CN108704624A - A kind of preparation method of photocatalytic activity adsorbent - Google Patents
A kind of preparation method of photocatalytic activity adsorbent Download PDFInfo
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- CN108704624A CN108704624A CN201810463270.4A CN201810463270A CN108704624A CN 108704624 A CN108704624 A CN 108704624A CN 201810463270 A CN201810463270 A CN 201810463270A CN 108704624 A CN108704624 A CN 108704624A
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 34
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920002678 cellulose Polymers 0.000 claims abstract description 47
- 239000001913 cellulose Substances 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 44
- 239000000843 powder Substances 0.000 claims description 42
- 239000000499 gel Substances 0.000 claims description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 23
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 229960000583 acetic acid Drugs 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 15
- 229920002522 Wood fibre Polymers 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 238000009413 insulation Methods 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims description 14
- 239000002025 wood fiber Substances 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 238000003763 carbonization Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 235000021110 pickles Nutrition 0.000 claims description 11
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 239000012362 glacial acetic acid Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 9
- 229960002218 sodium chlorite Drugs 0.000 claims description 9
- 241000219000 Populus Species 0.000 claims description 7
- MBLBDJOUHNCFQT-LXGUWJNJSA-N aldehydo-N-acetyl-D-glucosamine Chemical compound CC(=O)N[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO MBLBDJOUHNCFQT-LXGUWJNJSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 229920005610 lignin Polymers 0.000 claims description 7
- 241000196324 Embryophyta Species 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 6
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000000352 supercritical drying Methods 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 229920000297 Rayon Polymers 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 239000002070 nanowire Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 24
- 239000004964 aerogel Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 9
- 239000004408 titanium dioxide Substances 0.000 abstract description 9
- 229920001661 Chitosan Polymers 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 7
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012855 volatile organic compound Substances 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000000356 contaminant Substances 0.000 abstract description 2
- 208000017983 photosensitivity disease Diseases 0.000 abstract description 2
- 231100000434 photosensitization Toxicity 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 208000028571 Occupational disease Diseases 0.000 description 2
- 239000002156 adsorbate Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 241000238557 Decapoda Species 0.000 description 1
- NGWKGSCSHDHHAJ-YPFQVHCOSA-N Liquoric acid Chemical compound C1C[C@H](O)C(C)(C)C2CC[C@@]3(C)[C@]4(C)C[C@H]5O[C@@H]([C@](C6)(C)C(O)=O)C[C@@]5(C)[C@@H]6C4=CC(=O)C3[C@]21C NGWKGSCSHDHHAJ-YPFQVHCOSA-N 0.000 description 1
- NGWKGSCSHDHHAJ-UHFFFAOYSA-N Liquoric acid Natural products C1CC(O)C(C)(C)C2CCC3(C)C4(C)CC5OC(C(C6)(C)C(O)=O)CC5(C)C6C4=CC(=O)C3C21C NGWKGSCSHDHHAJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 229910001872 inorganic gas Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
-
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- 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
-
- 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
-
- 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
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Dispersion Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of photocatalytic activity adsorbent, belong to technical field of adsorption material preparation.The present invention uses the charing matrix of nano-cellulose as the sorbing material of degradation of indoor air VOCs, by it and during nano-titanium dioxide mixes, synergistic effect and photosensitization will occurs in it between titania molecule, nano-titanium dioxide can form film in charcoal-aero gel hole in the present invention, charcoal-aero gel can make the volatile organic contaminant fast enriching of low concentration, be conducive to increase charcoal-aero gel under low consistency conditions to the enrichment area of organic pollution, to accelerate catalysis reaction, so that titanium dioxide shows stronger catalytic activity under visible light, titanium dioxide, the coordinating effect generated between charcoal-aero gel and chitosan molecule improves the photocatalytic activity of film, keep titanium dioxide more sensitive to organic gas volatile matter, organic pollution catalytic degradation concentration can be reduced, it has a extensive future.
Description
Technical field
The invention discloses a kind of preparation methods of photocatalytic activity adsorbent, belong to sorbing material technology of preparing neck
Domain.
