CN109865514A - A kind of preparation method of copper/titanic oxide composite photochemical catalyst material - Google Patents
A kind of preparation method of copper/titanic oxide composite photochemical catalyst material Download PDFInfo
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- CN109865514A CN109865514A CN201910234459.0A CN201910234459A CN109865514A CN 109865514 A CN109865514 A CN 109865514A CN 201910234459 A CN201910234459 A CN 201910234459A CN 109865514 A CN109865514 A CN 109865514A
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Abstract
The present invention provides a kind of preparation method of copper/titanic oxide composite photochemical catalyst material, copper/titanic oxide composite photochemical catalyst material preparation method is using titanium potassium oxalate as titanium source, using Gerhardite as copper source, using ethylene glycol and water as reaction dissolvent, copper/the titanic oxide composite photochemical catalyst material being combined by the copper and anatase titania of cubic phase is made by hydro-thermal reaction, wherein, ethylene glycol can not only be used for reaction dissolvent, keep entire reaction system evenly dispersed, simultaneously but also as reducing agent, electronics is provided to be used to copper ion being reduced to elemental copper, synthesis process is simple, it is at low cost, it is not introduced into any toxicity reducing agent, production process is environmentally protective, meet needs of production, there is biggish application potential.
Description
Technical field
The present invention relates to catalysis material technical field, in particular to a kind of copper/titanic oxide composite photochemical catalyst material
Preparation method.
Background technique
With the fast development of industrial civilization, the demand to the energy linearly increases, adjoint and next serious energy shortage
With problem of environmental pollution.The fast development of photocatalysis technology provides possibility to solve this two big global problems, and design is efficient, can
It makes full use of the photochemical catalyst of solar energy and has been developed into domestic and international research applied to environmental improvement and fungible energy source
The hot spot of person's concern.In the flow of research of photocatalysis nano material, nano-titanium dioxide has redox due to itself
Ability is strong, high catalytic efficiency and it is nontoxic, stability is good, valence band and conduction band positions low in cost and special are available
In the degradation of photocatalytic hydrogen production by water decomposition and organic pollutant many advantages, such as, it is considered to be the currently most light of application potential
Catalysis material.But due to titanium dioxide greater band gap (anatase=3.2eV), model only is utilized to ultraviolet light response spectrum
Enclose it is narrow, in addition, its electron hole easily quickly it is compound lead to carrier low efficiency, limit the application of titanium dioxide in practice.
Researcher is modified titanium dioxide by different methods, such as ion doping, semiconductors coupling, noble metal
Load, the regulation of pattern crystal face etc., main purpose is the hair for widening light abstraction width, promoting quantum efficiency, promoting surface reaction
It is raw.Based on to nano-titanium dioxide photo electric Quality Research, nano-titanium dioxide is carried out by above-mentioned means of different
It is modified, so that titanium dioxide base nano material has well in photocatalysis degradation organic contaminant and photodissociation aquatic products hydrogen field
Application prospect.Wherein, by noble metal loading, it can effectively capture light induced electron and then improve semiconductor catalytic activity, noble metal
It is deposited on semiconductor surface and is usually expressed as two aspect effects: first is that being conducive to photo-generate electron-hole to efficiently separating；Second is that
Improve photocatalytic activity by reducing the overpotential of reduction reaction, but noble metal is rare and expensive, hinder its into
The practical application of one step.In view of effect and its own limitation of the noble metal in Photocatalyst, for alternative
Non-noble metal exploration is of great significance, and in the selection of non-noble metallic materials, metallic copper is high, cheap due to natural abundance
Being easy to get becomes potential candidate.However, the synthesis of copper at present usually requires addition sodium borohydride, ascorbic acid, glucose, water
It closes hydrazine etc. and is used as reducing agent, it is unfriendly that the introducing of these reducing agents increases the toxicity of reaction system, environment, such as sodium borohydride
It is explosive, hydrazine hydrate toxicity is big, therefore, need to carry out close supervision to its dosage and usage mode in use, carry out
Safeguard procedures, this increases the complexity of experimentation to a certain extent.
Therefore, developing the catalysis material preparation method that a kind of synthesis is simple, raw material is green non-poisonous, synthesis cost is low has
Highly important meaning.
