, and the oscillation time is 1-8 h; in the hot water washing process, the temperature of the hot water is 60-90 ℃, and the washing times are 1-5 times.
Specifically, the sludge activated carbon is dried and roasted after reacting with a metal copper salt.
The drying temperature is 90-150 ℃, the drying time is 3-20 h, preferably, the drying temperature is 100-120 ℃, and the drying time is 4-12 h; the roasting process is carried out under the protection of air atmosphere, oxygen-poor atmosphere or nitrogen atmosphere, preferably under the protection of nitrogen atmosphere, the roasting temperature is 300-600 ℃, and the roasting time is 4-8 h.
Specifically, the metal copper salt is a copper-based metal precursor salt, and is one or more of copper nitrate, copper acetate, copper carbonate and copper chloride, and preferably, copper nitrate and copper acetate are selected.
In a second aspect of the present invention, a method for preparing the above copper-based catalyst-loaded sludge activated carbon is provided, which includes the following steps:
s1, preparing sludge activated carbon:
drying and dehydrating the sludge, crushing and sieving to obtain sludge powder, wherein the particle size of the dried and dehydrated sludge is 150-350 meshes, more preferably 200-250 meshes, the water content of the dried sludge is 6-10%, the dry organic matter content is 40-70%, and the dry ash content is 40-60%;
drying and dehydrating biomass materials, crushing and sieving to obtain biomass material powder, wherein the biomass material powder is dried, dehydrated and crushed to have the granularity of 150-350 meshes, more preferably 200-250 meshes, the water content of the biomass material powder is 6-10%, the dry-basis organic matter content of the biomass material powder is 70-99%, and the dry-basis ash content of the biomass material powder is 1-40%;
uniformly mixing the sludge powder, the biomass material powder and the binder according to a formula ratio, adding a proper amount of water, kneading for 40-60 min to obtain a mixed material, conveying the mixed material to a strip extruding machine for granulation molding, and performing aging treatment (the aging temperature is 60-85 ℃, and the aging time is 8-24 h) to obtain an active carbon raw blank, wherein the diameter of the active carbon raw blank is 8-10 mm, and the length of the active carbon raw blank is 3-15 mm;
carbonizing and activating the raw activated carbon blank to obtain sludge activated carbon;
s2, modification treatment of sludge activated carbon:
soaking the sludge activated carbon in a hydrochloric acid solution for a period of time, washing the sludge activated carbon to be neutral by water,
placing the pretreated sludge activated carbon into an ethanol solution for oscillation treatment, and then washing and filtering;
then washing the sludge activated carbon for multiple times by using hot water, and filtering to obtain a sludge activated carbon carrier;
s3, loading a copper-based catalyst:
weighing a formula amount of copper salt, adding water, stirring and dissolving to form a solution, adding modified sludge activated carbon serving as a carrier into the solution according to a proportion, shaking at a constant temperature until the water is evaporated to dryness (the shaking temperature is 80 ℃), obtaining a granular substance,
and drying and roasting the granular substances to obtain the sludge activated carbon loaded with the copper-based catalyst.
The third aspect of the invention provides an application of the sludge activated carbon loaded with the copper-based catalyst, and the sludge activated carbon loaded with the copper-based catalyst is used in the field of flue gas desulfurization and denitrification.
Compared with the prior art, the invention has the following beneficial effects:
(1) The sludge activated carbon loaded with the copper-based catalyst is prepared from sludge and biomass solid waste, so that the quality of the activated carbon is improved, and the activated carbon has a developed pore structure, a large specific surface area, abundant surface functional groups and good adsorption performance; the high adsorption performance of the carrier (sludge activated carbon) is combined with the catalytic performance of the copper-based catalyst, so that the adsorption and degradation of organic pollutants are facilitated, the denitration efficiency is excellent, the purpose of' treating wastes with processes of wastes is achieved, and the principle of recycling solid wastes is met;
(2) The material is simple in preparation process, easy to operate and strong in market competitiveness, achieves the integrated process target of desulfurization and denitrification, and achieves the environmental protection targets of reduction, harmlessness and recycling treatment of municipal sludge.
