CN104841470A - Composite titanium dioxide nano-sheet photocatalyst, preparation method and applications thereof - Google Patents
Composite titanium dioxide nano-sheet photocatalyst, preparation method and applications thereof Download PDFInfo
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Abstract
The present invention relates to a composite titanium dioxide nano-sheet photocatalyst, a preparation method and applications thereof, wherein the composite titanium dioxide nano-sheet photocatalyst comprises, by weight, 0.01-0.02% of carbon quantum dots, 39.44-70.73% of carbon nitride, and 29.25-60.55% of titanium dioxide. According to the present invention, titanium tetraisopropanolate and melamine are respectively adopted as the titanium source and the nitrogen source, and the precursor synthesis method is used to compound the titanium dioxide, the carbon nitride and the carbon quantum dots, wherein the carbon quantum dot mass content is extremely low while the high photocatalytic activity is provided, and the product can be used in organic wastewater treatment and hydrogen production through water photodecomposition.
Description
Technical field
The invention belongs to photocatalysis technology field, be specifically related to a kind of compound titanium dioxide nanosheet photocatalyst and its preparation method and application.
Background technology
In recent years, because of the impact of PM2.5, metropolitan air pollution index (AQI) has become the focus that resident pays close attention to deeply, and the physical and mental health of people in serious threat, and indoor environmental quality has caused extensively to be paid attention to and pay close attention to, and becomes social hotspots gradually.Photocatalysis is surrounding purifying material the safest and the cleanest in the world at present, extensively use in regions such as America and Europe and Japan, Korea S, U.S.'s aerospace station cleaning project, oil pollution at sea degraded engineering and Japanese public transport company sterilization engineering all make photoactivation process.
Many-sided research is carried out to titanium dioxide optical catalyst catalytic activity and adsorptivity problem, comprising many levels such as Study on influencing factors, study mechanism, performance studies, each research level has achieved a lot of achievement in research.
The research of the superstructure that the preparation of titanium dioxide nano material and character mainly concentrate on one dimension, two peacekeeping one dimensions are assembled.But two-dimensional nanostructure is studied less.The patent No. is that the Chinese patent of CN201210462406.2 reports a kind of compound titanium dioxide nanotube array photocatalyst and preparation method thereof, compound titanium dioxide nanotube array photocatalyst prepared by the method, simulated solar irradiation is to 2 of 10mg/L, 4-dichlorphenoxyacetic acid its carry out photocatalysis, 3 hours efficiency of degrading is only 80%.
The catalytic activity selecting efficient method to improve photochemical catalyst is largely a complicated process, and the technology that photocatalytic activity improves has 5 kinds at least: element doping, semiconductors coupling, noble metal loading, the control etc. of the sensitization of organic matter fuel and size and pattern.Wherein element doping and semiconductors coupling are 2 kinds of main modification mode.
Summary of the invention
For the above-mentioned problems in the prior art, the object of the present invention is to provide a kind of compound titanium dioxide nanosheet photocatalyst and its preparation method and application, it is carbon quantum dot, carbonitride and titanium dioxide composite photocatalyst, this catalyst has high light catalytic efficiency, effectively can reduce the energy cost of decomposition water, and preparation method is simple, this catalyst is in visible region, make full use of solar energy, to the organic pollution in organic wastewater, as rhodamine B, carry out photocatalysis treatment, there is the speed of degraded and the high feature of efficiency.
The compound titanium dioxide nanosheet photocatalyst of described one, it is characterized in that for carbon quantum dot, carbonitride and titanium dioxide composite photocatalyst, the weight percentage of described carbon quantum dot, carbonitride and titanium dioxide is: carbon quantum dot 0.01 ~ 0.02%, carbonitride 39.44 ~ 70.73%, titanium dioxide 29.25 ~ 60.55%.。
The preparation method of described a kind of compound titanium dioxide nanosheet photocatalyst, is characterized in that comprising the steps:
1) titanium dioxide nanoplate of two-dimensional sheet structure is prepared
Concentrated hydrochloric acid and isopropyl titanate mix by a in flask, stir the yellow solution that 15 ~ 20min obtains clarifying;
B configures P
123with absolute ethyl alcohol mixed liquor, this mixed liquor is added in the yellow solution of the clarification that step a) obtains, stir 28-32min, obtain mixed solution;
C, by the mixed solution in step b) and ethylene glycol mixing, after stirring, puts into autoclave;
The autoclave of step c) is placed in air dry oven and places 20h at 120 DEG C by d, uses absolute ethanol washing afterwards 3 ~ 5 times, puts into vacuum drying chamber 78-82 DEG C, and 2.5-3.5h is dried, and obtains preliminary solid product;
E) by the solid product that tentatively the obtains tube furnace roasting 2h at 500 ~ 550 DEG C, then Temperature fall is to room temperature, obtains the carbon dioxide nanometer sheet of white two-dimensional sheet structure;
2) carbon quantum dot of dilute with water 10g/L obtains the carbon quantum dot solution of 10 ~ 20mg/L;
3) titanium dioxide nanoplate and the melamine of getting the two-dimensional sheet structure of step 1) take mass ratio as 1:2 ~ 10 mixed liquors that obtain soluble in water, the carbon quantum dot solution of mixed liquor and 10 ~ 20mg/L is mixed with the volume ratio of 3 ~ 4:1, stirs 5-7h at 60 ~ 70 DEG C;
4) solution that step 3) obtains is placed in revolve steam instrument, 80 ~ 83 DEG C revolve steaming, then put into air dry oven and dry 10-15h at 100 DEG C, obtain white powder;
5) dried white powder in step 4) is scraped, be placed in silica crucible, compacting, put into tube furnace, air flow is 10 ~ 15 ml/min, 550 DEG C, roasting 10 ~ 30min, naturally be down to room temperature, obtain the compound titanium dioxide nanoplate of khaki one, wherein the content of titanium dioxide is 29.25 ~ 60.55%.
