CN103127947A - Construction method of phosphoric acid functionalized carbon nanometer pipe-titanium dioxide composite nanometer photocatalyst - Google Patents
Construction method of phosphoric acid functionalized carbon nanometer pipe-titanium dioxide composite nanometer photocatalyst Download PDFInfo
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Abstract
The invention discloses a construction method of a phosphoric acid functionalized carbon nanometer pipe-titanium dioxide composite nanometer photocatalyst, and relates to a construction method of a photocatalyst. The construction method provided by the invention solves the technical problem that the activity of the existing carbon nanometer pipe and titanium dioxide composite photocatalyst is poor. The method comprises the following steps of: firstly, preparing a phosphoric acid functionalized carbon nanometer pipe; secondly, adding the phosphoric acid functionalized carbon nanometer pipe in butyl titanate, then adding a mixed liquid in toluene, and obtaining an organic phase; and thirdly, placing the organic phase in a reaction tank, then placing the reaction tank in a high pressure reaction kettle with distilled water, reacting, cooling to the room temperature, taking a paste body in the reaction tank, distilling the paste body, drying, grinding, and obtaining the phosphoric acid functionalized carbon nanometer pipe-titanium dioxide composite nanometer photocatalyst. The construction method provided by the invention utilizes phosphoric acid to realize functionalization on the carbon nanometer pipe, improves the oxygen adsorption capacity of the carbon nanometer pipe, and further enhances the capacity of promoting a photon-generated carrier to be separated and react of the carbon nanometer pipe in a compound system. The construction method provided by the invention belongs to the field of preparation of photocatalysts.
Description
Technical field
The present invention relates to a kind of construction method of photochemical catalyst.
Background technology
To have the photochemical catalytic oxidation ability strong due to it for titanium dioxide, and nontoxic cheapness prepares the study hotspot that the characteristics such as simple always are photochemical catalyst.But higher this bottleneck of its photo-generated carrier recombination probability has seriously limited the further raising of its performance.Carried out extensive work for this bottleneck people, wherein the carbon-based material take CNT as representative becomes the focus that people pay close attention to.Researchers had been carried out a large amount of about CNT and the compound work of titanium dioxide, comprising the exploitation of synthetic method and the research of active mechanism etc. in the last few years in succession.In existing achievement in research, although synthetic method is numerous, due to complex process, appointed condition is harsh, and the Product Activity of gained is poor etc., and factor makes people still constantly research is effectively simple, is applicable to the synthetic method of suitability for industrialized production.Mechanism of action people for the CNT in CNT-titanium dioxide complex system have also carried out extensive work, but under the light-catalyzed reaction system, and CNT seldom is mentioned as the simple and effective method of modifying in electronics and oxygen reaction district.
Summary of the invention
The objective of the invention is the technical problem for the poor activity that solves existing CNT and titanium dioxide composite photocatalyst, the construction method of a kind of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst is provided.
The construction method of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst carries out according to following steps:
One, CNT is joined in red fuming nitric acid (RFNA), refluxed 4～8 hours under the condition of 120 ℃～140 ℃, centrifugal, the washing, the oven dry, obtain the acidifying CNT;
Two, the acidifying CNT is joined in the phosphate aqueous solution that concentration is 0.1mol/L～1.0mol/L, stir 20min～60min, ultrasonic 30min～60min, then centrifugal, washing, drying, roasting, grinding obtain the phosphoric acid functionalized CNT;
In step 2, the mass ratio of acidifying CNT and phosphate aqueous solution is 1: 20～30;
Three, 0.05～0.5 mass parts phosphoric acid functionalized CNT is joined in 40～60 mass parts butyl titanates, then according to first stir 10min～30min the order of more ultrasonic 10min～30min repeat 2～5 times, then mixed liquor is joined in the toluene of 30～50 mass parts again, stir 10min～30min, obtain organic phase;
Four, organic phase is put into reaction tank, and then reaction tank is put into the autoclave that fills distilled water, react 4h～8h under the condition of 110 ℃～130 ℃, then be cooled to room temperature, take out the lotion in reaction tank, 120 ℃～130 ℃ distillations, then dry, grinding, namely get phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst with lotion.The mass fraction of the described red fuming nitric acid (RFNA) of step 1 is 65%.
