CN112452112A - Isopropanol waste gas water absorption coupling photocatalytic purification method - Google Patents
Isopropanol waste gas water absorption coupling photocatalytic purification method Download PDFInfo
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 title claims abstract description 216
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000002912 waste gas Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 39
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 32
- 230000008878 coupling Effects 0.000 title claims abstract description 26
- 238000010168 coupling process Methods 0.000 title claims abstract description 26
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 26
- 238000000746 purification Methods 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000007146 photocatalysis Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000005286 illumination Methods 0.000 claims abstract description 11
- 238000013032 photocatalytic reaction Methods 0.000 claims abstract description 9
- 238000005507 spraying Methods 0.000 claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 47
- 239000007921 spray Substances 0.000 claims description 28
- 239000003054 catalyst Substances 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 16
- 238000012856 packing Methods 0.000 claims description 14
- 230000008859 change Effects 0.000 claims description 7
- 238000003988 headspace gas chromatography Methods 0.000 claims description 6
- 238000004817 gas chromatography Methods 0.000 claims description 5
- 229910052724 xenon Inorganic materials 0.000 claims description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052753 mercury Inorganic materials 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 description 5
- 239000001509 sodium citrate Substances 0.000 description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000002135 nanosheet Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
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- 239000007790 solid phase Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 238000006065 biodegradation reaction Methods 0.000 description 2
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- -1 isopropyl fatty acid isopropyl ester Chemical class 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 239000002385 cottonseed oil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- ULYZAYCEDJDHCC-UHFFFAOYSA-N isopropyl chloride Chemical compound CC(C)Cl ULYZAYCEDJDHCC-UHFFFAOYSA-N 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—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 absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—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 absorption
- B01D53/1418—Recovery of products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—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 absorption
- B01D53/1487—Removing organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
- B01D2252/103—Water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/80—Type of catalytic reaction
- B01D2255/802—Photocatalytic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention discloses an isopropanol waste gas water absorption coupling photocatalytic purification method which is characterized in that isopropanol waste gas is introduced into spraying liquid of absorption liquid, photocatalyst is added into the spraying liquid absorbing isopropanol, absorption coupling photocatalytic reaction is carried out under the conditions of illumination and stirring, the waste gas after reaction reaches the standard and is discharged, and isopropanol and the absorption liquid are recovered from the spraying liquid; the isopropanol waste gas water absorption coupling photocatalysis purification process provided by the invention can combine water absorption and photocatalysis into a whole, has small occupied area, simple equipment, simple and convenient operation and mild reaction conditions, can be widely applied to the treatment of isopropanol waste gas in various industries, and has the purification rate of the isopropanol waste gas reaching 97.1 percent and the degradation rate reaching 90.6 percent.
Description
(I) technical field
The invention relates to an isopropanol waste gas water absorption coupling photocatalytic purification method.
(II) background of the invention
The isopropanol is used as an important chemical product and raw material and can be used for generating acetone, isopropyl ether, isopropyl chloride, isopropyl fatty acid isopropyl ester, isopropyl chlorofatty acid isopropyl ester and the like; the product can be used as an industrially cheaper solvent, has wide application, can be freely mixed with water, has stronger dissolving capacity to lipophilic substances than ethanol, and can be used for producing coatings, cottonseed oil extracting agents in the grease industry, cleaning and deoiling agents in the electronic industry, demolding of animal-derived tissues and the like. However, a large amount of isopropanol exhaust gas with high concentration is inevitably generated in the using process, the high concentration exhaust gas can affect human bodies and the environment, and the high concentration exhaust gas can cause combustion and explosion when meeting open fire and high heat.