Summary of the invention
In view of this, the present invention is directed to propose a kind of preparation method of copper/titanic oxide composite photochemical catalyst material, to solve
The problem that existing catalysis material synthesis process is complicated, toxicity is high and synthesis cost is high.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of preparation method of copper/titanic oxide composite photochemical catalyst material, comprising the following steps:
1) titanium potassium oxalate is dissolved in water, obtains titanium potassium oxalate solution；
2) Gerhardite is dissolved in the titanium potassium oxalate solution, obtains mixed solution A；
3) it disperses ethylene glycol in the mixed solution A, obtains suspension B；
4) by the suspension B heat carry out hydro-thermal reaction, to the hydro-thermal reaction after, be cooled to room temperature, then,
Centrifuge separation, washing, vacuum drying, cooling, obtained copper/titanic oxide composite photochemical catalyst material.
Optionally, the molar concentration of titanium potassium oxalate solution described in the step 1) is 0.03~0.3mol/L.
Optionally, Gerhardite described in the step 2) and the titanium potassium oxalate molar ratio are 1: 20~4: 1.
Optionally, the volume ratio of ethylene glycol described in the step 3) and water described in the step 1) is 1: 3~3: 1.
Optionally, the heating temperature of heating described in the step 4) be 120 DEG C~180 DEG C, heating time be 6h~
18h。
Copper/titanic oxide composite photochemical catalyst material synthesis mechanism of the invention are as follows:
Firstly, in water and glycol system, titanium potassium oxalate issues unboiled water and depolymerize in high temperature hydrothermal condition generates dioxy
Change titanium, the titanium dioxide surface of synthesis is adsorbed with a large amount of ethylene glycol, and the bivalent cupric ion in ethylene glycol and reaction system is complexed,
So that bivalent cupric ion is uniformly adsorbed on the surface of titanium dioxide；Finally, as reaction dissolvent ethylene glycol in high temperature hydro-thermal
Under the conditions of simultaneously be used as reducing agent, the bivalent cupric ion for being adsorbed on titanium dioxide surface is reduced to elemental copper, be made copper/dioxy
Change titanium composite photocatalyst material.
Compared with the existing technology, the preparation method of copper/titanic oxide composite photochemical catalyst material of the present invention have with
Lower advantage:
1, copper/titanic oxide composite photochemical catalyst material preparation method of the invention is using titanium potassium oxalate as titanium source, with three
Nitric hydrate copper is copper source, and using ethylene glycol and water as reaction dissolvent, the copper and rutile titania by cubic phase is made by hydro-thermal reaction
Copper/titanic oxide composite photochemical catalyst material that mine titanium dioxide is combined, wherein ethylene glycol can not only be used for reaction dissolvent, make
Entire reaction system is evenly dispersed, while but also as reducing agent, providing electronics for copper ion to be reduced to elemental copper, synthesizing
Process is simple, at low cost, is not introduced into any toxicity reducing agent, and production process is environmentally protective, meets needs of production, has larger
Application potential.
2, copper/titanic oxide composite photochemical catalyst material produced by the present invention makes titanium dioxide surface due to the introducing of elemental copper
Property changes, to be conducive to the absorption of organic pollutant, in addition, the introducing of copper promotes the transfer of electronics, realizes
Photo-generated carrier efficiently separates, and since the surface ion resonance effects (SPR) of nano copper particle urges the complex light
Change material and show high photocatalysis performance under visible light illumination, absorption and photocatalytic degradation efficiency are substantially better than monomer
Titanium dioxide.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is copper/titanic oxide composite photochemical catalyst material X-ray diffraction analysis instrument described in the embodiment of the present invention 1
(XRD) map；
Fig. 2 is monomer titanium dioxide (a) described in the embodiment of the present invention 1, elemental copper (b) and copper/titanium dioxide complex light
The SEM scanned photograph of catalysis material (c)；
Fig. 3 is copper/titanic oxide composite photochemical catalyst material described in the embodiment of the present invention 1 and monomer titanium dioxide to dyestuff
The performance comparison figure of Congo red absorption；
Fig. 4 is copper/titanic oxide composite photochemical catalyst material described in the embodiment of the present invention 1 and monomer titanium dioxide to dyestuff
Congo red Photocatalytic Activity for Degradation performance comparison figure；
Fig. 5 is copper/titanic oxide composite photochemical catalyst material described in the embodiment of the present invention 1 and monomer titanium dioxide to dyestuff
Congo red absorption-Photocatalytic Activity for Degradation circulation absorption degradation figure.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
Below in conjunction with drawings and examples, the present invention will be described in detail.
