CN109939745A - A kind of nano-titanium dioxide/wood flour composite material and its preparation method and application - Google Patents
A kind of nano-titanium dioxide/wood flour composite material and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of nano-titanium dioxide/wood flour composite materials and its preparation method and application, belong to nanocomposite technical field.Nano-titanium dioxide/the wood flour composite material is combined by titanium dioxide and Hu mulberry branch wood powder, wherein Hu mulberry branch wood powder is carrier, and titanium dioxide is dispersed in wood powder surface in the form of nano particle.Preparation method of the present invention is simple, and solvent for use NaOH/ urea is cheap and easy to get, and equipment is simple and easy；Nano-titanium dioxide/wood flour composite material of preparation contains 43% or so TiO2；97% is reached to the removal efficiency of light degradation waste water from dyestuff Methylene Blue；Titanium dioxide/wood flour composite material prepared by the present invention, cheap environmental protection have good practicability in terms of the processing as Photodegradation catalyst and methylene blue waste water.
Description
Technical field
The invention belongs to nano-titanium dioxide/wood flour composite material technical fields, and in particular to and a kind of nano-titanium dioxide/
Wood flour composite material and its preparation method and application.
Background technique
Titanium dioxide (TiO2) it is a kind of important wide bandgap semiconductor functional material, rutile titanium dioxide at room temperature
Forbidden bandwidth is 3.0eV, and anatase titanium dioxide forbidden bandwidth is 3.2eV.Its chemical physical property is quite stable, has nothing
Advantage malicious, pollution-free, low in cost, and oxidation susceptibility is excellent, has special thermally conductive, conducting function, TiO2As one kind
Semiconductor material is widely used in the fields such as photochemical catalyst, gas sensor, solar battery and biosensor.Nanometer
TiO2Micro mist has superior antibacterial, photocatalysis and absorption property, but traditional single nano-TiO2Will appear easy in inactivation,
The problems such as separation and recovery easy to reunite, not easily settled, difficult.Prepare extinction effect protrusion, loaded nano TiO2Composite material both may be used
One-component photochemical catalyst stability is poor, disadvantage of extinction effect difference to solve, and can solve photochemical catalyst and recycle secondary benefit
The problem of using.And have ceramics as the common carrier of loaded photocatalyst, active carbon, and the nanofiber that has excellent performance and
Nanotube etc..But the reduction of the following photochemical catalyst extinction efficiency and the price problem system of nanofiber and nanotube
The about further investigation of the method.
In the art, other effects of type composite material in terms of extinction efficiency are less desirable.In Chinese patent
Apply in CN106362799A, discloses that a kind of based on NaOH/ urea liquid direct precipitation method to prepare nano-ZnO cellulose compound
The method and application of material are the previous research of the applicant, use the NaOH/ urea liquid of low temperature for solvent, chlorination
Zinc is zinc source, and Direct precipitation obtains ZnO cellulose composite material, obtained composite material to the removal rate of methylene blue solution most
A height of 69.73%.
Summary of the invention
Goal of the invention: aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of nanometer titanium dioxides
Titanium/wood flour composite material meets the use demand of photochemical catalyst.It is another object of the present invention to provide a kind of nano-silicas
Change titanium/wood flour composite material preparation method.
Technical solution: to solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
A kind of nano-titanium dioxide/wood flour composite material is combined by titanium dioxide and Hu mulberry branch wood powder, wherein
Hu mulberry branch wood powder is carrier, and titanium dioxide is dispersed in wood powder surface in the form of nano particle.
Nano-titanium dioxide/the wood flour composite material, the mass content of titanium dioxide are 43%.
Nano-titanium dioxide/wood flour composite material preparation method: into the aqueous solution of low temperature NaOH/ urea,
Hu mulberry branch wood powder is added, stirring obtains the suspension of wood powder to being partly dissolved rapidly；Hanging drop is added to titanium source solution
In, stirring ageing obtains mixture；Mixture is transferred in hydrothermal reaction kettle, hydro-thermal reaction, after the reaction was completed natural cooling
To room temperature；Sediment is collected, is rinsed with deionized water to neutrality, drying obtains nano-titanium dioxide/wood flour composite material.
Nano-titanium dioxide/wood flour composite material preparation method, in the aqueous solution of the NaOH/ urea,
NaOH: urea: H2The mass ratio of O is 7: 12: 81.
Nano-titanium dioxide/wood flour composite material preparation method, titanium source is titanium sulfate solution.
Nano-titanium dioxide/wood flour composite material preparation method, stirring digestion time are 30min.