Detailed Description
The catalysts of the present invention, their preparation and use are further illustrated by the following examples, but the invention should not be construed as being limited to the examples.
In the embodiment of the application, the papermaking sludge with the water content of 32% is selected as the sludge, the coconut shell is selected as the biomass material, and the polyethylene glycol 4000 is selected as the binder.
Example 1
A preparation method of sludge activated carbon loaded with a copper-based catalyst comprises the following steps:
s1, preparing sludge activated carbon:
(1) Drying and dehydrating a paper making sludge raw material with the water content of 32%, crushing, and sieving with a 200-mesh sieve to obtain paper making sludge powder;
(2) Drying and dehydrating the coconut shell fragments, crushing, and sieving with a 200-mesh sieve to obtain coconut shell powder;
(3) Mixing paper-making sludge powder, coconut shell powder and a binder polyethylene glycol 4000 in a weight ratio of 8:2:1, uniformly mixing, adding a proper amount of water, and kneading for 60min to obtain a mixed material;
(4) Conveying the mixed material to a strip extruding machine for granulation molding to obtain a cylindrical active carbon wet blank with the diameter of 10mm, and then performing aging treatment for 8 hours at the temperature of 60 ℃ to obtain an active carbon raw blank;
(5) Conveying the active carbon raw blank into a carbonization-activation integrated furnace, and carrying out pyrolysis and carbonization treatment under the conditions that the carbonization temperature is 600 ℃, the carbonization time is 0.5h, and the carbonization temperature rise is 10 ℃/min to obtain a carbonized material;
and selecting a physical activation mode, wherein the activation temperature is 900 ℃, the activation time is 1h, the activation temperature rise temperature is 10 ℃/min, the water-carbon ratio is 1:1, performing high-temperature activation treatment, drying, granulating and packaging to obtain a high-performance sludge activated carbon finished product;
s2, modification treatment of sludge activated carbon:
(1) Putting the sludge activated carbon into 5mol/L hydrochloric acid solution, soaking for 2h at 80 ℃, washing with water until the pH value is neutral,
(2) Placing the pretreated sludge activated carbon into an ethanol solution for oscillation treatment at the oscillation temperature of 40 ℃ for 2 hours, and then washing and filtering;
(3) Repeatedly washing 3 the sludge-washing activated carbon by using hot water at 60 ℃, and filtering to obtain a sludge activated carbon carrier;
s3, loading a copper-based catalyst:
(1) Weighing copper nitrate, putting the copper nitrate into a beaker, adding deionized water into the beaker, and dissolving a solid into a solution by using magnetic stirring;
(2) Taking the modified sludge activated carbon as a carrier, wherein the mass ratio of an active component (copper nitrate) to the carrier (sludge activated carbon) is 0.1:1 is added into the solution at a constant temperature of 80 ℃, and is shaken until the water is evaporated to dryness to obtain granular substances;
(3) And drying the granular substances at 120 ℃ for 8h, and roasting at 550 ℃ for 5h under the nitrogen protection atmosphere to obtain the sludge activated carbon loaded with the copper-based catalyst.