At present, main treatment methods aiming at the isopropanol waste gas comprise an absorption method, a combustion method, a biodegradation method, a photocatalysis method and the like. The absorption method is a common treatment process for water-soluble organic waste gas, can treat high-concentration isopropanol waste gas, but in the absorption process, the concentration of the isopropanol in the water body is continuously increased, the subsequent absorption effect on the isopropanol waste gas is limited, and the high-concentration isopropanol waste gas can generate wastewater after being absorbed by water, so that serious secondary pollution is caused and certain toxicity is achieved. The combustion method capable of thoroughly eliminating the isopropanol waste gas needs a large amount of energy consumption in the combustion process, isopropanol vapor can form a mixture with a wide explosion range with air, and the mixture is dangerous to explode when meeting a heat source and open fire, so that certain potential safety hazards exist. The problem of low degradation efficiency, large occupied area and the like exists when the biodegradation method is used for degrading the isopropanol waste gas. Photocatalysis is used as a green and clean new energy source, can convert solar energy into chemical energy, has the outstanding characteristics of low energy consumption, environmental friendliness and the like, but can generate more intermediate products in the process of treating isopropanol waste gas, and has the problems of incomplete degradation and low mineralization rate.
Due to the characteristic that isopropanol can be mixed and dissolved with water, the existing isopropanol waste gas treatment technology is mainly a water absorption process. The absorption method has the advantages of low energy consumption, low cost, simple operation, wide practical range and the like, but how to overcome the secondary pollution to the water body after absorption and exert the advantages thereof effectively solves the problem of isopropanol waste gas pollution and can be applied in large scale, and is a technical problem which needs to be solved urgently in the field of environmental purification at present.
Disclosure of the invention
The invention aims to overcome the defects of the existing isopropanol waste gas purification treatment technology, and provides an isopropanol waste gas water absorption coupling photocatalytic purification method, which combines a water absorption process with a photocatalytic oxidation technology, solves the problems of limited absorption later effect and wastewater pollution existing in the water absorption method, solves the problems of easy inactivation, slow oxidation rate, low mineralization rate and the like of a catalyst existing in gas-solid phase photocatalysis, and simultaneously saves the operation cost, thereby being an isopropanol waste gas treatment technology with high efficiency and practicability.
The technical scheme adopted by the invention is as follows:
the invention provides a gas-water absorption coupling photocatalytic purification method for isopropanol waste gas, which comprises the steps of introducing the isopropanol waste gas into a spray liquid of an absorption liquid, simultaneously adding a photocatalyst into the spray liquid absorbing the isopropanol, carrying out absorption coupling photocatalytic reaction under the conditions of illumination and stirring, and discharging the waste gas after the reaction up to the standard (when the concentration of the isopropanol is lower than 50 mg/m)3Discharging when reaching standards), and recovering isopropanol and absorption liquid from the spray liquid; the absorption liquid is water; the illumination adopts 100-500W light source (preferably 300W).
Further, the photocatalyst comprises g-C3N4、TiO2、ZnO、MoS2、BiVO4A composite photocatalyst formed by compounding two or more semiconductor materials with the semiconductor photocatalyst (such as g-C)3N4/TiO2) And supported photocatalyst supported by metal element such as Au, Ag, Pt or the like (for example, Ag/g-C)3N4/TiO2) And a photocatalyst modified by doping a nonmetallic element such as B, S, P (for example, H)3BO3-g-C3N4) Preferably TiO2、g-C3N4、g-C3N4/TiO2Composite catalyst or Ag/g-C3N4/TiO2Composite catalyst of which g-C3N4/TiO2g-C in the composite catalyst3N4The mass content is 60%; Ag/g-C3N4/TiO2g-C in the composite catalyst3N4Accounts for 60 percent of the mass content and 1.2 percent of the mass content of Ag.