Nano-titanium dioxide/wood flour composite material preparation method, hydrothermal temperature are 80-140 DEG C, hydro-thermal
Reaction time is 4-16h.
Nano-titanium dioxide/wood flour composite material preparation method, the temperature of the aqueous solution of NaOH/ urea is-
12℃
Application of the nano-titanium dioxide/wood flour composite material as photochemical catalyst.
Application of the nano-titanium dioxide/wood flour composite material in photocatalytic degradation methylenum careuleum waste water.
The utility model has the advantages that compared with prior art, the invention has the advantages that
(1) compared with prior art, original position one step hydro thermal method of the present invention prepares nano-titanium dioxide/wood flour composite material
Method, method is simple, and equipment is simple and easy, at low cost, obtains the nano-TiO of different-shape by controlling reaction condition2/ wood powder
Composite material contains 43% or so titanium dioxide.
(2) nano-titanium dioxide/wood flour composite material prepared by the present invention contaminates light degradation as Photodegradation catalyst
Expect the methylene blue removal efficiency with higher in waste water, removal rate is up to 97%, has good practicability.
(3) present invention realize sericulture byproduct Hu mulberry branch resource utilization, reduce environmental pollution, and for
Wood powder prepares load type titanium dioxide catalyst as carrier, has good practicability.
Detailed description of the invention
Fig. 1 is the electron microscope of 1 product of embodiment；
Fig. 2 is the ultraviolet-visible spectrogram of 1 product of embodiment；
Fig. 3 is the TG figure of 1 product of embodiment；
Fig. 4 is the XRD diagram of 1 product of embodiment；
Fig. 5 is the methylene blue removal rate figure of embodiment 1；
Fig. 6 is the dynamic analysis figure that the different materials of embodiment 1 degrade to methylenum careuleum；
Fig. 7 is the electron microscope of 2 product of embodiment；
Fig. 8 is the XRD diagram of 2 product of embodiment；
Fig. 9 is the electron microscope of 3 product of embodiment；
Figure 10 is the XRD diagram of 3 product of embodiment；
Figure 11 is the electron microscope of 4 product of embodiment；
Figure 12 is the XRD diagram of 4 product of embodiment.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right combined with specific embodiments below
A specific embodiment of the invention is described in detail.
Embodiment 1
2g Hu mulberry branch wood powder is taken to be added to the aqueous solution (NaOH: urea: H that 50g is cooled to -12 DEG C of NaOH/ urea in advance2O
Mass ratio be 7: 12: 81) in, rapidly stir 30min after, wood powder is partly dissolved to obtain the suspension of certain viscosity, will hang
Supernatant liquid is slowly dropped in 50mL titanium sulfate solution (1mol/L), and after stirring ageing 30min, mixture is transferred to hydro-thermal reaction
In kettle, 12h is heated at 120 DEG C, cooled to room temperature collects sediment, is rinsed several times with deionized water, adjusts filtrate pH
To neutrality, drying weighing obtains nano-TiO in 70 DEG C of baking ovens2/ wood flour composite material.To the nano-TiO of preparation2/ wood powder composite wood
Material is characterized, specific as follows:
Prepared nano-TiO2The electron microscope of/wood flour composite material from electron microscope as shown in Figure 1, can be seen that TiO2With
The form of nano particle is gathered in wood powder surface, surface porosity, is conducive to improve it and contacts with photochemical catalyst, improves its photocatalysis
Degradation efficiency.
To prepared nano-TiO2/ wood flour composite material (being indicated with BC) and commodity titanium dioxide P25 (being indicated with P25)
UV, visible light analysis is carried out, ultraviolet-visible spectrogram is as shown in Fig. 2, the nano-TiO prepared2/ wood flour composite material is in ultraviolet light
Part has apparent absorption, big compared to absorption intensity with commodity titanium dioxide P25 and mobile to visible light direction.
Control group (being indicated with WP) without titanium sulfate, other synthesis technology steps are identical as BC experimental group, test to BC
Group and WP control group carry out TG analysis, and it is as shown in Figure 3 that TG analyzes result.TiO in the composite material prepared as can be seen from Figure 32
Content is 43%.
To prepared nano-TiO2/ wood flour composite material carries out XRD test, as a result as shown in Figure 4.It can from XRD diagram
To find out, 2 θ=23.35 ° of the angle of diffraction, 37.01 °, 48.0 ° and 54.30 °, corresponding TiO2(101) of crystal, (004),
(200) it matches with the standard card JCPDS No.21-1272 of (211) crystal face and titanium dioxide anatase.2 θ=14.8 °
With 22.6 ° at there are two characteristic peak, corresponding is the diffraction maximum of cellulose, illustrates that the product is TiO2With the compound production of wood powder
Object.