Example 2
A preparation method of sludge activated carbon loaded with a copper-based catalyst comprises the following steps:
s1, preparing sludge activated carbon:
(1) Drying and dehydrating a paper making sludge raw material with the water content of 32%, crushing, and sieving with a 200-mesh sieve to obtain paper making sludge powder;
(2) Drying and dehydrating the coconut shell fragments, crushing, and sieving with a 200-mesh sieve to obtain coconut shell powder;
(3) Mixing paper-making sludge powder, coconut shell powder and a binder polyethylene glycol 4000 in a weight ratio of 8:2:1, uniformly mixing, adding a proper amount of water, and kneading for 60min to obtain a mixed material;
(4) Conveying the mixed material to a strip extruding machine for granulation molding to obtain a cylindrical active carbon wet blank with the diameter of 10mm, and then performing aging treatment for 8 hours at the temperature of 60 ℃ to obtain an active carbon raw blank;
(5) Conveying the active carbon raw blank into a carbonization-activation integrated furnace, and carrying out pyrolysis and carbonization treatment under the conditions that the carbonization temperature is 600 ℃, the carbonization time is 0.5h, and the carbonization temperature rise is 10 ℃/min to obtain a carbonized material;
and selecting a physical activation mode, wherein the activation temperature is 900 ℃, the activation time is 1h, the activation temperature rise temperature is 10 ℃/min, the water-carbon ratio is 1:1, performing high-temperature activation treatment, drying, granulating and packaging to obtain a high-performance sludge activated carbon finished product;
s2, modification treatment of sludge activated carbon:
(1) Placing the sludge activated carbon in 7mol/L hydrochloric acid solution, soaking for 1h at 60 ℃, washing with water until the pH value is neutral,
(2) Placing the pretreated sludge activated carbon into an ethanol solution for oscillation treatment at the oscillation temperature of 40 ℃ for 2 hours, and then washing and filtering;
(3) Repeatedly washing 3 the sludge-washing activated carbon by using hot water at 60 ℃, and filtering to obtain a sludge activated carbon carrier;
s3, loading a copper-based catalyst:
(1) Weighing copper acetate, putting the copper acetate into a beaker, adding deionized water into the beaker, and dissolving the solid into a solution by magnetic stirring;
(2) Taking the modified sludge activated carbon as a carrier, wherein the mass ratio of an active component (copper acetate) to the carrier (sludge activated carbon) is 0.05:1 is added into the solution at a constant temperature of 80 ℃, and is shaken until the water is evaporated to dryness to obtain granular substances;
(3) And drying the granular substances at 120 ℃ for 8h, and roasting at 600 ℃ for 4h under the nitrogen protection atmosphere to obtain the sludge activated carbon loaded with the copper-based catalyst.
Example 3
A preparation method of sludge activated carbon loaded with a copper-based catalyst comprises the following steps:
s1, preparing sludge activated carbon:
(1) Drying and dehydrating a paper making sludge raw material with the water content of 32%, crushing, and sieving with a 200-mesh sieve to obtain paper making sludge powder;
(2) Drying and dehydrating the coconut shell fragments, crushing, and sieving with a 200-mesh sieve to obtain coconut shell powder;
(3) Mixing paper mill sludge powder, coconut shell powder and a binder polyethylene glycol 4000 in a weight ratio of 8:2:1, uniformly mixing, adding a proper amount of water, and kneading for 60min to obtain a mixed material;
(4) Conveying the mixed material to a strip extruding machine for granulation molding to obtain a cylindrical active carbon wet blank with the diameter of 10mm, and aging at 60 ℃ for 8 hours to obtain an active carbon raw blank;
(5) Conveying the active carbon raw blank into a carbonization-activation integrated furnace, and carrying out pyrolysis and carbonization treatment under the conditions that the carbonization temperature is 600 ℃, the carbonization time is 0.5h, and the carbonization temperature rise is 10 ℃/min to obtain a carbonized material;
and selecting a physical activation mode, wherein the activation temperature is 900 ℃, the activation time is 1h, the activation temperature rise temperature is 10 ℃/min, the water-carbon ratio is 1:1, performing high-temperature activation treatment, drying, granulating and packaging to obtain a high-performance sludge activated carbon finished product;
s2, modification treatment of sludge activated carbon:
(1) Placing the sludge activated carbon in 3mol/L hydrochloric acid solution, soaking for 4h at 80 ℃, washing with water until the pH value is neutral,
(2) Placing the pretreated sludge activated carbon into an ethanol solution for oscillation treatment at the oscillation temperature of 40 ℃ for 2 hours, and then washing and filtering;
(3) Repeatedly washing the sludge activated carbon for 3 times by using hot water at 70 ℃, and filtering to obtain a sludge activated carbon carrier;
s3, loading a copper-based catalyst:
(1) Weighing copper nitrate and copper acetate in a mass ratio of 1:1, putting the copper nitrate and the copper acetate into a beaker, adding deionized water into the beaker, and dissolving the solid into a solution by magnetic stirring;
(2) Taking the modified sludge activated carbon as a carrier, wherein the mass ratio of active components (copper nitrate and copper acetate) to the carrier (sludge activated carbon) is 0.13:1 is added into the solution at a constant temperature of 80 ℃, and is shaken until the water is evaporated to dryness to obtain granular substances;
(3) And drying the granular substances at 120 ℃ for 8h, and then roasting the granular substances at 300 ℃ for 8h under the nitrogen protection atmosphere to obtain the sludge activated carbon loaded with the copper-based catalyst.