Background technology
Adsorbent is also referred to as absorbent.This substance can make active constituent be attached to its particle surface, make the micro chemical combination of liquid
Object additive becomes solid compounds, is conducive to implement uniformly to mix.It is one kind can effectively adsorb from gas or liquid
The solid matter of some of which ingredient.With big specific surface, suitable pore structure and surface texture;Have to adsorbate strong
Adsorption capacity;It is not chemically reacted with adsorbate and medium generally;Easily manufactured, regenerating easily;Have fabulous adsorptivity and
Mechanicalness characteristic.
Common adsorbent has to be adsorbed by the various acticarbons and metal of raw material, nonmetal oxide class of carbonaceous
Agent(Such as silica gel, aluminium oxide, molecular sieve, natural clay).Most representative adsorbent is activated carbon, and absorption property is suitable
It is good, but cost is relatively high, once applies the toluene being used in the event of Song Hua River in adsorbed water body.Secondly there are molecular sieve, silicon
Glue, activated aluminum, polymer absorbant and biological adsorption agent etc..
Finishing pollution is referred to as indoor " stealthy killer ", and harmful substance therein is to women, children and the injury of old man
It is more serious.In subcommercial indoor environment, 50~300 kinds of volatile organic compounds can be seen.Newly-decorated house
This interior five classes harmful substance is much exceeded, seriously endangers the life and health of people.In addition, the various occupational diseases in China increase year by year
Add, and the occupational disease number that Long Term Contact chemical products generate occupies prodigious ratio.Some electronics workshops are commonly used
Chemical solvent, chemical solvent, which is evaporate into air, causes environmental pollution.As the development and various countries of world economy are to industry security
The concern of production, people are also constantly deepening the understanding of toxic and harmful gas harmfulness, surround the purification of toxic and harmful gas
Disposition, domestic and international numerous researchers have developed the spirit for daring to exploring, and constantly look for reasonable efficient solution, a system
The measure for showing malicious cleaning harmful gas processing is used in emergency disposal and the purification of daily industrial production waste gas.It is industrial common
Adsorbent include:Activated carbon, activated alumina, silica gel, synthesis zeolite, organic resin adsorbent etc., wherein including
Activated carbon including granular active carbon and activated carbon fibre is widely used because its is cheap and easy to get.But above-mentioned adsorbent
It is easily saturated in the presence of absorption, is easy the shortcomings that airborne dust causes secondary pollution.Therefore, a kind of photocatalytic activity gas absorption is invented
Agent has positive effect to technical field of adsorption material preparation.
Invention content
Present invention mainly solves the technical issues of, in current subcommercial indoor environment, 50~300 can be seen
Volatile organic compounds is planted, the volatile organic content in newly-decorated house is much exceeded, however current adsorbent
Noxious material and the defect of nontoxic small molecule inorganic gas and water can not be decomposed into effective adsorption chamber, provide a kind of light
The preparation method of catalytic activity adsorbent.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of photocatalytic activity adsorbent, it is characterised in that specifically preparation process is:
(1)It takes 200~300g poplars to be put into pulverizer, crushes 1~2h, cross standard screen, obtain wooden powder, weigh 100~
150g wooden powders are placed in Soxhlet extractor, and benzyl carbinol and water are mixed to get benzyl carbinol solution at normal temperatures, then by 300~
400mL benzyl carbinol solution pours into Soxhlet extractor, and extracting obtains thick wood fiber powder after removing extract;
(2)Thick wood fiber powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, obtain mixed liquor, and
The pH of mixed liquor is adjusted with glacial acetic acid solution, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains comprehensive fiber
Element;
(3)With 120~150mL sodium hydroxide solutions, holocellulose, heat-insulation soaking, filtering removal are impregnated under the conditions of certain temperature
Filtrate obtains purifying cellulose, and purifying cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer at ultrasound
Wooden nano-cellulose is made in reason;
(4)50~60mL absolute ethyl alcohols are added in the beaker equipped with 6~8mL ethyl orthosilicates, 10~15min is stirred, by 3~
4mL water is added in beaker, after stirring 10~12min, then hydrochloric acid is added into beaker and adjusts pH value of solution in beaker, stand, obtain
Silicon dioxide gel;
(5)40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and the wooden nano-celluloses of 2~3g, ultrasonic disperse obtain
Cellulose suspension is placed in the conical flask with blender by cellulose suspension, is added into conical flask with dropping funel
18~20mL butyl titanates, while starting blender, stirring 10~15min with the rotating speed of 200~300r/min is mixed
Liquid;
(6)4~5mL acetic acid solutions are added into mixed liquor, 20~30mL silicon dioxide gels stir 1~2h, obtain Nanowire
Element/TiO 2 sol is tieed up, it is still aging, dry colloidal sol is obtained, dry colloidal sol is placed in drying in baking oven, gel piece is obtained, will coagulate
Blob of viscose is put into 30~35min of grinding in mortar, and sieving obtains gel powder;
(7)It takes the shrimp shell of 100~120g clean drieds to be placed in 200~230mL dilute hydrochloric acid to impregnate, obtains pickle liquor, to acidleach
80~90g gel powders, 40~50mL liquor natrii hypochloritis and 70~80mL sodium hydroxide solutions are added in liquid, heat temperature raising is protected
Temperature reaction is placed on drying in supercritical drying drying system, obtains aeroge, aeroge is put into retort, in argon gas atmosphere
It is carbonized, obtains photocatalytic activity adsorbent.
