CN104549145A - Titanium dioxide/lignocellulose-based active carbon composite material and preparation method thereof - Google Patents
Titanium dioxide/lignocellulose-based active carbon composite material and preparation method thereof Download PDFInfo
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- CN104549145A CN104549145A CN201410717352.9A CN201410717352A CN104549145A CN 104549145 A CN104549145 A CN 104549145A CN 201410717352 A CN201410717352 A CN 201410717352A CN 104549145 A CN104549145 A CN 104549145A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 70
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 title abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000007935 neutral effect Effects 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001179 sorption measurement Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 45
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- 239000011159 matrix material Substances 0.000 claims description 23
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 16
- 229920002522 Wood fibre Polymers 0.000 claims description 15
- 229920002678 cellulose Polymers 0.000 claims description 15
- 239000001913 cellulose Substances 0.000 claims description 15
- 230000003647 oxidation Effects 0.000 claims description 15
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000001994 activation Methods 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 9
- 239000002250 absorbent Substances 0.000 claims description 8
- 230000002745 absorbent Effects 0.000 claims description 8
- 239000003610 charcoal Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 6
- 239000007864 aqueous solution Substances 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
- 238000001354 calcination Methods 0.000 claims description 6
- 235000013399 edible fruits Nutrition 0.000 claims description 6
- 230000008030 elimination Effects 0.000 claims description 6
- 238000003379 elimination reaction Methods 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 239000012978 lignocellulosic material Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000000247 postprecipitation Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 4
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 238000002386 leaching Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 2
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 claims description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract 3
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- B01J20/02—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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- 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
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a titanium dioxide/lignocellulose-based active carbon composite material and a preparation method thereof. The method comprises the following steps of firstly, preparing faint yellow transparent TiO2 sol by using tetrabutyl titanate, then, dissolving tetrabutyl titanate into a prepared lignocellulose solution, sufficiently reacting tetrabutyl titanate, filtering a liquid on the upper layer after ending the reaction and settling, then, standing in the air for 12-36 hours, next, respectively and alternately washing and filtering by using distilled water and absolute ethyl alcohol until the filtrate is neutral, and drying a product in a vacuum drying oven to prepare a titanium dioxide/lignocellulose composite material; and then, pre-oxidizing, carbonizing and activating the composite material to prepare the titanium dioxide/lignocellulose-based active carbon composite material with efficient adsorption and catalysis performance. The preparation method disclosed by the invention is simple in process; and the obtained titanium dioxide/lignocellulose-based active carbon composite material has relatively-strong adsorption performance and relatively-good photocatalytic degradation performance and has the advantage of catalyzing organic pollutants in wastewater or air.
Description
Technical field
The present invention relates to a kind of titanium dioxide/lignocellulosic matrix activated carbon composite and preparation method thereof, belong to absorbent charcoal composite material technology of preparing.
Background technology
The process of traditional dyeing and finishing method of wastewater treatment is not ideal, and mainly because Wastewater Dyes molecular structure stabilized, complicated component, percent of decolourization, COD clearance are not high, easily produce secondary pollution.Utilize the photocatalysis performance of semi-conducting material just the organic matter that many chemical methods and bioanalysis cannot be removed can be decomposed into carbon dioxide and water completely at ambient temperature, and not causing secondary pollution, the ultraviolet light contained in its available sunshine and fluorescent lamp makes excitaton source.Current, for degrading in the catalyst of environmental contaminants, titanium dioxide relies on the features such as high, the indissoluble of its photocatalytic activity, nontoxic and cost are low to become most one of photochemical catalyst with application prospect, and has purifying air, kill bacterium, the effects such as degraded hardly degraded organic substance.But traditional nano-TiO
2suspended phase photochemical catalyst easy in inactivation, easily cohesion, the difficult shortcoming reclaimed, therefore find one and have comparatively bigger serface, again with TiO
2the high-efficient carrier material of strong bonded is the key of practical technology.Absorbent charcoal material, as a kind of desirable sorbing material, is grow up on the basis that Carbon fibe technology and activated carbon technology combine.Active carbon has larger pore capacities and specific area, and based on micropore, therefore, is conducive to adsorbate and diffuses in hand-hole and active surface, and active carbon demonstrates higher adsorption capacity and adsorption/desorption speed faster.This active carbon is utilized effectively to adsorb and to remove the dyestuff, slurry, auxiliary agent, finish, soda acid, fiber impurity, inorganic salts etc. in sewage.