This patent not only utilizes phosphoric acid to realize functionalization to CNT, significantly improved the effect of CNT in this compound system, and further developed the hydrolysis-solvent-thermal method that is separated, make it be successfully applied to constructing of CNT-titanium dioxide complex, finally obtained the composite photo-catalyst that photocatalytic activity is higher and universality is strong.
Utilize phosphoric acid to realize functionalization to CNT in the present invention, improved the adsorption capacity of CNT to oxygen, and then strengthened the ability that in the compound system, the promotion photo-generated carrier of CNT separates, reacts.Develop the hydrolysis-solvent-thermal method that is separated, successfully solved the dispersion of CNT in organic phase in the building-up process, and selected suitable reaction temperature, realized the effectively compound of CNT and titanium dioxide.Method reaction condition gentleness, the technique that the present invention synthesizes phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst is simple, resulting catalyst performance is excellent, is fit to suitability for industrialized production.
Utilize the present invention to synthesize phosphoric acid functionalized CNT-titanium dioxide, CNT can generate through pernitric acid acidifying rear surface a certain amount of-COOH and-OH isopolarity group, can make the acid enhancing of carbon nano tube surface by the phosphoric acid functionalized process again, thereby therefore be more conducive to the absorption of oxygen is promoted the oxygen trapped electrons.In the complex building-up process, the phosphoric acid functionalized CNT Uniform Dispersion in nonpolar organic phase that makes the surface be polarity is to realize CNT and the effective compound key of titanium dioxide.Utilize titanium source-butyl titanate first the phosphoric acid functionalized CNT to be coated in advance, realize the non-polarization of phosphoric acid functionalized carbon nano tube surface, thereby solved the scattering problem of organic phase, guaranteed that simultaneously itself and titanium dioxide are effectively compound to the full extent.
Based on above analysis, phosphoric acid functionalized CNT-titanium dioxide that this invention obtains has higher photo-generated carrier separation, reaction efficiency, is comparatively desirable photochemical catalyst.
Description of drawings
Fig. 1 is the XPS figure of the P2p of acidifying CNT and phosphoric acid functionalized CNT in test one, in figure, a represents the XPS figure of the P2p of acidifying CNT, b represents the CNT of 0.1mol/L phosphoric acid solution functionalization, c represents the CNT of 0.5mol/L phosphoric acid solution functionalization, and d represents the CNT of 1.0mol/L phosphoric acid solution functionalization;
Fig. 2 is the O of phosphoric acid functionalized CNT in test one
2-TPD figure, in figure, a represents the CNT of 0.5mol/L phosphoric acid solution functionalization, b represents the acidifying CNT;
Fig. 3 is the XRD figure of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst in test one, in figure, a represents to adopt the XRD figure of the synthetic phosphoric acid functionalized CNT-titanium dioxide composite photocatalyst of 0.1mol/L phosphoric acid solution, b represents to adopt the XRD figure of the synthetic phosphoric acid functionalized CNT-titanium dioxide composite photocatalyst of 0.5mol/L phosphoric acid solution, c represents to adopt the XRD figure of the synthetic phosphoric acid functionalized CNT-titanium dioxide composite photocatalyst of 0.1mol/L phosphoric acid solution, d represents the XRD figure of CNT-titanium dioxide composite photocatalyst, e represents the XRD figure of titanium dioxide,
Fig. 4 is the TEM figure of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst in test two;
Fig. 5 is the partial enlarged drawing of Fig. 4;
Fig. 6 is the degradation rate column diagram of phosphoric acid functionalized CNT-titanium dioxide composite Nano photocatalyst for degrading rhodamine B aqueous solution in test one, in figure, a represents the photocatalytic activity of P25 titanium dioxide, b represents the photocatalytic activity of titanium dioxide, c represents the photocatalytic activity of CNT-titanium dioxide composite photocatalyst, d represents to adopt the photocatalytic activity of the synthetic phosphoric acid functionalized CNT-titanium dioxide composite photocatalyst of 0.1mol/L phosphoric acid solution, e represents to adopt the photocatalytic activity of the synthetic phosphoric acid functionalized CNT-titanium dioxide composite photocatalyst of 0.5mol/L phosphoric acid solution, f represents to adopt the photocatalytic activity of the synthetic phosphoric acid functionalized CNT-titanium dioxide composite photocatalyst of 1.0mol/L phosphoric acid solution,
Fig. 7 is the degradation rate column diagram of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst catalytic degradation phenol solution in test two, in figure
The total photocatalytic degradation efficiency of expression catalyst Pyrogentisinic Acid,