Step(1)The be sieved specification is 200 mesh, and mixed volume ratio is 2 ︰ 1, extracting to benzyl carbinol at normal temperatures with water
Temperature is 80~90 DEG C, and extraction times are 5~10h.
Step(2)Sodium chlorite solution's mass fraction is 20%, and glacial acetic acid solution mass fraction is 98%, is adjusted mixed
The pH for closing liquid is 4~5, and isothermal holding temperature is 75~80 DEG C, and the isothermal holding time is 5~7h.Step(3)The hydroxide
The mass fraction of sodium solution is 20%, and soaking temperature is 90~100 DEG C, and the heat-insulation soaking time is 2~3h, the quality of water slurry
Score be 10~20%, ultrasonic power be 1200~1500W, sonication treatment time be 30~45min, supersonic frequency be 30~
35kHz。
Step(4)The mass fraction of the hydrochloric acid is 15%, and it is 1.8~2.2 to adjust pH value of solution in beaker, time of repose
For 3~4h.
Step(5)The control ultrasonic power is 150~200W, and the ultrasonic disperse time is 4~6min, dropping funel drop
Rate of acceleration is 2~3mL/min.
Step(6)The mass fraction of the acetic acid solution is 20%, and the still aging time is 2~3 days, baking oven setting temperature
Degree is 60~70 DEG C, and drying time is 10~12h, and be sieved specification is sieved for 200 mesh.
Step(7)The mass fraction of the dilute hydrochloric acid is 5%, and soaking time is 2~3h, the quality of liquor natrii hypochloritis
Score is 2%, and the mass fraction of sodium hydroxide solution is 40%, and temperature is 50~55 DEG C after heat temperature raising, and the insulation reaction time is
40~50min, drying temperature be 70~80 DEG C, drying time be 20~for 24 hours, control carbonization temperature be 300~350 DEG C, charing
Time is 20~25min.
The beneficial effects of the invention are as follows:
(1)The present invention obtains wooden powder after pulverizing and sieving, wooden powder is placed in Soxhlet extractor using poplar as raw material,
Using benzyl carbinol solution as solvent extraction, thick wood fiber powder is obtained, by thick wood fiber powder with sodium chlorite solution, at glacial acetic acid solution
It manages, removes lignin under heating condition, obtain holocellulose, by holocellulose sodium hydroxide solution heat-insulation soaking, filtering point
From purifying cellulose is obtained, purifying cellulose is configured to water slurry, is ultrasonically treated, wooden nano-cellulose is made, it will just
Silester is mixed with absolute ethyl alcohol, and dilute hydrochloric acid acidification hydrolization is added to obtain silicon dioxide gel, by absolute ethyl alcohol and nanofiber
Element mixing, nano-cellulose suspension is obtained through ultrasonic disperse, and nano-cellulose suspension is added in tetraethyl titanate, and stirring is mixed
Conjunction obtains mixed liquor, and acetic acid, silicon dioxide gel are added dropwise into mixed liquor, stirs to get nano-cellulose/TiO 2 sol,
Titania gel powder is obtained by still aging, dry, grinding, it is solidifying by acidleach, incorporation using discarded shrimp shell as raw material
Rubber powder simultaneously obtains photocatalytic activity gas absorption with being dried to obtain aeroge after lye acetylation, then by aeroge charing process
Agent, the present invention uses the charing matrix of nano-cellulose as the sorbing material of degradation of indoor air VOCs, due to Nanowire
The charcoal-aero gel formed after dimension element charing has high-specific surface area, has very to gas trace heavy metal element and certain organic matters
Strong adsorption capacity, by it and during nano-titanium dioxide mixes, synergistic effect will occurs in it between titania molecule
And photosensitization, the photocatalytic activity of nano-titanium dioxide film can be improved, receptor of the nano-cellulose as electronics is easy
The light induced electron that titanium dioxide generates is received, to effectively inhibit compound, the raising photocatalysis efficiency of light induced electron and hole;
(2)Nano-titanium dioxide can form film in charcoal-aero gel hole in the present invention, and charcoal-aero gel can make low concentration