Be difficult to efficient removal for organic pollutant molecule in dyeing and printing sewage advanced treatment process and cause the problems such as recycling water utilization rate is low, in the urgent need to proposing or set up principle and the method for new and effective selective pollution abatement thing.Reaction platform based on nano material and Assembling of Nanoparticles, the interface of the special microenvironment of one class can be provided, by the interfacial interaction with organic pollutant molecule, under light action, trigger the special catalysis of this nano material or conversion effet, this kind of organic pollution is removed on safety, efficient selective ground.Fundamentally solve traditional treatment method for a long time under a large amount of concurrent conditions of general organic/inorganic thing cannot selective removal low concentration, high toxicity, persistent organic pollutants a difficult problem.
Summary of the invention
The present invention is in order to overcome above-mentioned the deficiencies in the prior art, and object there is provided a kind of titanium dioxide/lignocellulosic matrix activated carbon composite and preparation method thereof, and obtained composite has stronger absorption property and good Photocatalytic Degradation Property in this way.
To achieve these goals, the technical solution used in the present invention is:
A preparation method for titanium dioxide/lignocellulosic matrix activated carbon composite, is characterized in that: first butyl titanate is made faint yellow Ti0 by the method
2vitreosol, then added in the wood fibre cellulose solution for preparing, make it fully react, reaction terminate and precipitation after after leaching supernatant liquid, then be placed in air and place 12 ~ 36h, then replace washing and filtering with distilled water, absolute ethyl alcohol respectively, until filtrate is in neutral; Resulting product is placed in vacuum drying oven dry 4 ~ 8h under 50 ~ 80 DEG C of conditions, obtained titanium dioxide/lignocellulose composites; Again by titanium dioxide/lignocellulose composites through pre-oxidation, charing and activation process, be prepared into the titanium dioxide/lignocellulosic matrix activated carbon composite with efficient adsorption and catalytic performance; The method comprises the following steps:
1) TiO 2 sol preparation: 15 ~ 30 parts of butyl titanates and 5 ~ 15 parts of glacial acetic acid are dissolved in 50 ~ 80 parts of absolute ethyl alcohols, magnetic agitation 0.5 ~ 2h makes it to mix, in the mixed solution of slow instillation 80 ~ 95 parts of absolute ethyl alcohols and 5 ~ 20 parts of distilled water, control buret and drip speed, sealing stirring obtains faint yellow Ti0
2vitreosol, still aging 2 ~ 4h;
2) wood fibre cellulose solution preparation: be at room temperature dissolved in corresponding solvent by lignocellulosic, being mixed with volume mass mark (g/L) is the solution of 2 ~ 20%, and magnetic agitation is transparent to solution;
3) titanium dioxide/lignocellulose composites preparation: by step 1) TiO 2 sol and the step 2 that obtain) the wood fibre cellulose solution that obtains mixes according to the mass ratio 0.01: 1 ~ 0.5: 1 of solute, be stirred to and mix completely, reaction terminates postprecipitation, elimination supernatant liquid again, then be placed in air and place 12 ~ 36h, respectively with distilled water, absolute ethyl alcohol alternately washing, suction filtration, to filtrate in neutral, finally be placed in vacuum drying oven dry 4 ~ 8h under 50 ~ 80 DEG C of conditions, obtained titanium dioxide/lignocellulose composites;
4) absorbent charcoal composite material preparation: by step 3) obtained titanium dioxide/lignocellulose composites through pre-oxidation, charing and activation process, be prepared into titanium dioxide/lignocellulosic matrix activated carbon composite.
Described ligno-cellulosic materials is Powdered finished product obtained after utilizing plant raw material to process, and plant raw material comprise the stalk of all kinds of perennial and draft class plant, branch, leaf, skin and fruit shell.
Described step 2) lignocellulosic solvent used is one or more mixed solvent systems in dimethyl sulfoxide (DMSO), dimethyl formamide, dimethylacetylamide, N-methylmorpholine-N-oxide, etamon chloride solution, ammonium thiocyanate solution, triethanolamine, ammonia spirit, alkaline aqueous solution.
Described alkaline aqueous solution is alkali metal hydroxide aqueous solution, is specially NaOH, potassium hydroxide.
Described Pre oxidation controls at 50 ~ 350 DEG C; Activate the H at 5 ~ 20wt%
3pO
4carry out in the KOH solution of solution and 5 ~ 20wt%; Charing, in tubular type Muffle furnace, is carried out in atmosphere of inert gases, and temperature controls 400 ~ 600 DEG C of calcination.
Described inert gas is N
2.