Further, the g-C3N4/TiO2Preparation method (refer to King Wen, Zhao Qing Hua, et al. TiO)2/g-C3N4Preparation of composite nano photocatalyst and its photocatalytic performance [ J]Micro-nano electronic technology, 2020, 450-: firstly g-C3N4And TiO2Respectively adding into deionized water, respectively stirring for 1 hr, ultrasonic (50Hz) dispersing for 1 hr to obtain g-C3N4Suspension and TiO2Suspending liquid; under the condition of magnetic stirring, g-C is added3N4The suspension is added dropwise to the TiO2Continuously magnetically stirring the suspension for 12h, centrifuging at 8000r/min for 20min, washing the precipitate with deionized water for 3 times, and collecting the solid product at 200 deg.C under N2Heat treatment under atmosphere for 2h to obtain g-C3N4/TiO2A heterojunction photocatalyst; the TiO is2And g-C3N4The mass ratio is 1: 1.5; volume of the deionized water is used for TiO2The mass is 0.5-1L/g.
Further, the Ag/g-C3N4/TiO2Preparation method (refer to plum blossom, Zhangxian, etc.. g-C3N4/Ag//TiO2Construction of composite materials and photocatalytic Properties [ J ]]Inorganic chemistry bulletin 2020,36(03), 566-: adding TiO into the mixture2And PVP (polyvinylpyrrolidone) in water and stirred for 30min, then AgNO was added under stirring3And an aqueous solution of sodium citrate is added dropwise to the solution; subsequently, the mixed solution was stirred and maintained at 100 ℃ for 1 hour. Cooling to room temperature, collecting the product, washing with deionized water, adding anhydrous ethanol, centrifuging, and drying the precipitate at 60 deg.C for 12 hr to obtain Ag/TiO2(ii) a Mixing Ag with TiO2And g-C3N4Adding the nanosheet into absolute ethyl alcohol, ultrasonically dispersing for 2h at 50Hz, stirring for 48h at 500rpm, centrifuging, dispersing the precipitate with absolute ethyl alcohol, centrifuging, drying at 60 ℃ for 12h to obtain the catalyst Ag/g-C3N4/TiO2(ii) a The TiO is2The mass ratio of the PVP to the PVP is 1: 0.25; the volume of the water is TiO2The weight is 40 mL/g; the AgNO3And sodium citrate in a volume amount of TiO2The weight is 40 mL/g; the AgNO3And sodium citrate in aqueous solution, AgNO3The concentration is 1.125g/L, and the concentration of sodium citrate is 5 g/L; the Ag/TiO2And g-C3N4The mass ratio of the nano sheets is 1: 1.5; the volume dosage of the absolute ethyl alcohol for ultrasonic dispersion is Ag/TiO2And g-C3N4The total amount of the nano sheets is 240 mL/g.
Further, the amount of the photocatalyst added is 1g/L to 10g/L, preferably 3 g/L to 5g/L, in terms of the volume of the absorbed liquid.
Further, the absorption coupling photocatalytic reaction conditions are as follows: the temperature is 25 ℃, the pressure is 101.3KPa, and the stirring speed is 500 rpm.
Furthermore, the method is carried out by adopting an isopropanol waste gas water absorption coupling photocatalytic purification device, and the device comprises a spray tower T01 and a circulating pump P01; the spray tower T01 consists of a tower body and a tower seat for storing absorption liquid, and the tower body is hermetically connected with the tower seat; an exhaust port is formed in the top of the tower body and used for exhausting treated gas, a spray header 1 is arranged at the upper end inside the tower body, and a packing layer 2 is arranged below the spray header 1; the side surface of the bottom end of the tower body is provided with an air inlet for introducing isopropanol waste gas, and the air inlet is positioned below the packing layer; a stirrer 3 and a light source column 4 are arranged in the tower base, a water outlet is arranged on the side surface of the tower base, a filter screen 5 is arranged at the water outlet, and the water outlet is communicated with the spray header 1 through a circulating pump P01; the packing layer takes plastic hollow balls as packing;
the isopropanol waste gas treatment method comprises the following steps: adding absorption liquid and photocatalyst into a tower base, introducing isopropanol waste gas into the tower body from an air inlet, simultaneously starting a circulating pump to spray the absorption liquid into a packing layer, starting a light source and stirring, carrying out absorption coupling photocatalytic reaction at normal temperature and normal pressure (preferably 25 ℃, 101.3KPa), stirring (preferably 500rpm) and under illumination, detecting the concentration of isopropanol at the air outlet by adopting gas chromatography, and when the concentration of isopropanol is lower than 50mg/m3When the reaction is carried out, the treated gas is discharged after reaching the standard, otherwise, the treated gas is used as isopropanol waste gas to continue the reaction; measuring the concentration of isopropanol in the solution of the tower base by adopting a headspace gas chromatography, and recovering the isopropanol and recycling the absorption liquid when the concentration of the isopropanol in the solution does not change along with the change of time any more; the absorption liquid is water.