Volatile organic contaminant fast enriching, the organic pollution concentration on degradation nano-titanium dioxide film surface improves to room
The pickle liquor of interior photocatalytic oxidation efficiency, shrimp shell obtains chitosan, the formation of titanium deoxid film by alkalization is deacetylated
Using chitosan as carrier, and chitosan serves among composite film material is dispersed in the matrix of chitosan by crosslinking agent, has
It is catalyzed the structure of film layer formation rule conducive to composite material, makes in charcoal-aero gel hole that membrane structure is more regular, is conducive to increase
Big charcoal-aero gel, to the enrichment area of organic pollution, reacts, in addition, charcoal-aero gel under low consistency conditions to accelerate catalysis
Titanium dioxide forbidden band energy gap narrows after being doped in composite film material, generates red shift, nano-titanium dioxide film is allow to absorb
The light of more long wavelength, so that titanium dioxide shows stronger catalytic activity under visible light, chitosan is mixed as crosslinking agent
Enter in composite film material, although the specific surface area of film is caused to reduce, product is produced to the photocatalytic activity of catalyst
The influence of pole, the coordinating effect generated between titanium dioxide, charcoal-aero gel and chitosan molecule improve the photocatalytic activity of film,
Keep titanium dioxide more sensitive to organic gas volatile matter, organic pollution catalytic degradation concentration can be reduced, application prospect is wide
It is wealthy.
Specific implementation mode
It takes 200~300g poplars to be put into pulverizer, crushes 1~2h, cross 200 mesh standard sieves, obtain wooden powder, weigh
100~150g wooden powders are placed in Soxhlet extractor, are that 2 ︰ 1 are mixed to get benzene by volume at normal temperatures by benzyl carbinol and water
Ethanol solution, then 300~400mL benzyl carbinol solution is poured into Soxhlet extractor, 5~10h, removing are extracted at 80~90 DEG C
After extract, thick wood fiber powder is obtained;Thick wood fiber powder is put into beaker, 50~60mL mass fractions are added into beaker is
20% sodium chlorite solution, obtains mixed liquor, be used in combination mass fraction be 98% glacial acetic acid solution adjust mixed liquor pH to 4~
5,5~7h of isothermal holding under the conditions of 75~80 DEG C, repeat aforesaid operations 3~5 times, remove lignin, obtain holocellulose;With
The sodium hydroxide solution that 120~150mL mass fractions are 20%, impregnates holocellulose, heat-insulation soaking 2 under the conditions of 90~100 DEG C
~3h, filtering removal filtrate obtain purifying cellulose, purifying cellulose are made into the water slurry that mass fraction is 10~20%,
It is placed in ultrasonic wave plant cell pulverizer the power ultrasonic with 1200~1500W and handles 30~45min, control supersonic frequency is
Wooden nano-cellulose is made in 30~35kHz;The beaker equipped with 6~8mL ethyl orthosilicates is added in 50~60mL absolute ethyl alcohols
In, 10~15min is stirred, 3~4mL water is added in beaker, after stirring 10~12min, then mass fraction is added into beaker
It is 1.8~2.2 for pH value of solution in 15% hydrochloric acid adjusting beaker, stands 3~4h, obtain silicon dioxide gel;To ultrasonic disperse instrument
Middle addition 40~50mL absolute ethyl alcohols and the wooden nano-celluloses of 2~3g, control ultrasonic power are 150~200W, ultrasonic disperse 4
~6min, obtains cellulose suspension, and cellulose suspension is placed in the conical flask with blender, with dropping funel with 2
18~20mL butyl titanates are added into conical flask for the drop rate of~3mL/min, while starting blender, with 200~
The rotating speed of 300r/min starts 10~15min of stirring and obtains mixed liquor;It is 20% that 4~5mL mass fractions are added into mixed liquor
Acetic acid solution, 20~30mL silicon dioxide gels stir 1~2h, obtain nano-cellulose/TiO 2 sol, and still aging 2