Embodiment 1
A kind of preparation method of copper/titanic oxide composite photochemical catalyst material, comprising the following steps:
1) 4mmol titanium potassium oxalate is dissolved in by 20mL water using the method for ultrasonic dissolution, without precipitating after being clarified and being placed
Titanium potassium oxalate solution；
2) 2mmol Gerhardite is dissolved in by titanium potassium oxalate solution using the method for ultrasonic dissolution, obtains mixed solution
A；
3) it is dispersed 60mL ethylene glycol in mixed solution A using the method for ultrasonic disperse, obtains suspension B；
4) suspension B is placed in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), hydro-thermal is anti-under conditions of 180 DEG C
12h is answered, after hydro-thermal reaction, cooled to room temperature, then, centrifuge separation, washing, to remove impurity, then, 60
It is dried in vacuo under the conditions of DEG C, it is cooling after sufficiently drying, copper/titanic oxide composite photochemical catalyst material is made.
It is urged using copper/titanium dioxide complex light of the BrukeraxsD8 type X-ray diffraction analysis instrument (XRD) to the present embodiment
Change material and carry out material phase analysis, and it is compared with monomer titanium dioxide, elemental copper, test results are shown in figure 1.
Wherein, the preparation method of monomer titanium dioxide, includes the following steps:
4mmol titanium potassium oxalate is dissolved in by 20mL water using the method for ultrasonic dissolution, without precipitating after being clarified and being placed
Titanium potassium oxalate solution；
Titanium potassium oxalate solution is dispersed for 60mL ethylene glycol using the method for ultrasonic disperse, obtains suspension C；
Suspension C is placed in the stainless steel autoclave that liner is polytetrafluoroethylene (PTFE), hydro-thermal under conditions of 180 DEG C
12h is reacted, after hydro-thermal reaction, cooled to room temperature, then, and centrifuge separation, washing, to remove impurity, then,
It is dried under the conditions of 60 DEG C, it is cooling after sufficiently drying, obtain monomer titanium dioxide.
The preparation method of elemental copper, includes the following steps:
5mmol Gerhardite is dissolved in by 20mL water using the method for ultrasonic dissolution, obtains copper nitrate solution；
Copper nitrate solution is dispersed for 60mL ethylene glycol using the method for ultrasonic disperse, obtains suspension D；
Suspension D is placed in the stainless steel autoclave that liner is polytetrafluoroethylene (PTFE), hydro-thermal under conditions of 180 DEG C
12h is reacted, after hydro-thermal reaction, cooled to room temperature, then, and centrifuge separation, washing, to remove impurity, then,
It is dried in vacuo under the conditions of 60 DEG C, it is cooling after sufficiently drying, obtain elemental copper.
As shown in Figure 1, the characteristic peak of the elemental copper of cubic phase and anatase monomer titanium dioxide and standard diagram JCPDS
1-1241 and JCPDS 1-562 is consistent, not the appearance of other impurity peaks, and the copper of the present embodiment/titanium dioxide complex light is urged
Change and have diffraction maximum identical with elemental copper and monomer titanium dioxide in material, and occur without mixed and disorderly peak, illustrates this implementation
Copper/titanic oxide composite photochemical catalyst material purity of example is higher.
Using JEOL JSM-5510LV type scanning electron microscope (SEM) to the copper/titanium dioxide complex light of the present embodiment
Catalysis material (2c) carries out morphology analysis, and it is compared with monomer titanium dioxide (2a), elemental copper (2b), test result
As shown in Figure 2.
As shown in Figure 2, TiO in the copper/titanic oxide composite photochemical catalyst material of the present embodiment2For the aggregation of nanometer little particle
At ball, rough surface, copper is little particle.
To copper/titanic oxide composite photochemical catalyst material absorption of the present embodiment, photocatalytic degradation, absorption-visible light light
The Congo red performance of catalytic degradation is tested, and it is compared with monomer titanium dioxide.Test result such as Fig. 3, Fig. 4 and figure
Shown in 5.
Copper/titanic oxide composite photochemical catalyst material absorption of the present embodiment, photocatalytic degradation, absorption-visible light light are urged
The testing procedure for changing Congo red performance of degrading is respectively as follows:
1) the Congo red performance test of Adsorption
Copper/the titanic oxide composite photochemical catalyst material for weighing 0.01g the present embodiment is distributed in the Congo red solution of 40mL
(20mg/L) is placed in dark place magnetic agitation, takes out the suspension of 3mL at regular intervals, and centrifuge separation takes supernatant in quartz
In cuvette, Congo red absorbance change is analyzed in ultraviolet-visible spectrophotometer, the variation of its concentration is reacted, thus table
Levy its adsorption effect.Wherein, the calculation formula of adsorption rate is (C0-Ct)/C0× 100% (C0: Congo red initial concentration；Ct: absorption
Solution concentration when time t).
