CN103480353A - Method for synthesis of carbon quantum dot solution by hydrothermal process to prepare composite nano-photocatalyst - Google Patents
Method for synthesis of carbon quantum dot solution by hydrothermal process to prepare composite nano-photocatalyst Download PDFInfo
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Abstract
The invention presents a method for synthesis of a carbon quantum dot modified TiO2 composite nano-photocatalyst. The method includes: using vitamin C as a carbon source, in a mixed solution of ethanol absolute and deionized water, preparing a carbon quantum dot with an up-conversion characteristic by a hydrothermal process, then preparing spherical TiO2 powder by a sol-gel process, mixing the spherical TiO2 powder with a carbon quantum dot solution, and performing drying, thus obtaining the composite nano-photocatalyst. The method provided in the invention makes use of the up-conversion characteristic of the carbon quantum dot to modify TiO2 so as to prepare the composite nano-photocatalyst, has the advantages of simple operation, and low cost, etc., and has very high practical value and application prospects.
Description
Technical field
The present invention relates to a kind of synthetic method of visible light responsive photocatalyst, specially refer to a kind of hydrothermal synthesis of carbon quantum dot modified titanic oxide composite Nano photochemical catalyst preparation.
Background technology
Along with sharply increase and the socioeconomic high speed development of China's population, environmental problem becomes increasingly conspicuous, and oneself affect through becoming the matter of utmost importance that the modernization construction of Chinese society doctrine and the people produce, live.This wherein, the water pollution situation is particularly serious.Since at N-shaped semiconductor TiO
2since finding the photoelectrocatalysis decomposition of water on electrode, by TiO
2caused great attention as photochemical catalyst for researchs such as waste water controls.TiO
2the photochemical catalyst chemical property is stable and cost is low, toxicity is low, catalytic activity is high, oxidability is strong.Therefore, with TiO
2as the high-level oxidation technology of photochemical catalyst, extensive application aspect removal waste water, exhaust emission.Yet, for this catalyst, exist equally some open defects, one, when take sunshine or visible ray during as radiation source, it utilizes luminous energy efficiency lower, only less than 5% sunshine, can be utilized; Its two, the compound probability that its surface produces electron-hole is larger, thereby catalytic performance is restricted.
The carbon quantum dot is considered to a kind of novel luminescent material, at bio-sensing and biomedical sector, has great potential using value.Due to the impact of quantum size effect and Dielectric confinement effect, undersized carbon nano-particles has unique photoelectric property, makes it in fields such as luminous lighting, solar cell and biomarkers, demonstrate larger application prospect.The carbon quantum dot has upper conversion function, makes under visible ray and absorbs lower energy photon, and discharging high-energy photon.Utilize this characteristic, the quantum-dot modified titanium dioxide of carbon is just arranged, make the photochemical catalyst generation active specy that can be stimulated under visible ray, pollutant in the degraded water body.
Summary of the invention
The purpose of this invention is to provide a kind of preparation of the carbon quantum dot based on hydro-thermal method and to TiO
2carry out modification, prepare the method for complex light nanocatalyst, realize the composite photo-catalyst that the modification preparation based on this carbon quantum dot has visible absorption, realize the utilization to visible ray, and then improve photocatalysis efficiency.
The present invention can be achieved by the following technical programs:
Step 1: prepare the carbon quantum dot solution
(1) vitamin c solution of the solution allocation 0.125M that the absolute ethyl alcohol that is 1:1 by volume ratio and deionized water mix, obtain the transparent reaction precursor solution;
(2) precursor solution is joined in reactor, the reaction time is 2h～8h, and reaction temperature is 140 ℃～200 ℃, obtains the dark brown product;
(3) add carrene in above-mentioned dark brown product, repeatedly, after the extraction, get upper water solution and carry out separation and purification through dialysis membrane, obtain the carbon quantum dot solution;
Step 2: prepare the composite Nano photochemical catalyst
(1) butyl titanate is joined in absolute ethyl alcohol, then drip the iminodiacetic acid (salt) acid solution, obtain mixed solution, wherein the volume ratio of butyl titanate, absolute ethyl alcohol, iminodiacetic acid is 17:57.5:4.125, then use NaOH and hydrochloric acid solution that above-mentioned mixed solution pH value is adjusted to 6.0～8.0, obtain white suspension;
(2) to above-mentioned white suspension, at room temperature stir and evenly mix, dropwise add subsequently excessive absolute ethyl alcohol and stirring, collect the white depositions generated and wash drying by absolute ethyl alcohol and deionized water, under 300 ℃～500 ℃, calcining is 2 hours, makes TiO
2spherical nanoparticle;
(3) by TiO
2the carbon quantum dot solution that spherical nanoparticle and above-mentioned steps one obtain is 1:0～0.15 mix and blend in molar ratio, and under 60～100 ℃, drying is 12 hours, obtains the composite Nano photochemical catalyst.