~3 days, dry colloidal sol is obtained, dry colloidal sol is placed in the baking oven that set temperature is 60~70 DEG C, dry 10~12h obtains gel
Gel piece is put into 30~35min of grinding in mortar, crosses 200 mesh and sieve to obtain gel powder by block;Take 100~120g clean drieds
Shrimp shell, which is placed in the dilute hydrochloric acid that 200~230mL mass fractions are 5%, impregnates 2~3h, obtains pickle liquor, 80 are added into pickle liquor
The hydrogen-oxygen that the liquor natrii hypochloritis and 70~80mL mass fractions that~90g gel powders, 40~50mL mass fractions are 2% are 40%
Change sodium solution, is heated to 50~55 DEG C, 40~50min of insulation reaction is placed in supercritical drying drying system, 70~80
Dry 20 under the conditions of DEG C~for 24 hours, aeroge is obtained, aeroge is put into retort, is carbonized in argon gas atmosphere, is controlled
Carbonization temperature is 300~350 DEG C, and carbonization time is 20~25min, obtains photocatalytic activity adsorbent.
Example 1
It takes 200g poplars to be put into pulverizer, crushes 1h, cross 200 mesh standard sieves, obtain wooden powder, weigh 100g wooden powders
It is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will
300mL benzyl carbinol solution pours into Soxhlet extractor, and 5h is extracted at 80 DEG C, after removing extract, obtains thick wood fiber powder;It will
Thick wood fiber powder is put into beaker, and the sodium chlorite solution that 50mL mass fractions are 20% is added into beaker, obtains mixed liquor,
It is used in combination the glacial acetic acid solution that mass fraction is 98% to adjust pH to 4, isothermal holding 5h under the conditions of 75 DEG C of mixed liquor, in repetition
Operation 3 times is stated, lignin is removed, obtains holocellulose;The sodium hydroxide solution for being 20% with 120mL mass fractions, in 90 DEG C of items
Holocellulose, heat-insulation soaking 2h are impregnated under part, filtering removal filtrate obtains purifying cellulose, purifying cellulose is made into quality point
Number is 10% water slurry, is placed in ultrasonic wave plant cell pulverizer the power ultrasonic processing 30min with 1200W, and control is super
Acoustic frequency is 30kHz, and wooden nano-cellulose is made;50mL absolute ethyl alcohols are added in the beaker equipped with 6mL ethyl orthosilicates,
10min is stirred, 3mL water is added in beaker, after stirring 10min, then the hydrochloric acid that mass fraction is 15% is added into beaker and adjusts
PH value of solution is 1.8 in beaker, stands 3h, obtains silicon dioxide gel;40mL absolute ethyl alcohols and 2g are added into ultrasonic disperse instrument
Wooden nano-cellulose, control ultrasonic power are 150W, and ultrasonic disperse 4min obtains cellulose suspension, cellulose is suspended
Liquid is placed in the conical flask with blender, and 18mL titaniums are added into conical flask with the drop rate of 2mL/min with dropping funel
Sour four butyl esters, while starting blender, starting stirring 10min with the rotating speed of 200r/min obtains mixed liquor;Add into mixed liquor
Enter the acetic acid solution that 4mL mass fractions are 20%, 20mL silicon dioxide gels stir 1h, obtain nano-cellulose/titanium dioxide
Colloidal sol still aging 2 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 60 DEG C, and dry 10h is coagulated
Gel piece is put into mortar and grinds 30min by blob of viscose, crosses 200 mesh and sieves to obtain gel powder;The shrimp shell of 100g clean drieds is taken to be placed in
2h is impregnated in the dilute hydrochloric acid that 200mL mass fractions are 5%, obtains pickle liquor, 80g gel powders, 40mL mass are added into pickle liquor
The sodium hydroxide solution that the liquor natrii hypochloritis and 70mL mass fractions that score is 2% are 40% is heated to 50 DEG C, heat preservation
Reaction 40min is placed in supercritical drying drying system, and dry 20h, obtains aeroge, aeroge is put into charcoal under the conditions of 70 DEG C
Change in stove, carbonized in argon gas atmosphere, control carbonization temperature is 300 DEG C, carbonization time 20min, obtains photocatalysis work
Property adsorbent.