Further, the interval between the light source columns is 30-70 cm, a xenon lamp or a mercury lamp is adopted as the light source, a 300W long-arc xenon lamp is preferred, the diameter is 24mm, and the length of the light emitting body is 190 mm.
Furthermore, the invention is provided with the filter screen to prevent the photocatalyst from blocking the filler layer in the spraying process.
The invention stops spraying after the introduction of isopropanol waste gas is stopped, continues to react under normal temperature and pressure, stirring and illumination, adopts the headspace gas chromatography to measure the concentration of isopropanol in the solution of the tower base, and recovers the isopropanol and the absorption liquid for cyclic utilization when the concentration of the isopropanol in the solution does not change along with the change of time any more.
The isopropanol waste gas is introduced into the spray tower, the isopropanol waste gas continuously rises to penetrate through the spray liquid, most of isopropanol organic molecules are captured by water and dissolved in the water in the rising process, and the rest isopropanol organic molecules which are not absorbed by the water continuously rise to continuously penetrate through the packing layer and fully contact with the water under the action of water spraying to be further absorbed, so that the isopropanol waste gas is converted into wastewater; irradiating the absorption liquid in the spray tower by using a light source in the absorption process, and oxidizing and decomposing isopropanol organic molecules captured in a water body into carbon dioxide and water in real time under the photocatalysis effect; and tail gas obtained after the isopropanol waste gas is treated by the absorption coupling photocatalysis technology is discharged into the air after reaching the standard through a gas outlet at the top of the tower. And after absorption, closing a circulating pump of the absorption spray tower, continuously illuminating under the stirring action, further oxidizing and decomposing the undegraded isopropanol organic molecules in the water after the water is treated by the absorption coupling photocatalysis technology, and continuously using the treated and purified water as isopropanol waste gas absorption liquid for recycling.
The principle of the invention for treating isopropanol waste gas is as follows: the water in the spray tower absorbs the isopropanol waste gas at the inlet, and the absorbed isopropanol waste gas is fully contacted with the photocatalyst dispersed in the water, and the photocatalyst can generate OH and O with oxidation capacity under the condition of illumination2-And h+Under the action of free radicals, isopropanol molecules are oxidized into carbon dioxide and water, so that isopropanol waste gas pollutants are thoroughly purified, and the purified gas is discharged and exhausted.
Compared with the prior art, the invention has the following advantages:
(1) the isopropanol waste gas can basically reach the standard after being subjected to a water absorption coupling photocatalysis purification process.
(2) The isopropanol waste gas water absorption coupling photocatalytic purification process provided by the invention solves the problems of large water consumption, limited effect at the later absorption stage, wastewater pollution and the like of the traditional isopropanol waste gas water absorption process.
(3) According to the isopropanol waste gas water absorption coupling photocatalytic purification process provided by the invention, due to the washing effect of the photocatalyst in a liquid phase, an intermediate product cannot be accumulated on the surface of the catalyst like gas-solid phase photocatalysis, and the problems that the catalyst is easy to inactivate and is incompletely oxidized to generate the intermediate product in the gas-solid phase photocatalytic reaction are solved.
(4) According to the water absorption coupling photocatalytic purification process for the isopropanol waste gas, the retention time of isopropanol organic molecules and a photocatalyst is increased after the isopropanol waste gas is absorbed by water, and the photocatalytic reaction rate is increased.