The control group (being indicated with CK) of wood powder is not added, other synthesis technology steps are identical as BC experimental group.Test b C experiment
The light degradation property of material in group, CK control group and P25 control group to methylene blue waste water.
The methylene blue solution that 50mL initial concentration is 20mg/L is added in three 250mL quartz beakers, is separately added into
BC experimental group, CK control group and P25 material 0.2g, are stirred on magnetic stirring apparatus, after stirring 30min in the dark, in ultraviolet light
Under the irradiation of sunshine light, every 30min sampling analysis Methylene Blue in Solution concentration, 2h is stirred altogether, three groups of materials are tested after 2h
To the removal rate of methylene blue.
The concentration ultraviolet-uisible spectrophotometer of methylene blue surveys absorbance according to methylene blue concentration mark at 664nm
Directrix curve obtains.The removal rate of methylenum careuleum, which calculates, uses formula:
η (%)=(C0-C)/C0* 100%
In formula, C0It is the concentration of light degradation front and back methylene blue solution respectively with C.
The removal rate effect of methylene blue is as shown in Figure 5.With the increase of light degradation time, nano-TiO in Fig. 52/ wood powder
Composite material gradually increases the removal rate of waste water from dyestuff Methylene Blue, and under similarity condition, CK control group material and commercialization
TiO2(P25) to the removal rate of methylene blue, the effect is unsatisfactory after 150min, distinguishes the maximum material removal rate of methylene blue
For 81.8% and 82.9%, and BC experimental group nano-TiO2Removal rate of/the wood flour composite material to waste water from dyestuff Methylene Blue
Up to 97%.
The kinetic results of BC experimental group, CK control group and P25 material light catalysis degradation of methylene blue are as shown in Figure 6.
TiO2/ wood flour composite material, CK control group and P25 are respectively to ln (C under methylene blue 20mg/L concentration0/ C) make with time t relationship
Figure.From fig. 6, it can be seen that lnC0/ C and reaction time t are substantially in a linear relationship, and R2 is 0.98 or more, reaction rate constant
Respectively 0.02464,0.01988,0.01228, this illustrates that the degradation of dyestuff methylene blue substantially conforms to first-order kinetics
Feature.
Embodiment 2
50g is taken to prepare the aqueous solution (NaOH: urea: H of the pre- NaOH/ urea for being cooled to -12 DEG C2The mass ratio of O is 7: 12
: 81), Hu mulberry branch wood powder of the 2g through ball milling pretreatment is added, hanging drop is added to 50mL titanium sulfate to dissolving by stirring rapidly
In solution (1mol/L), after stirring ageing 30min, mixture is transferred in hydrothermal reaction kettle, heats 4h at 120 DEG C, from
It is so cooled to room temperature, collects sediment, rinsed several times with deionized water, adjusting filtrate pH to neutrality, dry and claim in 70 DEG C of baking ovens
Restore nano-TiO2/ wood flour composite material.From the visible TiO of Fig. 7 electron microscope2Nanoparticle aggregate is dispersed in wood powder at cauliflower shape
Surface, to prepared nano-TiO2/ wood flour composite material carries out XRD test, as can be seen that the angle of diffraction from XRD diagram (Fig. 8)
2 θ=23.35 °, 37.01 °, 48.0 ° and 54.30 °, corresponding TiO2(101), (004), (200) and (211) of crystal
The standard card JCPDS No.21-1272 of crystal face and titanium dioxide anatase matches.Have two at 2 θ=14.8 ° and 22.6 °
A characteristic peak, corresponding is the diffraction maximum of cellulose, illustrates that the product is TiO2With the combination product of wood powder.
Embodiment 3
50g is taken to prepare the aqueous solution (NaOH: urea: H of the pre- NaOH/ urea for being cooled to -12 DEG C2The mass ratio of O is 7: 12
: 81), 2g Hu mulberry branch ball milling wood powder is added, hanging drop is added to 50mL titanium sulfate solution (1mol/ to dissolving by stirring rapidly
L in), after stirring ageing 30min, mixture is transferred in hydrothermal reaction kettle, 2h is heated at 90 DEG C, naturally cools to room
Temperature collects sediment, is rinsed several times with deionized water, adjusting filtrate pH to neutrality, dries in 70 DEG C of baking ovens, 300 DEG C of calcining 2h.