Example 2
It takes 250g poplars to be put into pulverizer, crushes 1.5h, cross 200 mesh standard sieves, obtain wooden powder, weigh 120g wood powders
End is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will
350mL benzyl carbinol solution pours into Soxhlet extractor, and 7h is extracted at 85 DEG C, after removing extract, obtains thick wood fiber powder;It will
Thick wood fiber powder is put into beaker, and the sodium chlorite solution that 55mL mass fractions are 20% is added into beaker, obtains mixed liquor,
It is used in combination the glacial acetic acid solution that mass fraction is 98% to adjust pH to 4, isothermal holding 6h under the conditions of 77 DEG C of mixed liquor, in repetition
Operation 4 times is stated, lignin is removed, obtains holocellulose;The sodium hydroxide solution for being 20% with 135mL mass fractions, in 95 DEG C of items
Holocellulose, heat-insulation soaking 2.5h are impregnated under part, filtering removal filtrate obtains purifying cellulose, purifying cellulose is made into quality
The water slurry that score is 15% is placed in ultrasonic wave plant cell pulverizer the power ultrasonic processing 40min with 1350W, control
Supersonic frequency is 32kHz, and wooden nano-cellulose is made;The beaker equipped with 7mL ethyl orthosilicates is added in 55mL absolute ethyl alcohols
In, 12min is stirred, 3mL water is added in beaker, after stirring 11min, then the hydrochloric acid that mass fraction is 15% is added into beaker
It is 2.0 to adjust pH value of solution in beaker, stands 3.5h, obtains silicon dioxide gel;The anhydrous second of 45mL is added into ultrasonic disperse instrument
Alcohol and the wooden nano-celluloses of 2g, control ultrasonic power are 170W, and ultrasonic disperse 5min obtains cellulose suspension, by fiber
Plain suspension is placed in the conical flask with blender, is added into conical flask with the drop rate of 2mL/min with dropping funel
19mL butyl titanates, while starting blender, starting stirring 12min with the rotating speed of 250r/min obtains mixed liquor;To mixing
In liquid be added 4mL mass fractions be 20% acetic acid solution, 25mL silicon dioxide gels, stir 1.5h, obtain nano-cellulose/
TiO 2 sol still aging 2 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 65 DEG C, dry
11h obtains gel piece, and gel piece is put into mortar and grinds 32min, crosses 200 mesh and sieves to obtain gel powder;Take 110g clean drieds
Shrimp shell be placed in the dilute hydrochloric acid that 215mL mass fractions are 5% and impregnate 2.5h, obtain pickle liquor, it is solidifying that 85g be added into pickle liquor
The sodium hydroxide solution that the liquor natrii hypochloritis and 75mL mass fractions that rubber powder, 45mL mass fractions are 2% are 40%, heating rise
To 52 DEG C, insulation reaction 45min is placed in supercritical drying drying system temperature, and dry 22h, obtains aeroge under the conditions of 75 DEG C,
Aeroge is put into retort, is carbonized in argon gas atmosphere, control carbonization temperature is 320 DEG C, and carbonization time is
22min obtains photocatalytic activity adsorbent.