2) the Congo red performance test of photocatalytic degradation
Copper/the titanic oxide composite photochemical catalyst material for weighing 0.01g the present embodiment is distributed in the Congo red solution of 40mL
(20mg/L) is placed in and reaches within dark place magnetic agitation 2 hours adsorption-desorption balance, then, in the 500W xenon lamp Imitating sun
Light irradiates (400nm ultraviolet light below is filtered with optical filter), takes out the suspension of 3mL, centrifuge separation at regular intervals
It takes supernatant in quartz colorimetric utensil, Congo red absorbance change is analyzed in ultraviolet-visible spectrophotometer, it is dense to react its
Degree variation, to characterize its degradation effect.Wherein, the calculation formula of degradation rate is (C0-Ct)/C0× 100% (C0: Congo red
Beginning concentration；Ct: solution concentration when degradation time t).
3) the Congo red cycle performance test of adsorption-photocatalytic degradation
Copper/the titanic oxide composite photochemical catalyst material for weighing 0.01g the present embodiment is distributed in the Congo red solution of 40mL
(20mg/L) is placed in and reaches within dark place magnetic agitation 2 hours adsorption-desorption balance, take 3mL suspension, and centrifuge separation takes
Clear liquid surveys its absorbance value, and solid precipitating returns to reaction system；Then, it is irradiated in 500W xenon lamp Imitating sunlight (visible
Light), 3mL suspension is taken after irradiating 4h, centrifuge separation takes supernatant to survey its absorbance value, and solid precipitating returns to reaction system.Point
It Ji Suan not adsorption rate and photocatalytic activity；By the liquid centrifugation after absorption-Photocatalytic Activity for Degradation reaction, obtains solid light and urge
Agent continuously adds the Congo red solution of 40mL (20mg/L), repeats above-mentioned experiment 5 times.
Wherein, photo catalysis reactor is the golden source CEL-LB70 type photo catalysis reactor of middle religion, long arc in above-mentioned performance test
Xenon source is the golden source CEL-LAX500 type lamp source of middle religion.Ultraviolet specrophotometer model UV2800.
From the figure 3, it may be seen that in the copper/titanic oxide composite photochemical catalyst material of the present embodiment copper introducing, make it to Congo red
Absorption property be obviously improved, this is because the introducing of copper, so that monomer titanium dioxide surface property changes, be conducive to just
Arnotto molecule is in its adsorption.
As shown in Figure 4, monomer titanium dioxide is under visible light illumination to Congo red no obvious degradation effect, and the present embodiment
Copper/titanic oxide composite photochemical catalyst material have apparent degradation effect to Congo red, after 4h radiation of visible light, 80% or so
It is Congo red by photocatalytic degradation.
As shown in Figure 5, after 5 circulation experiments, the copper/titanic oxide composite photochemical catalyst material of the present embodiment is to the Congo
It is red that still there is excellent adsorption-photocatalytic degradation effect, illustrate that its stability, cyclicity are good, there is practical application value.
Embodiment 2
A kind of preparation method of copper/titanic oxide composite photochemical catalyst material, comprising the following steps:
1) 4mmol titanium potassium oxalate is dissolved in by 40mL water using the method for ultrasonic dissolution, without precipitating after being clarified and being placed
Titanium potassium oxalate solution；
2) 8mmol Gerhardite is dissolved in by titanium potassium oxalate solution using the method for ultrasonic dissolution, obtains mixed solution
A；
3) it is dispersed 40mL ethylene glycol in mixed solution A using the method for ultrasonic disperse, obtains suspension B；
4) suspension B is placed in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), hydro-thermal is anti-under conditions of 180 DEG C
18h is answered, after hydro-thermal reaction, cooled to room temperature, then, centrifuge separation, washing, to remove impurity, then, 60
It is dried in vacuo under the conditions of DEG C, it is cooling after sufficiently drying, copper/titanic oxide composite photochemical catalyst material is made.