The present invention also comprises the titanium dioxide/lignocellulosic matrix activated carbon composite utilizing above-mentioned method to prepare.
Preparation method's process of the present invention is simple, obtain titanium dioxide/lignocellulosic matrix activated carbon composite there is stronger absorption property and good Photocatalytic Degradation Property.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
The invention provides a kind of titanium dioxide/lignocellulosic matrix activated carbon composite and preparation method thereof, first butyl titanate is made faint yellow Ti0 by the method
2vitreosol, then added in the wood fibre cellulose solution for preparing, make it fully react, reaction terminate and precipitation after after leaching supernatant liquid, then be placed in air and place 12 ~ 36h, then replace washing and filtering with distilled water, absolute ethyl alcohol respectively, until filtrate is in neutral; Resulting product is placed in vacuum drying oven dry 4 ~ 8h under 50 ~ 80 DEG C of conditions, obtained titanium dioxide/lignocellulose composites; Again by titanium dioxide/lignocellulose composites through pre-oxidation, charing and activation process, be prepared into the titanium dioxide/lignocellulosic matrix activated carbon composite with efficient adsorption and catalytic performance; Preparation method's process of the present invention is simple, obtain titanium dioxide/cellulosic activity carbon composite there is stronger absorption property and good Photocatalytic Degradation Property.
Embodiment 1:
A kind of titanium dioxide/cellulosic activity carbon composite and preparation method thereof, it comprises the steps:
1) TiO 2 sol preparation: 15 parts of butyl titanates and 5 parts of glacial acetic acid are dissolved in 50 parts of absolute ethyl alcohols, magnetic agitation 0.5h makes it to mix, in the mixed solution of slow instillation 80 parts of absolute ethyl alcohols and 5 parts of distilled water, control buret and drip speed, sealing stirring obtains faint yellow Ti0
2vitreosol, still aging 2h;
2) wood fibre cellulose solution preparation: be at room temperature dissolved in dimethyl sulfoxide (DMSO) by lignocellulosic, being mixed with volume mass mark (g/L) is the solution of 2%, and magnetic agitation is transparent to solution; Described ligno-cellulosic materials is Powdered finished product obtained after utilizing plant raw material to process, and plant raw material comprise the stalk of all kinds of perennial and draft class plant, branch, leaf, skin and fruit shell;
3) titanium dioxide/lignocellulose composites preparation: by step 1) obtained TiO 2 sol and step 2) the wood fibre cellulose solution that obtains mixes according to the mass ratio 0.01: 1 of solute, be stirred to and mix completely, reaction terminates postprecipitation, elimination supernatant liquid again, then be placed in air and place 24h, respectively with distilled water, absolute ethyl alcohol alternately washing, suction filtration, to filtrate in neutral, finally be placed in vacuum drying oven dry 4h under 50 DEG C of conditions, obtained composite;
4) absorbent charcoal composite material preparation: by step 3) obtained lignocellulosic based composites is through pre-oxidation, charing and activation process, and Pre oxidation is 150 DEG C, at the H of 5wt%
3pO
4activate in the KOH solution of solution and 5wt%; In tubular type Muffle furnace, inert gas N
2carbonize in atmosphere, temperature controls 450 DEG C of calcination, is finally prepared into titanium dioxide/lignocellulosic matrix activated carbon composite.
Embodiment 2:
A kind of titanium dioxide/cellulosic activity carbon composite and preparation method thereof, it comprises the steps:
1) TiO 2 sol preparation: 20 parts of butyl titanates and 10 parts of glacial acetic acid are dissolved in 60 parts of absolute ethyl alcohols, magnetic agitation 1h makes it to mix, in the mixed solution of slow instillation 85 parts of absolute ethyl alcohols and 10 parts of distilled water, control buret and drip speed, sealing stirring obtains faint yellow Ti0
2vitreosol, still aging 3h;
2) wood fibre cellulose solution preparation: be at room temperature dissolved in dimethyl formamide by lignocellulosic, being mixed with volume mass mark (g/L) is the solution of 8%, and magnetic agitation is transparent to solution; Described ligno-cellulosic materials is Powdered finished product obtained after utilizing plant raw material to process, and plant raw material comprise the stalk of all kinds of perennial and draft class plant, branch, leaf, skin and fruit shell;
3) titanium dioxide/lignocellulose composites preparation: by step 1) obtained TiO 2 sol and step 2) the wood fibre cellulose solution that obtains mixes according to the mass ratio 0.1: 1 of solute, be stirred to and mix completely, reaction terminates postprecipitation, elimination supernatant liquid again, then be placed in air and place 24h, respectively with distilled water, absolute ethyl alcohol alternately washing, suction filtration, to filtrate in neutral, finally be placed in vacuum drying oven dry 5h under 60 DEG C of conditions, obtained composite;
4) absorbent charcoal composite material preparation: by step 3) obtained lignocellulosic based composites is through pre-oxidation, charing and activation process, and Pre oxidation is 180 DEG C, at the H of 10wt%
3pO
4activate in the KOH solution of solution and 10wt%; In tubular type Muffle furnace, inert gas N
2carbonize in atmosphere, temperature controls 450 DEG C of calcination, is finally prepared into titanium dioxide/lignocellulosic matrix activated carbon composite.