Example 3
It takes 300g poplars to be put into pulverizer, crushes 2h, cross 200 mesh standard sieves, obtain wooden powder, weigh 150g wooden powders
It is placed in Soxhlet extractor, benzyl carbinol and water is mixed to get benzyl carbinol solution for 2 ︰ 1 by volume at normal temperatures, then will
400mL benzyl carbinol solution pours into Soxhlet extractor, and 10h is extracted at 90 DEG C, after removing extract, obtains thick wood fiber powder;
Thick wood fiber powder is put into beaker, the sodium chlorite solution that 60mL mass fractions are 20% is added into beaker, is mixed
Liquid is used in combination the glacial acetic acid solution that mass fraction is 98% to adjust pH to 5, isothermal holding 7h under the conditions of 80 DEG C of mixed liquor, is repeated
Aforesaid operations 5 times remove lignin, obtain holocellulose;The sodium hydroxide solution for being 20% with 150mL mass fractions, 100
Holocellulose, heat-insulation soaking 3h are impregnated under the conditions of DEG C, filtering removal filtrate obtains purifying cellulose, purifying cellulose is made into matter
The water slurry that score is 20% is measured, the power ultrasonic processing 45min with 1500W, control are placed in ultrasonic wave plant cell pulverizer
Supersonic frequency processed is 35kHz, and wooden nano-cellulose is made;The burning equipped with 8mL ethyl orthosilicates is added in 60mL absolute ethyl alcohols
In cup, 15min is stirred, 4mL water is added in beaker, after stirring 12min, then the salt that mass fraction is 15% is added into beaker
It is 2.2 that acid, which adjusts pH value of solution in beaker, stands 4h, obtains silicon dioxide gel;The anhydrous second of 50mL is added into ultrasonic disperse instrument
Alcohol and the wooden nano-celluloses of 3g, control ultrasonic power are 200W, and ultrasonic disperse 6min obtains cellulose suspension, by fiber
Plain suspension is placed in the conical flask with blender, is added into conical flask with the drop rate of 3mL/min with dropping funel
20mL butyl titanates, while starting blender, starting stirring 15min with the rotating speed of 300r/min obtains mixed liquor;To mixing
The acetic acid solution that 5mL mass fractions are 20% is added in liquid, 30mL silicon dioxide gels stir 2h, obtain nano-cellulose/bis-
Titanium oxide sol still aging 3 days, obtains dry colloidal sol, dry colloidal sol is placed in the baking oven that set temperature is 70 DEG C, dry 12h,
Gel piece is obtained, gel piece is put into mortar and grinds 35min, 200 mesh is crossed and sieves to obtain gel powder;Take the shrimp of 120g clean drieds
Shell, which is placed in the dilute hydrochloric acid that 230mL mass fractions are 5%, impregnates 3h, obtains pickle liquor, be added into pickle liquor 90g gel powders,
The sodium hydroxide solution that the liquor natrii hypochloritis and 80mL mass fractions that 50mL mass fractions are 2% are 40%, is heated to 55
DEG C, insulation reaction 50min is placed in supercritical drying drying system, is dried for 24 hours under the conditions of 80 DEG C, aeroge is obtained, by airsetting
Glue is put into retort, is carbonized in argon gas atmosphere, and control carbonization temperature is 350 DEG C, and carbonization time 25min is obtained
Photocatalytic activity adsorbent.
Comparative example
With the photocatalytic activity adsorbent of Changzhou company production as a comparison case to photocatalytic activity produced by the present invention
Photocatalytic activity adsorbent in adsorbent and comparative example carries out performance detection
Test method:
Formaldehyde removal rate is tested:It takes the adsorbent 25g in example 1~3 and comparative example to be put into dry bag, is used in combination clip close
After bag mouth sealing, any corner indoors is placed, wherein every square metre is placed 3 dry bags that adsorbent is housed, 10h is placed, surveys
Formaldehyde after content of formaldehyde and 10h before 10h;
Saturated extent of adsorption test is detected by GB/T 19587-2004 standards;
Photocatalysis efficiency is tested:Adsorbent in example 1~3 and comparative example is put into dry bag, clip is used in combination to seal
After sack, any corner indoors is placed, by measuring its photocatalytic of the Assessment of Changes of degradation speed of formaldehyde under fluorescent lamp
Energy.
Photocatalytic activity adsorbent produced by the present invention is good for the formaldehyde absorbing effect in room air, removal rate
It is relatively high, and there is no any harm for human body and environment, degradation rate is high, and photocatalysis effect is good, has broad application prospects.