Expression catalyst Pyrogentisinic Acid's adsorption efficiency, the photocatalytic degradation efficiency of 1 expression titanium dioxide, the adsorption efficiency of 2 expression titanium dioxide, the photocatalytic degradation efficiency of 3 expression CNT-titanium dioxide composite photocatalysts, the adsorption efficiency of 4 expression CNT-titanium dioxide composite photocatalysts, the photocatalytic degradation efficiency of 5 expression phosphoric acid functionalized CNT-titanium dioxide composite photocatalysts, the adsorption efficiency of 6 expression phosphoric acid functionalized CNT-titanium dioxide composite photocatalysts.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the construction method of present embodiment phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst carries out according to following steps:
One, CNT is joined in red fuming nitric acid (RFNA), refluxed 4～8 hours under the condition of 120 ℃～140 ℃, centrifugal, the washing, the oven dry, obtain the acidifying CNT;
Two, the acidifying CNT is joined in the phosphate aqueous solution that concentration is 0.1mol/L～1.0mol/L, stir 20min～60min, ultrasonic 30min～60min, then centrifugal, washing, drying, roasting, grinding obtain the phosphoric acid functionalized CNT;
In step 2, the mass ratio of acidifying CNT and phosphate aqueous solution is 1: 20～30;
Three, 0.05～0.5 mass parts phosphoric acid functionalized CNT is joined in 40～60 mass parts butyl titanates, then according to first stir 10min～30min the order of more ultrasonic 10min～30min repeat 2～5 times, then mixed liquor is joined in the toluene of 30～50 mass parts again, stir 10min～30min, obtain organic phase;
Four, organic phase is put into reaction tank, and then reaction tank is put into the autoclave that fills distilled water, react 4h～8h under the condition of 110 ℃～130 ℃, then be cooled to room temperature, take out the lotion in reaction tank, 120 ℃～130 ℃ distillations, then dry, grinding, namely get phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst with lotion.
The specific embodiment two: present embodiment is different from the specific embodiment one is that the mass fraction of the described red fuming nitric acid (RFNA) of step 1 is 65%.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different from one of the specific embodiment one or two is to reflux 5 hours under the condition of 130 ℃ in step 1.Other is not identical with one of the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three is that the concentration of phosphate aqueous solution in step 2 is 0.5mol/L.Other is identical with one of specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four is that in step 2, the mass ratio of acidifying CNT and phosphate aqueous solution is 1: 25.Other is identical with one of specific embodiment one to four.
The specific embodiment six: what present embodiment was different from one of specific embodiment one to five is in step 3,0.3 mass parts phosphoric acid functionalized CNT to be joined in 50 mass parts butyl titanates.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different from one of specific embodiment one to six is in step 3, mixed liquor to be joined in the toluene of 40 mass parts again, stirs 20min.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different from one of specific embodiment one to seven is to react 5h in step 4 under the condition of 120 ℃.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different from one of specific embodiment one to eight is to react 7h in step 4 under the condition of 115 ℃.Other is identical with one of specific embodiment one to eight.
The specific embodiment ten: present embodiment is different from one of specific embodiment one to nine be in step 4 with lotion 125 ℃ of distillations.Other is identical with one of specific embodiment one to nine.
Adopt following verification experimental verification effect of the present invention:
Test one:
The construction method of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst carries out according to following steps:
One, the 2g CNT is joined in the 60mL red fuming nitric acid (RFNA), refluxed 4～8 hours under the condition of 120 ℃～140 ℃, centrifugal, the washing, the oven dry, obtain the acidifying CNT;
Two, 0.5g acidifying CNT is joined in the phosphate aqueous solution that 20mL concentration is 0.1mol/L～1.0mol/L, stir 30min, ultrasonic 30min, then centrifugal, washing, drying, roasting, grinding obtain the phosphoric acid functionalized CNT;
In step 2, the mass ratio of acidifying CNT and phosphate aqueous solution is 1: 23;
Three, 0.5g phosphoric acid functionalized CNT is joined in the 45g butyl titanate, then according to first stir 20min the order of more ultrasonic 20min repeat 3 times, then mixed liquor is joined in the toluene of 54.5g again, stir 20min, obtain organic phase;
Four, organic phase is put into reaction tank, and then reaction tank is put into the autoclave that fills distilled water, react 6h under the condition of 120 ℃, then be cooled to room temperature, take out the lotion in reaction tank, 120 ℃ of distillations, then dry, grinding, namely get phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst with lotion.