The isopropanol waste gas water absorption coupling photocatalysis purification process provided by the invention can combine water absorption and photocatalysis into a whole, has small occupied area, simple equipment, simple and convenient operation and mild reaction conditions, can be widely applied to the treatment of isopropanol waste gas in various industries, and has the purification rate of the isopropanol waste gas reaching 97.1 percent and the degradation rate reaching 90.6 percent.
(IV) description of the drawings
FIG. 1 is a flow chart of a process for gas-water absorption coupling photocatalytic purification of isopropanol wastewater; t01-spray column; p01-circulating pump; 1-a spray header; 2-a filler layer; 3-a stirrer; 4-a light source column; 5-a filter screen.
FIG. 2 is a gas chromatogram of isopropanol.
FIG. 3 is a headspace gas chromatogram of isopropanol.
(V) detailed description of the preferred embodiments
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1
Referring to fig. 1, the isopropanol wastewater gas absorption coupling photocatalytic purification device comprises a spray tower T01 and a circulating pump P01; the spray tower T01 consists of a tower body and a tower seat for storing absorption liquid, and the tower body is hermetically connected with the tower seat; an exhaust port is formed in the top of the tower body and used for exhausting treated gas, a spray header 1 is arranged at the upper end inside the tower body, and a packing layer 2 is arranged below the spray header 1; the side surface of the bottom end of the tower body is provided with an air inlet for introducing isopropanol waste gas, and the air inlet is positioned below the packing layer; the improved shower head is characterized in that a stirrer 3 and a light source column 4 are arranged in the tower base, a water outlet is formed in the side face of the tower base, a filter screen 5 is arranged at the water outlet, and the water outlet is communicated with the shower head 1 through a circulating pump P01. The packing layer is filled with plastic hollow balls with the diameter of 50 mm.
The tower seat is filled with a photocatalyst which is powdered TiO2In which TiO is2The crystal form of (A) is anatase type. Tower with a tower bodyBody 40mm 200mm, column base 250mm 40 mm.
The isopropanol waste gas treatment method comprises the following steps: adding 100mL of water as an absorption liquid into a tower seat, and adding TiO20.5g of photocatalyst, 1 long-arc xenon lamp (diameter 24mm, light-emitting body length 190mm) of 300W was set as the light source; will contain 1000mg/m3Introducing isopropanol air as isopropanol waste gas into spray tower at flow rate of 0.3L/min from gas inlet, starting circulation pump and light source, performing absorption coupling photocatalytic reaction at normal temperature and pressure (25 deg.C, 101.3KPa), stirring (500rpm) and under illumination, monitoring isopropanol concentration at gas outlet by gas chromatography, and when the isopropanol concentration at gas outlet is lower than 50mg/m3Discharging the obtained product after reaching the standard, or continuously introducing the obtained product into a spray tower as isopropanol waste gas; and (3) measuring the concentration of the isopropanol in the solution in the tower base by adopting a headspace gas chromatography, and separating and recovering the isopropanol after reduced pressure distillation when the concentration of the isopropanol in the solution is almost not changed, wherein water is used as an absorption liquid for recycling.
Detecting the concentration of the isopropanol at the air inlet and the air outlet by adopting gas chromatography in the reaction process, wherein the peak area of the concentration of the isopropanol at the air inlet is C0The peak area of the concentration of the isopropanol at the air outlet is C, and the calculated purification rate is 1-C/C0The results are shown in Table 1. The conditions for detecting isopropanol in the gas by gas chromatography (Jiemio GC1620) are as follows: sample inlet temperature 200 ℃, detector temperature 250 ℃, column box temperature 200 ℃, capillary column model: agilent HP-5, mobile phase: nitrogen, results are shown in figure 2.
Measuring the change of the concentration of isopropanol in the solution with time under the illumination condition by adopting a headspace gas chromatography, and recording the peak area of the first sampling chromatographic detection as C0', the peak area of the last sampling chromatographic detection is C ', and the degradation rate is calculated to be 1-C '/C0', the results are shown in Table 1. The detection conditions of the headspace gas chromatography are as follows: sample inlet temperature 200 ℃, detector temperature 250 ℃, column box temperature 60 ℃, capillary column model: agilent HP-5, mobile phase: nitrogen, sample introduction amount: 50uL, see FIG. 3 for results.
