CN101011654B - Preparing method of activated carbon fibre loaded titanium oxide thin film and application method thereof - Google Patents
Preparing method of activated carbon fibre loaded titanium oxide thin film and application method thereof Download PDFInfo
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- CN101011654B CN101011654B CN200710013501A CN200710013501A CN101011654B CN 101011654 B CN101011654 B CN 101011654B CN 200710013501 A CN200710013501 A CN 200710013501A CN 200710013501 A CN200710013501 A CN 200710013501A CN 101011654 B CN101011654 B CN 101011654B
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Abstract
The invention discloses a making method and using method of loaded titanium oxide film of active carbon fiber to dispose organic pollution in the water, which is characterized by the following: adopting felted active carbon fiber as carrier; fixing titanium oxide sol on the surface of active carbon; processing under nitrogen atmosphere through high temperature; adopting ultraviolet as exciting light source with solution depth at 0.4-0.6cm under 20-40 deg.c; setting the irradiating quantity on each unit area of surface at 12.5-12.8mW/cm2; maintaining the density of dissolved oxygen.
Description
Technical field
The invention belongs to a kind of new material and this preparation methods and methods for using them, relate in particular to a kind of preparation method and application process method thereof that is used for handling the carbon base optic catalytic composite material of water organic pollution.
Background technology
The control of environmental pollution is the key subjects that human society faces and expects to solve with administering.Because modern industry all water body discharging towards periphery contains the waste water of a large amount of organic pollutions, many organic pollutions contain biology are strong inhibiting phenyl ring, are difficult to biodegradation, thereby make available water resource fewer and feweri.
Handle at present that to use more in the method for the organic pollution of difficult for biological degradation in the water be photocatalytic oxidation.Photocatalytic oxidation is a kind of directly effective processing method, more and more is subject to people's attention, and especially utilizes TiO
2Semiconductor powder has become the focus of research as the catalytic oxidation new technology of photochemical catalyst.It can realize the permineralization of pollutant, is degraded to simple inorganic matter such as carbon dioxide, water, rather than pollutant is transferred to another kind of medium from a kind of medium.But Ti0 with highlight catalytic active
2Generally based on nanometer grade powder or graininess, in actual applications, often there are shortcomings such as the difficult recovery of easy cohesion in suspended state, has seriously limited its practical application at liquid-phase system, so TiO
2On different carriers, fixedly become the focus of material science and technology research field in recent years.TiO
2Fixing on suitable backing material, the lower target contaminant of body phase solution concentration can be concentrated to around the titanium dioxide, reach the purpose that improves light-catalyzed reaction efficient.Not only can solve the recovery and the recycling problem of catalyst, also can continue the photocatalytic activity and the degree of depth mineralising effect that keep high.
Active carbon is the more class carbon absorbent of research, also is to obtain a sure class effective carrier in photocatalysis field so far.Many results of study show: will be titania oxide supported after on the active carbon, the simulating pollution thing that is used for degrading, the degradation effect of discovery pollutant are faster during all than the non-activity charcoal.Therefore think and to exist cooperative effect between the two that promptly pollutant is moved to titanium dioxide surface or interface then gradually degradation reaction is taken place at first by charcoal absorption.Because active carbon is generally in the majority with granular and powdery, great majority and the complexs of titanium dioxide still keep the original form of active carbon, and it separates with to reclaim technology relative miscellaneous, weares and teares easily and efflorescence in the application process.Simultaneously titanium dioxide powder is fixing insecure, enters solution easily and becomes suspension system.
NACF (Activated carbon fiber, ACF) be a kind of novel carbon absorbent that grows up the 1980s, having abundant and flourishing pore structure, can require to be made into cloth shape or felted according to reality, be a kind of desirable load carriers.Therefore the present invention adopts the carrier of NACF as titanium oxide, substitutes the active carbon in the former studies.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application process method thereof of separating with the activated carbon fibre loading titanium oxide thin film that reclaims the organic pollution that is easy to be used for to handle the water difficult for biological degradation.
The present invention is achieved by the following technical solution:
The present invention is fixed in the fiber-reactive carbon surface with the NACF of the felted carrier as titanium dioxide with the TiO 2 sol for preparing, and realizes the load of titanium dioxide on the NACF felt through high-temperature process then under blanket of nitrogen.