The preparation method of described a kind of compound titanium dioxide nanosheet photocatalyst, is characterized in that the volume ratio of concentrated hydrochloric acid and isopropyl titanate in step 1) is 1:3 ~ 4.
The preparation method of described a kind of compound titanium dioxide nanosheet photocatalyst, is characterized in that P in step 1)
123be 1:14 ~ 16 with the mass ratio of absolute ethyl alcohol.
The preparation method of described a kind of compound titanium dioxide nanosheet photocatalyst, is characterized in that the mixed solution of the step b) in step 1) and ethylene glycol volume ratio are 1:8 ~ 10.
The preparation method of described a kind of compound titanium dioxide nanosheet photocatalyst, is characterized in that the carbon dioxide nanometer sheet of the two-dimensional sheet structure described in step 3) and the mass ratio that feeds intake of melamine are 1:1 ~ 10.
The preparation method of described a kind of compound titanium dioxide nanosheet photocatalyst, it is characterized in that the carbon dioxide nanometer sheet of the two-dimensional sheet structure described in step 3) and the carbon quantum dot liquor capacity ratio of melamine mixed liquor and 10 ~ 20mg/L are 3 ~ 4:1, mixing time is 6h.
The preparation method of described a kind of compound titanium dioxide nanosheet photocatalyst, it is characterized in that putting in step 4) air dry oven drying time is 12h.
The application of described a kind of compound titanium dioxide nanosheet photocatalyst in treatment of Organic Wastewater and photodissociation aquatic products hydrogen.
By adopting above-mentioned technology, compared with prior art, beneficial effect of the present invention is:
1) the present invention is respectively titanium source and nitrogenous source with isopropyl titanate, melamine, by precursor synthesis method by titanium dioxide, carbonitride and carbon quantum dot compound, the material carbon quantum dot of compound, carbonitride and titanium dioxide are all sufficient on the earth and cheapness, do not use noble metal, greatly reduce experimental cost;
2) simple, the mild condition of the preparation method of catalyst of the present invention, low for equipment requirements, convenient post-treatment;
3) catalyst that the present invention obtains reacts for water Photocatalyzed Hydrogen Production, its efficiency improves greatly, light degradation organic matter speed also than comparatively fast, because the overpotential of carrying out Water oxidize reaction is in the presence of a catalyst lower, reaction is more easily occurred, effectively reduces the energy cost of decomposition water.
Detailed description of the invention
The weight ratio that the present invention is directed to titanium dioxide nanoplate and melamine has carried out a serial case study on implementation.
The weight ratio that the present invention is directed to titanium dioxide nanoplate and melamine has carried out a serial case study on implementation.
Case study on implementation one:
Configuration quality is than the P for 1:14
123with absolute ethyl alcohol mixed liquor, the mixed liquor obtained is added in the concentrated hydrochloric acid that volume ratio is 1:3 and isopropyl titanate mixed liquor, stir 30min.Get above-mentioned solution and ethylene glycol that volume ratio is 1:8, mix and add in autoclave, at 120 DEG C, reaction 20h, afterwards by the absolute ethanol washing 4 times of solid product in still, put into vacuum drying chamber 80 DEG C, 3h is dried, and obtains the titanium dioxide nanoplate of white.Get 100mg titanium dioxide nanoplate at the tube furnace roasting 2h of 500 DEG C, then Temperature fall is to room temperature, obtains white solid.
Take titanium dioxide nanoplate that mass ratio is 1:2 and melamine soluble in water, the carbon quantum dot solution of mixed liquor and 15mg/L is mixed with the volume ratio of 3:1, at 69 ~ 70 DEG C, stir 6h, then solution is carried out at 80 DEG C revolving steaming, after the dry 12h in blower kiln, be placed in tube furnace, purging air, carries out roasting 10min, after cooling at 550 DEG C, obtained described carbon quantum dot, carbonitride and titanium dioxide composite photocatalyst, wherein the mass content of titanium dioxide is 56%.