Example 2
The light source in example 1 was changed to a 300W high-pressure mercury lamp, and the results are shown in Table 1, except that the example 1 was changed.
Example 3
The photocatalyst in example 1 was changed to powder g-C3N4Otherwise, the results are shown in Table 1, as in example 1.
Example 4
The photocatalyst in example 1 was changed to powder g-C3N4/TiO2Wherein g-C3N4The results are shown in Table 1, except that the catalyst accounts for 60% of the mass of the composite catalyst in the same manner as in example 1.
g-C3N4/TiO2Preparation method (refer to King Wen, Zhao Qing Hua, et al. TiO)2/g-C3N4Preparation of composite nano photocatalyst and its photocatalytic performance [ J]Micro-nano electronic technology, 2020, 450-: firstly 0.15g g-C3N4And 0.1g TiO2Respectively adding into 100mL deionized water, respectively stirring for 1h, and ultrasonically dispersing for 1h (50Hz) to respectively obtain g-C3N4Suspension and TiO2The suspension is ready for use. Under the condition of magnetic stirring, g-C is added3N4The suspension is added dropwise to the TiO2Continuously magnetically stirring the suspension for 12h, centrifuging at 8000r/min for 20min, washing with deionized water for 3 times, and collecting solid product at 200 deg.C2Heat treatment under atmosphere for 2h to obtain g-C3N4/TiO2Heterojunction photocatalyst 0.25 g.
Example 5
The concentration of isopropanol in example 1 was changed to 2500mg/m3The photocatalyst is changed into powder g-C3N4/TiO2(same as example 4), wherein g-C3N4The results are shown in Table 1, except that the catalyst accounts for 60% of the mass of the composite catalyst in the same manner as in example 1.
Example 6
The photocatalyst in example 1 was changed to Ag/g-C in powder form3N4/TiO2Wherein g-C3N4The results are shown in Table 1, except that the catalyst composition accounts for 60% by mass of the composite catalyst, Ag accounts for 1.2% by mass of the composite catalyst, and the like.
Ag/g-C3N4/TiO2Preparation method (refer to plum blossom, Zhangxian, etc.. g-C3N4/Ag//TiO2Construction of composite materials and photocatalytic Properties [ J ]]Inorganic chemistry bulletin 2020,36(03), 566-: 0.5g of TiO2And 0.125g PVP (polyvinylpyrrolidone) in 20mL of water and stirred for 30min, then 0.0225g AgNO was added with stirring3And 20mL of an aqueous solution of 0.1g of sodium citrate was added dropwise to the above solution. Subsequently, the mixed solution was stirred and maintained at 100 ℃ for 1 hour. Cooling to room temperature, centrifuging, collecting product, washing with water, dissolving with anhydrous ethanol, centrifuging, and drying at 60 deg.C for 12 hr to obtain Ag/TiO20.51 g. 0.1g of Ag/TiO2And 0.15g g-C3N4Adding the nanosheets into 60mL of absolute ethyl alcohol, ultrasonically dispersing for 2h (50Hz), and stirring for 48h (500 rpm). Centrifuging, washing the product with 40mL of anhydrous ethanol, and drying at 60 deg.C for 12h to obtain catalyst Ag/g-C3N4/TiO20.25g。
Example 7
The concentration of isopropanol in example 1 was changed to 2500mg/m3The photocatalyst is changed into powdered Ag/g-C3N4/TiO2(same as example 6), wherein g-C3N4The results are shown in Table 1, except that the catalyst composition accounts for 60% by mass of the composite catalyst, Ag accounts for 1.2% by mass of the composite catalyst, and the like.
Example 8
The amount of the photocatalyst used in example 4 was adjusted to 0.3g, and the results are shown in Table 1, except that the amount of the photocatalyst used in example 1 was changed.