Concrete preparation method is as follows:
1. the preparation of TiO 2 sol:
(1) at room temperature the tetra-n-butyl titanate of 10-20mL is joined in the absolute ethyl alcohol of 20-30mL, stir 20-40min, the yellow solution that obtains homogeneous transparent 1.;
(2) at room temperature absolute ethyl alcohol, 10-30mL glacial acetic acid, the 5-10mL distilled water of 10-40mL is fully mixed, obtain solution 2., place liquid separatnig container standby;
(3) under magnetic agitation and constant temperature 20-40 ℃ condition, with solution 2. slowly be added drop-wise to solution 1. in, obtain the colloidal sol of homogeneous transparent,
2. the load of titanium dioxide on the NACF felt:
(1) it is stand-by after 2-4 hour that the colloidal sol that will just prepare places 20-40 ℃ of insulating box ageing;
(2) with ACF felt (viscose glue base, 1000-1500m
2/ g, total hole volume 0.3-0.9cm
3/ g) cut into bulk, after oven dry is handled 3-6 hour under the 100-140 ℃ of condition, take out, entirely put in pallet, then the colloidal sol after the ageing is poured on the ACF felt equably, treat that its absorption is saturated after, place 80 ℃ of oven dry of baking oven;
(3) after the oven dry, it is saturated to its absorption to topple over colloidal sol again on the ACF felt, places baking oven 70-90 ℃ oven dry again, and three times so repeatedly, the load of realization titania precursor body and ACF;
(4) the ACF felt of titania precursor body in the load is changed over to carry out calcination processing in the carbonization-activation stove; heating rate 3-10 ℃/min; nitrogen flow is 20-40mL/min; after reaching 500-700 ℃; calcining at constant temperature 1.5-3h; directly enter the nature temperature-fall period afterwards, take out sample after being cooled to normal temperature under the nitrogen protection, obtain the composite photocatalyst material (also claiming carbon base optic catalytic composite material) of titanium oxide and ACF load.
Carbon base optic catalytic composite material application process of the present invention (biodegrading process that promptly is used for liguid phase pollutant): light-catalyzed reaction with ultraviolet light as excitation source.Photocatalytic reaction conditions is:
(1) light source is ultraviolet and visible light source, and light source direct irradiation solution, solution deep are 0.4-0.6 centimetre, and the irradiation of solution surface unit are is 12.5-12.8mW/cm
2
(2) temperature constant of solution system is at 20-40 ℃, and lasting bubbling air is kept the concentration of dissolved oxygen.
The present invention compares with prior art has outstanding feature and progress:
1. carbon base optic catalytic composite material is active high, can reduce pollutant levels at short notice fast, finally pollutant almost completely can be degraded.
2. the preparation process of carbon base optic catalytic composite material is simple, and titanium dioxide does not have serious obscission in the surperficial fixation of NACF.
3. carbon base optic catalytic composite material is reusable, and photocatalysis efficiency almost remains unchanged.
The specific embodiment
The invention will be further described below in conjunction with example:
1. the preparation of TiO 2 sol:
(1) at room temperature the tetra-n-butyl titanate of 0.05mol is joined in the absolute ethyl alcohol of 30mL, stir 30min, the yellow solution that obtains homogeneous transparent 1.;
(2) at room temperature absolute ethyl alcohol, 20mL glacial acetic acid, the 7.2mL distilled water of 28.32mL is fully mixed, obtain solution 2., place separatory funnel standby;
(3) under magnetic agitation and 30 ℃ of conditions of constant temperature, with solution 2. slowly be added drop-wise to solution 1. in, obtain the colloidal sol of homogeneous transparent.
2. the load of titanium dioxide on the NACF felt:
(1) it is stand-by after 3 hours that the colloidal sol that will just prepare places 30 ℃ of insulating box ageings;
(2) with ACF felt (viscose glue base, BET specific area 1276m
2/ g, total hole volume 0.597cm
3/ g) cut into the pane of 100 * 25mm, after oven dry is handled 4 hours under 120 ℃ of conditions, take out, entirely be placed in the clean and dry pallet, then the colloidal sol after the ageing is poured on the ACF felt equably, after treating that its absorption is saturated, place 80 ℃ of oven dry of baking oven;
(3) after the oven dry, it is saturated to its absorption to topple over colloidal sol again on the ACF felt, places 80 ℃ of oven dry of baking oven again, and three times so repeatedly, the load of realization titania precursor body and ACF;
(4) the ACF felt of titania precursor body in the load is changed over to carry out calcination processing in the carbonization-activation stove; heating rate is 5 ℃/min; nitrogen flow is 30mL/min; after reaching 600 ℃ of target temperatures; calcining at constant temperature 2 hours; directly enter the nature temperature-fall period afterwards, take out sample after being cooled to normal temperature under the nitrogen protection, obtain the composite photocatalyst material of titanium oxide and ACF load.