Comparative example 1
This comparative example is a comparative example to example 1, the main differences being:
in the embodiment, the sludge activated carbon finished product is prepared through the formula proportioning and the preparation flow in the step S1, and subsequent modification treatment and operation of loading a copper-based catalyst are not performed on the sludge activated carbon finished product.
Comparative example 2
This comparative example is a comparative example to example 1, the main differences being:
in the step S3, the mass ratio of the active component (copper nitrate) to the carrier (sludge activated carbon) added during the reaction is 0.25:1, other preparation methods and component ratios are the same as those of example 1.
Comparative example 3
This comparative example is a comparative example to example 1, the main differences being:
in step S3, the roasting temperature of the particulate matter under the nitrogen atmosphere is 600 ℃, and other preparation methods and component ratios are the same as those in example 1.
Examples of the experiments
The desulfurization and denitrification performance tests were performed on the finished products prepared in example 1 and comparative examples 1 to 3, respectively.
The specific test process is as follows: and when simulating flue gas desulfurization and denitrification, a gas cylinder is adopted for supplying gas, and all gases except an oxygen gas cylinder and a nitrogen gas cylinder use nitrogen as carrier gas.
The total gas content of the simulated smoke is 2.5L, wherein the simulated smoke contains 400ppmNO,500ppmSO 2 170ppm NH 3 16% of O 2 10% of water vapor and the balance of N 2 . The method adopts an MRU5 flue gas analyzer of York corporation in America to detect SO in simulated flue gas before and after reaction under different conditions 2 And the concentration of NO.
According to SO 2 And the change of the inlet series data and the outlet series data of NO, and calculating the desulfurization value and the denitrification rate of the sample to be tested.
The test results are shown in Table 1.
TABLE 1
As can be seen from the test results in table 1:
comparing the performance test results of the sludge activated carbon loaded with the copper-based catalyst in the example 1 with the performance test results of the sludge activated carbon prepared in the comparative example 1, the denitration performance of the papermaking sludge activated carbon material loaded with the copper-based catalyst is remarkably improved, and the desulfurization performance is also improved. The method is mainly characterized in that the catalytic performance of the copper-based catalyst is effectively combined with the adsorption performance of the carrier due to the loading of the copper-based catalyst, and the desulfurization performance and the denitration performance are comprehensively improved under the simulated flue gas condition with ammonia as a reducing agent.
Compared with example 1, comparative example 2 changes the mass ratio of the active component (copper nitrate) added in the reaction with the carrier (sludge activated carbon) to 0.25:1, the dosage of the active component is increased, and at the moment, the desulfurization performance and the denitration performance of the sludge activated carbon material loaded with the copper-based catalyst in the comparative example 2 are both remarkably improved. This is mainly because the copper-based catalyst has a high loading ratio and enhanced catalytic performance, so that the removal effect of the finished product is enhanced.
Compared with the example 1, in the comparative example 3, the roasting temperature of the granular substances in the step S3 is changed to 600 ℃, that is, the roasting temperature is increased, and at this time, the desulfurization performance and the denitration performance of the sludge activated carbon material loaded with the copper-based catalyst in the comparative example 3 are both significantly improved. This is mainly because the copper-based catalyst has enhanced catalytic performance, so that the removal effect of the finished product is enhanced.