Embodiment 3
A kind of preparation method of copper/titanic oxide composite photochemical catalyst material, comprising the following steps:
1) 2mmol titanium potassium oxalate is dissolved in by 40mL water using the method for ultrasonic dissolution, without precipitating after being clarified and being placed
Titanium potassium oxalate solution；
2) 1mmol Gerhardite is dissolved in by titanium potassium oxalate solution using the method for ultrasonic dissolution, obtains mixed solution
A；
3) it is dispersed 40mL ethylene glycol in mixed solution A using the method for ultrasonic disperse, obtains suspension B；
4) suspension B is placed in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), hydro-thermal is anti-under conditions of 120 DEG C
8h is answered, after hydro-thermal reaction, cooled to room temperature, then, centrifuge separation, washing, to remove impurity, then, 60
It is dried in vacuo under the conditions of DEG C, it is cooling after sufficiently drying, copper/titanic oxide composite photochemical catalyst material is made.
Embodiment 4
A kind of preparation method of copper/titanic oxide composite photochemical catalyst material, comprising the following steps:
1) 6mmol titanium potassium oxalate is dissolved in by 20mL water using the method for ultrasonic dissolution, without precipitating after being clarified and being placed
Titanium potassium oxalate solution；
2) 3mmol Gerhardite is dissolved in by titanium potassium oxalate solution using the method for ultrasonic dissolution, obtains mixed solution
A；
3) it is dispersed 60mL ethylene glycol in mixed solution A using the method for ultrasonic disperse, obtains suspension B；
4) suspension B is placed in the stainless steel cauldron that liner is polytetrafluoroethylene (PTFE), hydro-thermal is anti-under conditions of 180 DEG C
18h is answered, after hydro-thermal reaction, cooled to room temperature, then, centrifuge separation, washing, to remove impurity, then, 60
It is dried in vacuo under the conditions of DEG C, it is cooling after sufficiently drying, copper/titanic oxide composite photochemical catalyst material is made.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of copper/titanic oxide composite photochemical catalyst material, which comprises the following steps:
1) titanium potassium oxalate is dissolved in water, obtains titanium potassium oxalate solution；
2) Gerhardite is dissolved in the titanium potassium oxalate solution, obtains mixed solution A；
3) it disperses ethylene glycol in the mixed solution A, obtains suspension B；
4) by the suspension B heat carry out hydro-thermal reaction, to the hydro-thermal reaction after, be cooled to room temperature, then, centrifugation
Separation, washing, vacuum drying, cooling, obtained copper/titanic oxide composite photochemical catalyst material.
2. the preparation method of copper/titanic oxide composite photochemical catalyst material according to claim 1, which is characterized in that described
The molar concentration of titanium potassium oxalate solution described in step 1) is 0.03~0.3mol/L.
3. the preparation method of copper/titanic oxide composite photochemical catalyst material according to claim 1, which is characterized in that described
Gerhardite described in step 2) and the titanium potassium oxalate molar ratio are 1: 20~4: 1.
4. the preparation method of copper/titanic oxide composite photochemical catalyst material according to claim 1, which is characterized in that described
The volume ratio of water described in ethylene glycol described in step 3) and the step 1) is 1: 3~3: 1.
5. the preparation method of copper/titanic oxide composite photochemical catalyst material according to claim 1, which is characterized in that described
The heating temperature of heating described in step 4) is 120 DEG C~180 DEG C, and heating time is 6h~18h.
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| CN113492007A (en) * | 2021-06-30 | 2021-10-12 | 武汉工程大学 | Copper-titanium dioxide core-shell structure composite material and preparation method and application thereof |
| CN113996299A (en) * | 2021-11-30 | 2022-02-01 | 南京邮电大学 | Titanium-based copper nano heterogeneous catalyst material and preparation method and application thereof |
| CN115430411A (en) * | 2021-06-02 | 2022-12-06 | 长春理工大学 | Aluminum-titanium dioxide composite photocatalytic material for treating VOC and preparation method thereof |
| CN115770572A (en) * | 2022-11-23 | 2023-03-10 | 浙江工业大学 | Biochar coupled copper catalyst and preparation method and application thereof |
| CN115845856A (en) * | 2022-11-30 | 2023-03-28 | 化学与精细化工广东省实验室 | Ultraviolet light-assisted prepared nano composite material and preparation method thereof |
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| CN115770572A (en) * | 2022-11-23 | 2023-03-10 | 浙江工业大学 | Biochar coupled copper catalyst and preparation method and application thereof |
| CN115845856A (en) * | 2022-11-30 | 2023-03-28 | 化学与精细化工广东省实验室 | Ultraviolet light-assisted prepared nano composite material and preparation method thereof |
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Application publication date: 20190611 |