Application example 1: get the carbon base optic catalytic composite material of 5 100 * 25mmACF felts through 600 ℃ of calcinings, with line with its suspension and be uniformly distributed in the 250mL reactor, light source is the high-pressure sodium lamp of 500W, solution deep is 0.4 centimetre, the temperature constant of solution system is at 20 ℃, and lasting bubbling air is kept the concentration of dissolved oxygen.With methyl orange is the simulating pollution thing, and initial concentration is 120mg/L.Behind the illumination reaction 6 minutes, methyl orange solution decolours fully; Fresh original solution is removed and be replaced by to solution in the reactor, carry out the reaction of second stage again, after 6 minutes, methyl orange solution decolours fully; In the phase III reaction, after 9 minutes, methyl orange solution decolours fully; The quadravalence section can cause methyl orange solution and decolour fully in 9 minutes.
Application example 2: get the carbon base optic catalytic composite material of 5 little 100 * 25mmACF felts through 600 ℃ of calcinings, with line with its suspension and be uniformly distributed in the 250mL reactor, light source is the high-pressure sodium lamp of 500W, solution deep is 0.6 centimetre, the temperature constant of solution system is at 40 ℃, and lasting bubbling air is kept the concentration of dissolved oxygen.With the acid fuchsin is the simulating pollution thing, and initial concentration is 200mg/L.Behind the illumination reaction 20 minutes, methyl orange solution decolours fully; Fresh original solution is removed and be replaced by to solution in the reactor, carry out the reaction of second stage again, after 20 minutes, methyl orange solution decolours fully; In the phase III reaction, after 20 minutes, methyl orange solution decolours fully; The quadravalence section also can cause methyl orange solution and decolour fully in 20 minutes.
The parameter value that the present invention provides is a ratio value, and zooming in or out in proportion belongs to protection scope of the present invention equally.
Claims (4)
1. the preparation method of activated carbon fibre loading titanium oxide thin film is characterized in that comprising following content:
(1) it is stand-by after 2-4 hour that the TiO 2 sol that will just prepare places 20-40 ℃ of insulating box ageing;
(2) the NACF felt is cut into bulk, after oven dry under the 100-140 ℃ of condition is handled 3-6 hour, takes out, then the colloidal sol after the ageing is poured on the NACF felt equably, treat that its absorption is saturated after, place 80 ℃ of oven dry of baking oven;
(3) after the oven dry, the colloidal sol after toppling over ageing on the NACF felt is saturated to its absorption again, places baking oven 70-90 ℃ oven dry again, three times so repeatedly, realizes the load of titania precursor body and NACF;
(4) the NACF felt of titania precursor body in the load is changed over to carry out calcination processing in the carbonization-activation stove; heating rate is 3-10 ℃/min; nitrogen flow is 20-40mL/min; after reaching 500-700 ℃; calcining at constant temperature 1.5-3 hour; directly enter the nature temperature-fall period afterwards, be cooled to normal temperature under the nitrogen protection after, obtain activated carbon fibre loading titanium oxide thin film.
2. the preparation method of activated carbon fibre loading titanium oxide thin film according to claim 1 is characterized in that also comprising the preparation method of TiO 2 sol:
(1) at room temperature the tetra-n-butyl titanate of 10-20mL is joined in the absolute ethyl alcohol of 20-30mL, stir 20-40min, the yellow solution that obtains homogeneous transparent 1.;
(2) at room temperature absolute ethyl alcohol, 10-30mL glacial acetic acid, the 5-10mL distilled water of 10-40mL is fully mixed, fully 2. stirring and dissolving forms solution, places liquid separatnig container standby;
(3) under magnetic agitation and constant temperature 20-40 ℃ condition, with solution 2. slowly be added drop-wise to solution 1. in, obtain the TiO 2 sol of homogeneous transparent.
3. the preparation method of activated carbon fibre loading titanium oxide thin film according to claim 1 and 2, it is characterized in that: described NACF felt is the viscose glue base, BET specific area 1000-1500m
2/ g, total hole volume 0.3-0.9cm
3/ g.
4. according to the application process of the preparation-obtained activated carbon fibre loading titanium oxide thin film of preparation method of the described activated carbon fibre loading titanium oxide thin film of claim 1, it is characterized in that photocatalytic reaction conditions is:
(1) light source is ultraviolet and visible light source, and light source direct irradiation solution, solution deep are 0.4-0.6 centimetre, and the irradiation of solution surface unit are is 12.5-12.8mW/cm
2
(2) temperature constant of solution system is at 20-40 ℃, and lasting bubbling air is kept the concentration of dissolved oxygen.
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| CN106732503A (en) * | 2016-12-14 | 2017-05-31 | 上海华明高技术（集团）有限公司 | NACF of load nano-titanium dioxide film and its production and use |
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