The XPS figure of the P2p of the phosphoric acid functionalized CNT that obtains in this test as shown in Figure 1, has realized that successfully the phosphoric acid functionalized of CNT and modification amount are controlled; The O of phosphoric acid functionalized CNT
2-TPD figure, as shown in Figure 2, the phosphoric acid functionalized CNT is to O
2Adsorption capacity far above the acidifying CNT; Shown in Figure 3, the size of the introducing of phosphoric acid functionalized CNT to TiO 2 particles, the crystalline phase composition does not make a significant impact.
Phosphoric acid functionalized CNT-the titanium dioxide that obtains in this test carries out according to the following steps to the ultraviolet-visible photocatalytic degradation of the rhodamine B aqueous solution: adopt the spherical xenon lamp of 150W as radiation source, the aqueous solution of the rhodamine B of 100ml 20mg/L is placed in the 150ml glass reactor, add 0.1g phosphoric acid functionalized CNT-titanium dioxide composite nano-catalyst, be positioned over apart from xenon lamp 10cm place, keep the reaction solution equalization of concentration with magnetic agitation in course of reaction.First secretly adsorb 0.5h before illumination, then begin light reaction, and the 10ml that takes a sample after reaction beginning 1h.Measure the concentration of photocatalysis front and back rhodamine B solution (its maximum absorption wavelength is as 553nm) take ultraviolet-visible spectrophotometer;
The ultraviolet-visible photocatalytic degradation of phenol solution carries out according to the following steps: adopt the spherical xenon lamp of 150W as radiation source, the aqueous solution of the phenol of 100ml 15mg/L is placed in the 150ml glass reactor, add 0.1g phosphoric acid functionalized CNT-titanium dioxide composite nano-catalyst, be positioned over apart from xenon lamp 10cm place, keep the reaction solution equalization of concentration with magnetic agitation in course of reaction.First secretly adsorb 0.5h before illumination, then begin light reaction, and the 10ml that takes a sample after reaction beginning 1h, with the colour developing of 4-AA method, mensuration concentration.Measure the concentration of photocatalysis front and back phenol solution (after its colour developing, maximum absorption wavelength is as 510nm) take ultraviolet-visible spectrophotometer.
Test two:
The construction method of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst carries out according to following steps:
One, the 2g CNT is joined in the 60mL red fuming nitric acid (RFNA), refluxed 4～8 hours under the condition of 120 ℃～140 ℃, centrifugal, the washing, the oven dry, obtain the acidifying CNT;
Two, 0.5g acidifying CNT is joined in the phosphate aqueous solution that 20mL concentration is 0.5mol/L, stir 30min, ultrasonic 30min, then centrifugal, washing, drying, roasting, grinding obtain the phosphoric acid functionalized CNT;
In step 2, the mass ratio of acidifying CNT and phosphate aqueous solution is 1: 23;
Three, 0.5g phosphoric acid functionalized CNT is joined in the 45g butyl titanate, then according to first stir 20min the order of more ultrasonic 20min repeat 3 times, then mixed liquor is joined in the toluene of 54.5g again, stir 20min, obtain organic phase;
Four, organic phase is put into reaction tank, and then reaction tank is put into the autoclave that fills distilled water, react 6h under the condition of 120 ℃, then be cooled to room temperature, take out the lotion in reaction tank, 120 ℃ of distillations, then dry, grinding, namely get phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst with lotion.
The TEM figure of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst as shown in Figure 4, can find out that product is compound better.