In conclusion, the sludge activated carbon loaded with the copper-based catalyst improves the quality of the activated carbon by using sludge and biomass solid waste as raw materials, and has a developed pore structure, a large specific surface area, abundant surface functional groups and good adsorption performance; the high adsorption performance of the carrier (sludge activated carbon) is combined with the catalytic performance of a copper-based catalyst, so that the adsorption and degradation of organic pollutants are facilitated, the denitration efficiency is excellent, the purpose of 'treating waste with waste' is achieved, and the principle of recycling solid waste is met; the preparation process of the material is simple, the operation is easy, the market competitiveness is strong, the integrated process target of desulfurization and denitrification is achieved, and the environmental protection targets of reduction, harmlessness and resource treatment of municipal sludge are realized.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (10)
1. The sludge activated carbon loaded with the copper-based catalyst is characterized by being prepared by reacting sludge activated carbon with a copper metal salt;
wherein the sludge activated carbon is prepared from the following components in percentage by mass (50-90): (10-50): (5-25) the sludge, the biomass material and the binder, and after the raw materials are mixed, the raw materials are carbonized and activated;
the mass ratio of the metal copper salt to the sludge activated carbon is (0.01-0.25): 1.
2. the copper-based catalyst-loaded sludge activated carbon according to claim 1, wherein the sludge activated carbon is subjected to modification treatment before being reacted with a copper metal salt.
3. The copper-based catalyst-supported sludge activated carbon according to claim 2, wherein the modification treatment process comprises hydrochloric acid impregnation treatment, ethanol washing and hot water rinsing.
4. The copper-based catalyst-loaded sludge activated carbon according to claim 3, wherein in the hydrochloric acid impregnation treatment process, the concentration of a hydrochloric acid solution is 2-7 mol/L, the impregnation time is 1-4 h, and the impregnation temperature is 40-150 ℃; in the ethanol cleaning treatment process, the pretreated sludge activated carbon is placed in an ethanol solution for oscillation treatment, the oscillation temperature is 20-60 ℃, and the oscillation time is 1-8 h; in the hot water washing process, the temperature of the hot water is 60-90 ℃, and the washing times are 1-5 times.
5. The copper-based catalyst-loaded sludge activated carbon according to claim 1, wherein the sludge activated carbon is dried and roasted after reacting with a copper metal salt.
6. The copper-based catalyst-loaded sludge activated carbon according to claim 5, wherein the drying temperature is 90-150 ℃, and the drying time is 3-20 h; the roasting process is carried out under the protection of air atmosphere, oxygen-poor atmosphere or nitrogen atmosphere, the roasting temperature is 300-600 ℃, and the roasting time is 4-8 h.
7. The copper-based catalyst-supported sludge activated carbon according to claim 1, wherein the metallic copper salt is one or more of copper nitrate, copper acetate, copper carbonate and copper chloride.
8. The copper-based catalyst-supported sludge activated carbon according to claim 1, wherein the mass ratio of the copper metal salt to the sludge activated carbon is (0.05-0.13): 1.
9. the method for preparing the copper-based catalyst-loaded sludge activated carbon according to any one of claims 1 to 8, which comprises the following steps:
s1, preparing sludge activated carbon:
drying and dehydrating the sludge, crushing and sieving to obtain sludge powder, drying and dehydrating the biomass material, crushing and sieving to obtain biomass material powder,
uniformly mixing the sludge powder, the biomass material powder and the binder according to the formula ratio, adding a proper amount of water for kneading to obtain a mixed material, granulating and molding the mixed material, aging to obtain an active carbon raw blank,
carbonizing and activating the raw activated carbon blank to obtain sludge activated carbon;
s2, modification treatment of sludge activated carbon:
soaking the sludge activated carbon in a hydrochloric acid solution for a period of time, washing the sludge activated carbon to be neutral by water,
placing the pretreated sludge activated carbon into an ethanol solution for oscillation treatment, and then washing and filtering;
washing the sludge activated carbon for multiple times by using hot water, and filtering to obtain a sludge activated carbon carrier;
s3, loading a copper-based catalyst:
weighing the metal copper salt with the formula ratio, adding water into the metal copper salt, stirring and dissolving the metal copper salt to form a solution, taking the modified sludge activated carbon as a carrier, adding the modified sludge activated carbon into the solution according to a proportion to react to obtain granular substances,
and drying and roasting the granular substances to obtain the sludge activated carbon loaded with the copper-based catalyst.
10. The application of the copper-based catalyst-supported sludge activated carbon as claimed in any one of claims 1 to 8, wherein the copper-based catalyst-supported sludge activated carbon is used in the field of flue gas desulfurization and denitrification.
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