The present invention has following innovative point:
(1) synthetic carbon quantum dot in reactor, can improve the particle size distribution of carbon quantum dot by simple change reaction time and reaction temperature, regulate transfer characteristic on it.
(2) by sol-gal process, synthetic titanium dioxide powder has multiple hole, and bigger serface can impel the mass transport process of catalytic reaction, accelerates degradation reaction speed.
(3) raw material that preparation is used is cheap and easy to get, without expensive device.
The accompanying drawing explanation
The up-conversion fluorescence performance diagram that Fig. 1 is the synthetic CQDs of reaction 4h under 180 ℃;
The spherical TiO that does not add the carbon quantum dot that Fig. 2 is synthesized of the present invention
2the scanning electron microscope (SEM) photograph of sample (SEM), (a) be 10000 times of multiplication factors; (b) be 20000 times of multiplication factors;
The spherical TiO that Fig. 3 is synthesized of the present invention
2the scanning electron microscope (SEM) photograph of/CQDs sample (SEM);
The TiO that Fig. 4 is synthesized of the present invention
2/ CQDs and TiO
2the N of sample
2the adsorption-desorption isothermal curve;
The TiO that Fig. 5 is synthesized of the present invention
2/ CQDs and TiO
2the UV-vis DRS spectrogram of sample;
The TiO that Fig. 6 is synthesized of the present invention
2the degradation property of the composite Nano photochemical catalyst different from the CQDs mol ratio relatively.
The specific embodiment
Synthetic and the catalytic performance of implementation procedure of the present invention and photocatalyst material are illustrated by embodiment.
Embodiment 1: the hydrothermal synthesis of carbon quantum dot
Take the 1.10g vitamin C, be dissolved in 25mL deionized water and 25mL absolute ethyl alcohol mixed solution.Vigorous stirring 2 hours, obtain clear solution.Solution is transferred in reactor, under 180 ℃, after reaction 4h, obtains the dark brown product.With carrene, product being extracted, is the 1000 dialysis membranes purifying of being dialysed by obtained upper strata water through molecular weight, finally obtains the yellow solution that contains the carbon quantum dot.The upper transfer characteristic of prepared carbon quantum dot is shown in that Fig. 1, under different exciting lights, launches different fluorescence.
Embodiment 2
According to the preparation method of embodiment 1, the reaction time is 2h, prepares the yellow solution of carbon quantum dot.
According to the preparation method of embodiment 1, reaction temperature is 6h, prepares the yellow solution of carbon quantum dot.
Embodiment 4
According to the preparation method of embodiment 1, reaction temperature is 8h, prepares the yellow solution of carbon quantum dot.
According to the preparation method of embodiment 1, reaction temperature is 140 ℃, prepares the yellow solution of carbon quantum dot.
Embodiment 6
According to the preparation method of embodiment 1, reaction temperature is 200 ℃, prepares the yellow solution of carbon quantum dot.
Embodiment 7: prepare spherical TiO
2nano particle
Butyl titanate, as the titanium source, prepares spherical TiO by sol-gal process
2powder.The 15mL butyl titanate is joined in the 50.7mL absolute ethyl alcohol, then drip 3.6mL iminodiacetic acid (salt) acid solution, then use NaOH and hydrochloric acid solution that above-mentioned pH is adjusted to 7.0, obtain white suspension.At room temperature continue stirring until and mix, dropwise add subsequently the 20ml absolute ethyl alcohol, continue to stir 30min, collect the white depositions generated and repeatedly wash by absolute ethyl alcohol and deionized water, drying, under 300 ℃, calcining is 2 hours, makes spherical TiO
2nano particle.The ESEM of this nano particle as shown in Figure 2, the TiO of formation
2particle is spherical, and diameter is about 550nm.
Embodiment 8
According to the preparation method of embodiment 7, pH is adjusted to 6.0, prepares spherical TiO
2nano particle.
Embodiment 9
According to the preparation method of embodiment 7, pH is adjusted to 8.0, prepares spherical TiO
2nano particle.
Embodiment 10:TiO
2the preparation method of/CQDs composite Nano photochemical catalyst
Spherical TiO by synthesized in embodiment 2
2in nano particle and embodiment 1, the CQDs solution of synthesized is 1:0.1 mix and blend 30min in molar ratio, and under 80 ℃, dry 12h, obtain TiO
2/ CQDs composite Nano photochemical catalyst.The electromicroscopic photograph of the photochemical catalyst obtained as shown in Figure 3, its pattern and size with compound before compare change not obvious.Compound front and back photochemical catalyst in embodiment 2 and 3 is carried out to the de-absorption representation of nitrogen, and as Fig. 4, wherein: compound front specific area is 193.7m
3/ g, compound is 206.5m afterwards
3/ g; The TiO of synthesized of the present invention
2/ CQDs and TiO
2the UV-vis DRS spectrogram of sample, as Fig. 5.