Example 9
The amount of the photocatalyst used in example 6 was adjusted to 0.3g, and the results are shown in Table 1, except that the amount of the photocatalyst used in example 1 was changed.
Example 10
The photocatalyst in example 1 was removed and no photocatalyst was added, and the results are shown in Table 1, which is the same as in example 1.
Example 11
The photocatalyst in example 1 was removed, no photocatalyst was added, and the concentration of isopropanol was changed to 2500mg/m3Otherwise, the results are shown in Table 1, as in example 1.
Table 1: purification efficiency treatment effect of isopropanol waste gas under different conditions
As can be seen from Table 1, the isopropanol waste gas treated by the method of the invention can be purified to reach the emission standard under the condition of changing the light source, the type and the dosage of the photocatalyst, and the absorption liquid can be recycled.
Claims (8)
1. A isopropanol waste gas water absorption coupling photocatalysis purification method is characterized in that isopropanol waste gas is introduced into spraying liquid of absorption liquid, photocatalyst is added into the spraying liquid absorbing isopropanol, absorption coupling photocatalysis reaction is carried out under the conditions of illumination and stirring, the waste gas after reaction reaches the standard and is discharged, and the isopropanol and the absorption liquid are recovered from the spraying liquid; the absorption liquid is water; the illumination adopts a light source of 100-500W.
2. The method of claim 1, wherein the photocatalyst is TiO2、g-C3N4、g-C3N4/TiO2Composite catalyst or Ag/g-C3N4/TiO2And (3) compounding a catalyst.
3. The method according to claim 1, wherein the photocatalyst is added in an amount of 1g/L to 10g/L in terms of the volume of the absorption liquid.
4. The method of claim 1, wherein the absorption coupled photocatalytic reaction conditions are: the temperature is 25 ℃, the pressure is 101.3KPa, and the stirring speed is 500 rpm.
5. The method of claim 1, wherein the light source is a xenon lamp or a mercury lamp.
6. The method of claim 1, wherein the method is carried out by using an isopropanol waste gas water absorption coupling photocatalytic purification device, the device comprises a spray tower, a circulating pump; the spray tower consists of a tower body and a tower base for storing absorption liquid, and the tower body is hermetically connected with the tower base; an exhaust port is arranged at the top of the tower body and used for exhausting the treated gas, a spray header is arranged at the upper end inside the tower body, and a packing layer is arranged below the spray header; the side surface of the bottom end of the tower body is provided with an air inlet for introducing isopropanol waste gas, and the air inlet is positioned below the packing layer; a stirrer and a light source column are arranged in the tower base, a water outlet is arranged on the side surface of the tower base, a filter screen is arranged at the water outlet, and the water outlet is communicated with the spray header through a circulating pump; the packing layer takes plastic hollow balls as packing;
the isopropanol waste gas treatment method comprises the following steps: adding absorption liquid and photocatalyst into a tower base, introducing isopropanol waste gas into the tower body from an air inlet, simultaneously starting a circulating pump to spray the absorption liquid into a packing layer, starting a light source and stirring, carrying out absorption coupling photocatalytic reaction under normal temperature and pressure, stirring and illumination, detecting the concentration of isopropanol at an air outlet by adopting gas chromatography, and when the concentration of isopropanol is lower than 50mg/m3When the reaction is carried out, the treated gas is discharged after reaching the standard, otherwise, the treated gas is used as isopropanol waste gas to continue the reaction; measuring the concentration of isopropanol in the solution of the tower base by adopting a headspace gas chromatography, and recovering the isopropanol and recycling the absorption liquid when the concentration of the isopropanol in the solution does not change along with the change of time any more; the absorption liquid is water.
7. The method of claim 8, wherein the light source posts are spaced 30-70 cm apart.
8. The method of claim 6, wherein the light source is a 300W long arc xenon lamp with a diameter of 24mm and a phosphor length of 190 mm.
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