The degradation rate column diagram of the phosphoric acid functionalized CNT that above test obtains-optically catalytic TiO 2 rhodamine B degradation and phenol solution, as Fig. 6, shown in Figure 7, no matter be coloured rhodamine B or colourless phenol, the introducing of phosphoric acid functionalized CNT can improve the photocatalytic activity of complex, and higher than the activity of CNT-titanium dioxide.
Claims (10)
1. the construction method of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst is characterized in that the construction method of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst carries out according to following steps:
One, CNT is joined in red fuming nitric acid (RFNA), refluxed 4～8 hours under the condition of 120 ℃～140 ℃, centrifugal, the washing, the oven dry, obtain the acidifying CNT;
Two, the acidifying CNT is joined in the phosphate aqueous solution that concentration is 0.1mol/L～1.0mol/L, stir 20min～60min, ultrasonic 30min～60min, then centrifugal, washing, drying, roasting, grinding obtain the phosphoric acid functionalized CNT;
In step 2, the mass ratio of acidifying CNT and phosphate aqueous solution is 1: 20～30;
Three, 0.05～0.5 mass parts phosphoric acid functionalized CNT is joined in 40～60 mass parts butyl titanates, then according to first stir 10min～30min the order of more ultrasonic 10min～30min repeat 2～5 times, then mixed liquor is joined in the toluene of 30～50 mass parts again, stir 10min～30min, obtain organic phase;
Four, organic phase is put into reaction tank, and then reaction tank is put into the autoclave that fills distilled water, react 4h～8h under the condition of 110 ℃～130 ℃, then be cooled to room temperature, take out the lotion in reaction tank, lotion is distilled under 120 ℃～130 ℃, and then dry, grinding, namely get phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst.
2. the construction method of phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1, the mass fraction that it is characterized in that the described red fuming nitric acid (RFNA) of step 1 is 65%.
3. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2, is characterized in that refluxing 5 hours under the condition of 130 ℃ in step 1.
4. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2, the concentration that it is characterized in that phosphate aqueous solution in step 2 is 0.5mol/L.
5. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2 is characterized in that in step 2, the mass ratio of acidifying CNT and phosphate aqueous solution is 1: 25.
6. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2, is characterized in that in step 3,0.3 mass parts phosphoric acid functionalized CNT being joined in 50 mass parts butyl titanates.
7. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2, is characterized in that in step 3, mixed liquor being joined in the toluene of 40 mass parts again, stirs 20min.
8. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2, is characterized in that reacting 5h in step 4 under the condition of 120 ℃.
9. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2, is characterized in that reacting 7h in step 4 under the condition of 115 ℃.
10. the construction method of described phosphoric acid functionalized CNT-titanium dioxide composite Nano photochemical catalyst according to claim 1 and 2 is characterized in that in step 4 lotion 125 ℃ of distillations.
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| CN109225310A (en) * | 2018-11-20 | 2019-01-18 | 安徽元琛环保科技股份有限公司 | The preparation method of titanium dioxide hollow nanotube, titanium dioxide hollow nanotube and using it as the preparation method of the middle low-temperature denitration catalyst of carrier |
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| CN1953935A (en) * | 2004-05-14 | 2007-04-25 | 索尼德国有限责任公司 | Composite materials comprising carbon nanotubes and metal carbonates |
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| CN1953935A (en) * | 2004-05-14 | 2007-04-25 | 索尼德国有限责任公司 | Composite materials comprising carbon nanotubes and metal carbonates |
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| TOBY SAINSBURY ET AL: "Templated Assembly of Semiconductor and Insulator Nanoparticles at the Surface of Covalently Modified Multiwalled Carbon Nanotubes", 《CHEM. MATER.》, vol. 16, no. 19, 27 August 2004 (2004-08-27) * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109225310A (en) * | 2018-11-20 | 2019-01-18 | 安徽元琛环保科技股份有限公司 | The preparation method of titanium dioxide hollow nanotube, titanium dioxide hollow nanotube and using it as the preparation method of the middle low-temperature denitration catalyst of carrier |
| CN109225310B (en) * | 2018-11-20 | 2021-06-29 | 安徽元琛环保科技股份有限公司 | Preparation method of titanium dioxide hollow nanotube, titanium dioxide hollow nanotube and preparation method of medium-low temperature denitration catalyst using titanium dioxide hollow nanotube as carrier |
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