Embodiment 11
According to the preparation method of embodiment 10, wherein baking temperature is 60 ℃, obtains TiO
2/ CQDs composite Nano photochemical catalyst.
Embodiment 12
According to the preparation method of embodiment 10, wherein baking temperature is 100 ℃, obtains TiO
2/ CQDs composite Nano photochemical catalyst.
Embodiment 13
According to the preparation method of embodiment 10, wherein mol ratio is 1:0.05, obtains TiO
2/ CQDs composite Nano photochemical catalyst.
Embodiment 14
According to the preparation method of embodiment 10, wherein mol ratio is 1:0.15, obtains TiO
2/ CQDs composite Nano photochemical catalyst.
Embodiment 15: the investigation method of composite Nano photochemical catalyst visible light catalysis activity
Use the methyl blue dyestuff as degraded object of the present invention, specific operation process is as follows: get TiO described in 0.05g embodiment 10
2/ CQDs composite Nano photochemical catalyst joins in the 100ml methylene blue solution that concentration is 20mg/L, by its ultrasonic dispersion 10min, catalyst is dispersed in reaction solution, form suspension, be transferred to subsequently camera bellows and stir 30min, make solution reach the adsorption/desorption balance.At this moment, sampling is as the photocatalytic degradation initial concentration.Then reaction vessel is placed under the irradiation of xenon lamp to (with optical filter elimination 420nm wavelength following ultraviolet light) and carries out the photocatalytic degradation reaction.Get at set intervals certain volume solution in course of reaction and get supernatant liquor after centrifugation, measure its absorbance.Calculate the methylene blue degradation rate.Photocatalytic degradation efficiency figure, as Fig. 6.The present invention contrasts the catalytic degradation performance of the photochemical catalyst of compound front and back, and as can be seen from the figure, the catalyst after compound has higher catalytic activity in visible-range.
Embodiment 16
According to the investigation method of embodiment 15, use composite Nano photochemical catalyst in embodiment 13, investigate its photocatalysis performance.
Embodiment 17
According to the investigation method of embodiment 15, use composite Nano photochemical catalyst in embodiment 14, investigate its photocatalysis performance.
Claims (10)
1. a carbon quantum dot solution synthetic by hydro-thermal method prepares the method for composite Nano photochemical catalyst, and its feature comprises the following steps:
Step 1: prepare the carbon quantum dot solution
(1) vitamin c solution of the solution allocation 0.125M that the absolute ethyl alcohol that is 1:1 by volume ratio and deionized water mix, obtain the transparent reaction precursor solution;
(2) precursor solution is joined in reactor, the reaction time is 2h～8h, and reaction temperature is 140 ℃～200 ℃, obtains the dark brown product;
(3) add carrene in above-mentioned dark brown product, repeatedly extraction, get upper water solution and carry out separation and purification through dialysis membrane, obtains the carbon quantum dot solution;
Step 2: prepare the composite Nano photochemical catalyst
(1) butyl titanate is joined in absolute ethyl alcohol, then drip the iminodiacetic acid (salt) acid solution, obtain mixed solution, wherein the volume ratio of butyl titanate, absolute ethyl alcohol, iminodiacetic acid is 17:57.5:4.125, then using NaOH and hydrochloric acid solution to regulate the pH value to above-mentioned mixed solution is 6.0～8.0, obtains white suspension;
(2) above-mentioned white suspension is stirred, dropwise add subsequently excessive absolute ethyl alcohol also to stir, collect the white depositions generated and wash drying by absolute ethyl alcohol and deionized water, under 300 ℃～500 ℃, calcining is 2 hours, makes TiO
2spherical nanoparticle;
(3) by TiO
2the carbon quantum dot solution that spherical nanoparticle and step 1 obtain is 1:0～0.15 mix and blend in molar ratio, and under 60～100 ℃, drying is 12 hours, obtains the composite Nano photochemical catalyst.
2. method according to claim 1, it is characterized in that: the reaction time in described reactor is 4h.
3. method according to claim 1 and 2, it is characterized in that: the reaction temperature in described reactor is 180 ℃.
4. method according to claim 1 and 2, it is characterized in that: in step 2, pH is 7.0.
5. method according to claim 3, it is characterized in that: in step 2, pH is 7.0.
6. according to claim 1,2 or 5 described methods, it is characterized in that: in step 2, baking temperature is 80 ℃.
7. the preparation method of spherical composite photo-catalyst according to claim 3, it is characterized in that: in step 2, baking temperature is 80 ℃.
8. the preparation method of spherical composite photo-catalyst according to claim 4, it is characterized in that: in step 2, baking temperature is 80 ℃.
9. according to claim 1,2,5,7 or 8 described methods, it is characterized in that: the mol ratio of the TiO2 spherical nanoparticle described in step 2 and carbon quantum dot solution is 1:0.1.
10. method according to claim 6, it is characterized in that: the mol ratio of the TiO2 spherical nanoparticle described in step 2 and carbon quantum dot solution is 1:0.1.
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