Weighing obtains nano-TiO2/ wood flour composite material.From the visible TiO through calcining of Fig. 9 electron microscope2It is sintered together, only on a small quantity
Particle floats on the surface.To prepared nano-TiO2/ wood flour composite material carries out XRD test, can from XRD diagram (Fig. 8)
Out, 2 θ=23.35 ° of the angle of diffraction, 37.01 °, 48.0 ° and 54.30 °, corresponding TiO2(101) of crystal, (004),
(200) it matches with the standard card JCPDS No.21-1272 of (211) crystal face and titanium dioxide anatase.2 θ=27.5 °
There is the characteristic peak of titanium dioxide rutile, illustrates through calcining TiO2It is converted to rutile.
Embodiment 4
50g is taken to prepare the aqueous solution (NaOH: urea: H of the pre- NaOH/ urea for being cooled to -12 DEG C2The mass ratio of O is 7: 12
: 81), the Hu mulberry branch wood powder of the non-ball milling of 2g is added, after stirring evenly 30min rapidly, obtained hanging drop is added to 30mL
In titanium sulfate solution (1mol/L), after stirring ageing 30min, mixture is transferred in hydrothermal reaction kettle, is heated at 120 DEG C
12h, cooled to room temperature collect sediment, are rinsed several times with deionized water, adjusting filtrate pH to neutrality, in 70 DEG C of baking ovens
Drying weighing obtains nano TiO 2/wood flour composite material.From the visible TiO of electron microscope 112It is supported on wood powder surface, to prepared
Nano TiO 2/wood flour composite material carries out XRD test, from XRD diagram (Figure 12) as can be seen that 2 θ=23.35 ° of the angle of diffraction,
37.01 °, 48.0 ° and 54.30 °, (101) of corresponding TiO2 crystal, (004), (200) and (211) crystal face and dioxy
The standard card JCPDS No.21-1272 for changing titanium anatase matches.There are two characteristic peaks at 2 θ=14.8 ° and 22.6 °, right
What is answered is the diffraction maximum of cellulose, illustrates that the product is the combination product of TiO2 and wood powder.
Claims (10)
1. a kind of nano-titanium dioxide/wood flour composite material, which is characterized in that by titanium dioxide and Hu mulberry branch wood powder it is compound and
At, wherein Hu mulberry branch wood powder is carrier, and titanium dioxide is dispersed in wood powder surface in the form of nano particle.
2. nano-titanium dioxide/wood flour composite material according to claim 1, which is characterized in that dioxy in composite material
The mass content for changing titanium is 43%.
3. the preparation method of nano-titanium dioxide/wood flour composite material of any of claims 1 or 2, it is characterised in that: to low temperature
In the aqueous solution of NaOH/ urea, Hu mulberry branch wood powder is added, stirring obtains the suspension of wood powder to being partly dissolved rapidly；It will hang
Supernatant liquid is added drop-wise in titanium source solution, and stirring ageing obtains mixture；Mixture is transferred in hydrothermal reaction kettle, hydro-thermal reaction,
Cooled to room temperature after the reaction was completed；Sediment is collected, is rinsed with deionized water to neutrality, drying obtains nanometer titanium dioxide
Titanium/wood flour composite material.
4. the preparation method of nano-titanium dioxide/wood flour composite material according to claim 3, which is characterized in that described
In the aqueous solution of NaOH/ urea, NaOH: urea: H2The mass ratio of O is 7: 12: 81.
5. the preparation method of nano-titanium dioxide/wood flour composite material according to claim 3, which is characterized in that titanium source
For titanium sulfate solution.
6. the preparation method of nano-titanium dioxide/wood flour composite material according to claim 3, which is characterized in that stirring
Digestion time is 30min.
7. a kind of preparation method of nano-titanium dioxide/wood flour composite material according to claim 3, which is characterized in that
Hydrothermal temperature is 80-140 DEG C, the hydro-thermal reaction time 4-16h.
8. a kind of preparation method of nano-titanium dioxide/wood flour composite material according to claim 3, which is characterized in that
The temperature of the aqueous solution of NaOH/ urea is -12 DEG C.
9. application of the nano-titanium dioxide/wood flour composite material of any of claims 1 or 2 as photochemical catalyst.
10. nano-titanium dioxide/wood flour composite material of any of claims 1 or 2 is in photocatalytic degradation methylenum careuleum waste water
Using.
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| CN110860313A (en) * | 2019-12-09 | 2020-03-06 | 南京林业大学 | Nano zinc oxide/zinc ferrite/wood powder ternary composite material and preparation method and application thereof |
| CN113769782A (en) * | 2021-08-16 | 2021-12-10 | 武夷学院 | Preparation method and application of photocatalytic composite material |
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Application publication date: 20190628 |