Embodiment 3:
A kind of titanium dioxide/cellulosic activity carbon composite and preparation method thereof, it comprises the steps:
1) TiO 2 sol preparation: 25 parts of butyl titanates and 15 parts of glacial acetic acid are dissolved in 70 parts of absolute ethyl alcohols, magnetic agitation 1.5h makes it to mix, in the mixed solution of slow instillation 90 parts of absolute ethyl alcohols and 15 parts of distilled water, control buret and drip speed, sealing stirring obtains faint yellow Ti0
2vitreosol, still aging 3h;
2) wood fibre cellulose solution preparation: be at room temperature dissolved in by lignocellulosic in N-methylmorpholine-N-oxide, being mixed with volume mass mark (g/L) is the solution of 15%, and magnetic agitation is transparent to solution; Described ligno-cellulosic materials is Powdered finished product obtained after utilizing plant raw material to process, and plant raw material comprise the stalk of all kinds of perennial and draft class plant, branch, leaf, skin and fruit shell;
3) titanium dioxide/lignocellulose composites preparation: by step 1) obtained TiO 2 sol and step 2) the wood fibre cellulose solution that obtains mixes according to the mass ratio 0.2: 1 of solute, be stirred to and mix completely, reaction terminates postprecipitation, elimination supernatant liquid again, then be placed in air and place 24h, respectively with distilled water, absolute ethyl alcohol alternately washing, suction filtration, to filtrate in neutral, finally be placed in vacuum drying oven dry 7h under 70 DEG C of conditions, obtained composite;
4) absorbent charcoal composite material preparation: by step 3) obtained lignocellulosic based composites is through pre-oxidation, charing and activation process, and Pre oxidation is 200 DEG C, at the H of 15wt%
3pO
4activate in the KOH solution of solution and 15wt%; In tubular type Muffle furnace, inert gas N
2carbonize in atmosphere, temperature controls 500 DEG C of calcination, is finally prepared into titanium dioxide/lignocellulosic matrix activated carbon composite.
Embodiment 4:
A kind of titanium dioxide/cellulosic activity carbon composite and preparation method thereof, it comprises the steps:
1) TiO 2 sol preparation: 30 parts of butyl titanates and 15 parts of glacial acetic acid are dissolved in 80 parts of absolute ethyl alcohols, magnetic agitation 2h makes it to mix, in the mixed solution of slow instillation 95 parts of absolute ethyl alcohols and 20 parts of distilled water, control buret and drip speed, sealing stirring obtains faint yellow Ti0
2vitreosol, still aging 4h;
2) wood fibre cellulose solution preparation: at room temperature lignocellulosic is dissolved in ammonia/ammonium thiocyanate solution (NH
3/ NH
4sCN/H
2o system) in, being mixed with volume mass mark (g/L) is the solution of 20%, and magnetic agitation is transparent to solution; Described ligno-cellulosic materials is Powdered finished product obtained after utilizing plant raw material to process, and plant raw material comprise the stalk of all kinds of perennial and draft class plant, branch, leaf, skin and fruit shell;
3) titanium dioxide/lignocellulose composites preparation: by step 1) obtained TiO 2 sol and step 2) the wood fibre cellulose solution that obtains mixes according to the mass ratio 0.5: 1 of solute, be stirred to and mix completely, reaction terminates postprecipitation, elimination supernatant liquid again, then be placed in air and place 24h, respectively with distilled water, absolute ethyl alcohol alternately washing, suction filtration, to filtrate in neutral, finally be placed in vacuum drying oven dry 8h under 80 DEG C of conditions, obtained composite;
4) absorbent charcoal composite material preparation: by step 3) obtained lignocellulosic based composites is through pre-oxidation, charing and activation process, and Pre oxidation is 250 DEG C, at the H of 20wt%
3pO
4activate in the KOH solution of solution and 20wt%; In tubular type Muffle furnace, inert gas N
2carbonize in atmosphere, temperature controls 550 DEG C of calcination, is finally prepared into titanium dioxide/lignocellulosic matrix activated carbon composite.