Claims (8)
1. a kind of preparation method of photocatalytic activity adsorbent, it is characterised in that specifically preparation process is:
(1)It takes 200~300g poplars to be put into pulverizer, crushes 1~2h, cross standard screen, obtain wooden powder, weigh 100~
150g wooden powders are placed in Soxhlet extractor, and benzyl carbinol and water are mixed to get benzyl carbinol solution at normal temperatures, then by 300~
400mL benzyl carbinol solution pours into Soxhlet extractor, and extracting obtains thick wood fiber powder after removing extract;
(2)Thick wood fiber powder is put into beaker, 50~60mL sodium chlorite solutions are added into beaker, obtain mixed liquor, and
The pH of mixed liquor is adjusted with glacial acetic acid solution, isothermal holding repeats aforesaid operations 3~5 times, removes lignin, obtains comprehensive fiber
Element;
(3)With 120~150mL sodium hydroxide solutions, holocellulose, heat-insulation soaking, filtering removal are impregnated under the conditions of certain temperature
Filtrate obtains purifying cellulose, and purifying cellulose is made into water slurry, is placed in ultrasonic wave plant cell pulverizer at ultrasound
Wooden nano-cellulose is made in reason;
(4)50~60mL absolute ethyl alcohols are added in the beaker equipped with 6~8mL ethyl orthosilicates, 10~15min is stirred, by 3~
4mL water is added in beaker, after stirring 10~12min, then hydrochloric acid is added into beaker and adjusts pH value of solution in beaker, stand, obtain
Silicon dioxide gel;
(5)40~50mL absolute ethyl alcohols are added into ultrasonic disperse instrument and the wooden nano-celluloses of 2~3g, ultrasonic disperse obtain
Cellulose suspension is placed in the conical flask with blender by cellulose suspension, is added into conical flask with dropping funel
18~20mL butyl titanates, while starting blender, stirring 10~15min with the rotating speed of 200~300r/min is mixed
Liquid;
(6)4~5mL acetic acid solutions are added into mixed liquor, 20~30mL silicon dioxide gels stir 1~2h, obtain Nanowire
Element/TiO 2 sol is tieed up, it is still aging, dry colloidal sol is obtained, dry colloidal sol is placed in drying in baking oven, gel piece is obtained, will coagulate
Blob of viscose is put into 30~35min of grinding in mortar, and sieving obtains gel powder;
(7)It takes the shrimp shell of 100~120g clean drieds to be placed in 200~230mL dilute hydrochloric acid to impregnate, obtains pickle liquor, to acidleach
80~90g gel powders, 40~50mL liquor natrii hypochloritis and 70~80mL sodium hydroxide solutions are added in liquid, heat temperature raising is protected
Temperature reaction is placed on drying in supercritical drying drying system, obtains aeroge, aeroge is put into retort, in argon gas atmosphere
It is carbonized, obtains photocatalytic activity adsorbent.
2. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step
(1)The be sieved specification is 200 mesh, and mixed volume ratio is 2 ︰ 1 to benzyl carbinol at normal temperatures with water, and extraction temperature is 80~90
DEG C, extraction times are 5~10h.
3. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step
(2)Sodium chlorite solution's mass fraction is 20%, and glacial acetic acid solution mass fraction is 98%, and the pH for adjusting mixed liquor is 4
~5, isothermal holding temperature is 75~80 DEG C, and the isothermal holding time is 5~7h.
4. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step
(3)The mass fraction of the sodium hydroxide solution is 20%, and soaking temperature is 90~100 DEG C, and the heat-insulation soaking time is 2~3h,
The mass fraction of water slurry is 10~20%, and ultrasonic power is 1200~1500W, and sonication treatment time is 30~45min, is surpassed
Acoustic frequency is 30~35kHz.
5. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step
(4)The mass fraction of the hydrochloric acid is 15%, and it is 1.8~2.2 to adjust pH value of solution in beaker, and time of repose is 3~4h.
6. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step
(5)The control ultrasonic power be 150~200W, the ultrasonic disperse time be 4~6min, dropping funel drop rate be 2~
3mL/min。
7. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step
(6)The mass fraction of the acetic acid solution is 20%, and the still aging time is 2~3 days, and baking oven set temperature is 60~70 DEG C,
Drying time is 10~12h, and be sieved specification is sieved for 200 mesh.
8. a kind of preparation method of photocatalytic activity adsorbent according to claim 1, it is characterised in that:Step
(7)The mass fraction of the dilute hydrochloric acid is 5%, and soaking time is 2~3h, and the mass fraction of liquor natrii hypochloritis is 2%, hydrogen-oxygen
The mass fraction for changing sodium solution is 40%, and temperature is 50~55 DEG C after heat temperature raising, and the insulation reaction time is 40~50min, is done
Dry temperature be 70~80 DEG C, drying time be 20~for 24 hours, control carbonization temperature be 300~350 DEG C, carbonization time be 20~
25min。
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