Claims (7)
1. a preparation method for titanium dioxide/lignocellulosic matrix activated carbon composite, is characterized in that: first butyl titanate is made faint yellow Ti0 by the method
2vitreosol, then added in the wood fibre cellulose solution for preparing, make it fully react, reaction terminate and precipitation after after leaching supernatant liquid, then be placed in air and place 12 ~ 36h, then replace washing and filtering with distilled water, absolute ethyl alcohol respectively, until filtrate is in neutral; Resulting product is placed in vacuum drying oven dry 4 ~ 8h under 50 ~ 80 DEG C of conditions, obtained titanium dioxide/lignocellulose composites; Again by titanium dioxide/lignocellulose composites through pre-oxidation, charing and activation process, be prepared into the titanium dioxide/lignocellulosic matrix activated carbon composite with efficient adsorption and catalytic performance; The method comprises the following steps:
1) TiO 2 sol preparation: 15 ~ 30 parts of butyl titanates and 5 ~ 15 parts of glacial acetic acid are dissolved in 50 ~ 80 parts of absolute ethyl alcohols, magnetic agitation 0.5 ~ 2h makes it to mix, in the mixed solution of slow instillation 80 ~ 95 parts of absolute ethyl alcohols and 5 ~ 20 parts of distilled water, control buret and drip speed, sealing stirring obtains faint yellow Ti0
2vitreosol, still aging 2 ~ 4h;
2) wood fibre cellulose solution preparation: be at room temperature dissolved in corresponding solvent by lignocellulosic, being mixed with volume mass mark (g/L) is the solution of 2 ~ 20%, and magnetic agitation is transparent to solution;
3) titanium dioxide/lignocellulose composites preparation: by step 1) obtained TiO 2 sol and step 2) the wood fibre cellulose solution that obtains mixes according to the mass ratio 0.01: 1 ~ 0.5: 1 of solute, be stirred to and mix completely, reaction terminates postprecipitation, elimination supernatant liquid again, then be placed in air and place 12 ~ 36h, respectively with distilled water, absolute ethyl alcohol alternately washing, suction filtration, to filtrate in neutral, finally be placed in vacuum drying oven dry 4 ~ 8h under 50 ~ 80 DEG C of conditions, obtained titanium dioxide/lignocellulose composites;
4) absorbent charcoal composite material preparation: by step 3) obtained titanium dioxide/lignocellulose composites through pre-oxidation, charing and activation process, be prepared into titanium dioxide/lignocellulosic matrix activated carbon composite.
2. the preparation method of titanium dioxide/lignocellulosic matrix activated carbon composite according to claim 1, it is characterized in that: described ligno-cellulosic materials is Powdered finished product obtained after utilizing plant raw material to process, plant raw material comprise the stalk of all kinds of perennial and draft class plant, branch, leaf, skin and fruit shell.
3. the preparation method of titanium dioxide according to claim 1/lignocellulosic matrix activated carbon composite, is characterized in that: described step 2) lignocellulosic solvent used is one or more mixed solvent systems in dimethyl sulfoxide (DMSO), dimethyl formamide, dimethylacetylamide, N-methylmorpholine-N-oxide, etamon chloride solution, ammonium thiocyanate solution, triethanolamine, ammonia spirit, alkaline aqueous solution.
4. the preparation method of titanium dioxide according to claim 3/lignocellulosic matrix activated carbon composite, is characterized in that: described alkaline aqueous solution is alkali metal hydroxide aqueous solution, is specially NaOH, potassium hydroxide.
5. the preparation method of titanium dioxide according to claim 1/lignocellulosic matrix activated carbon composite, is characterized in that: described Pre oxidation controls at 50 ~ 350 DEG C; Activate the H at 5 ~ 20wt%
3pO
4carry out in the KOH solution of solution and 5 ~ 20wt%; Charing, in tubular type Muffle furnace, is carried out in atmosphere of inert gases, and temperature controls 400 ~ 600 DEG C of calcination.
6. the preparation method of titanium dioxide according to claim 5/lignocellulosic matrix activated carbon composite, is characterized in that: described inert gas is N
2.
7. the titanium dioxide that according to any one of claim 1-6 prepared by method/lignocellulosic matrix activated carbon composite.
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