Case study on implementation two:
Configuration quality is than the P for 1:15
123with absolute ethyl alcohol mixed liquor, the mixed liquor obtained is added in the concentrated hydrochloric acid that volume ratio is 1:3 and isopropyl titanate mixed liquor, stir 30min.Get above-mentioned solution and ethylene glycol that volume ratio is 1:8, mix and add in autoclave, at 120 DEG C, reaction 20h, afterwards by the absolute ethanol washing 3 times of solid product in still, put into vacuum drying chamber 80 DEG C, 3h is dried, and obtains the titanium dioxide nanoplate of white.Get 100mg titanium dioxide nanoplate at the tube furnace roasting 2h of 500 DEG C, then Temperature fall is to room temperature, obtains white solid.
Take titanium dioxide nanoplate that mass ratio is 1:4 and melamine soluble in water, the carbon quantum dot solution of mixed liquor and 12mg/L is mixed with the volume ratio of 3:1, at 69 ~ 70 DEG C, stir 6h, then solution is carried out at 80 DEG C revolving steaming, after the dry 12h in blower kiln, be placed in tube furnace, purging air, carries out roasting 10min, after cooling at 550 DEG C, obtained described carbon quantum dot, carbonitride and titanium dioxide composite photocatalyst, wherein the mass content of titanium dioxide is 51%.
Case study on implementation three:
Configuration quality is than the P for 1:15
123with absolute ethyl alcohol mixed liquor, the mixed liquor obtained is added in the concentrated hydrochloric acid that volume ratio is 1:4 and isopropyl titanate mixed liquor, stir 30min.Get above-mentioned solution and ethylene glycol that volume ratio is 1:10, mix and add in autoclave, at 120 DEG C, reaction 20h, afterwards by the absolute ethanol washing 3 times of solid product in still, puts into vacuum drying chamber 80 DEG C, 3h is dried, and obtains the titanium dioxide nanoplate of white.Get 100mg titanium dioxide nanoplate at the tube furnace roasting 2h of 500 DEG C, then Temperature fall is to room temperature, obtains white solid.
Take titanium dioxide nanoplate that mass ratio is 1:8 and melamine soluble in water, the carbon quantum dot solution of mixed liquor and 13mg/L is mixed with the volume ratio of 3:1, at 65 ~ 69 DEG C, stir 6h, then solution is carried out at 80 DEG C revolving steaming, after the dry 12h in blower kiln, be placed in tube furnace, purging air, carries out roasting 10min, after cooling at 550 DEG C, obtained carbonitride and titanium dioxide composite photocatalyst, wherein the mass content of titanium dioxide is 48%.
Case study on implementation four:
Configuration quality is than the P for 1:15
123with absolute ethyl alcohol mixed liquor, the mixed liquor obtained is added in the concentrated hydrochloric acid that volume ratio is 1:3 and isopropyl titanate mixed liquor, stir 30min.Get above-mentioned solution and ethylene glycol that volume ratio is 1:10, mix and add in autoclave, at 120 DEG C, reaction 20h, afterwards by the absolute ethanol washing 3 times of solid product in still, puts into vacuum drying chamber 80 DEG C, 3h is dried, and obtains the titanium dioxide nanoplate of white.Get 100mg titanium dioxide nanoplate at the tube furnace roasting 2h of 510 DEG C, then Temperature fall is to room temperature, obtains white solid.
Take titanium dioxide nanoplate that mass ratio is 1:10 and melamine soluble in water, the carbon quantum dot solution of mixed liquor and 14mg/L is mixed with the volume ratio of 3:1, at 65 ~ 70 DEG C, stir 6h, then solution is carried out at 80 DEG C revolving steaming, after the dry 12h in blower kiln, be placed in tube furnace, purging air, carries out roasting 10min, after cooling at 550 DEG C, obtained described carbon quantum dot, carbonitride and titanium dioxide composite photocatalyst, wherein the mass content of titanium dioxide is 44%.
Photocatalytic water splitting H2-producing capacity is tested
(1) pre-treatment of catalyst: take 50mg catalyst (TiO
2, P25, case study on implementation 1 ~ 4 composite) be placed in 50 ml beakers, add 35 ml water and 3wt% Pt(15 ml wherein, 0.032 mmol/L H
2ptCl
6), ultrasonic 10 min.
(2) reaction unit: the catalyst of above-mentioned process is poured in reaction inner bag, add 5ml triethanolamine and do sacrifice agent.Inner bag is placed in photochemistry autoclave, notes the gas outlet of four on inwall to align with four gas outlets of reactor, reactor is airtight.
(3) chromatograph operating procedure
1. open argon gas steel cylinder to 0.4 MPa, chromatogram pressure 0.1 MPa.
2. whether the inspection of TCD detector suds ventilates.
3. open chromatogram Power, by reset key.
4. post case temperature 110 DEG C is set, Sample Room 100 DEG C, conductance cell 100 DEG C, waits for that intensification completes.
5. open bridge electric current, detector current 80 mA is set.
(4) catalytic process
1., first with the air 5 times in argon gas row reactor, survey Chromatogram Baseline.
2. open xenon lamp and agitator, react 8 h, get a sample every 1 h.
(5) sample introduction analysis
1. first make that soap-film is long-living enriches foam, slowly open needle-valve, make air-flow in flowmeter rise to 10ml, shut needle-valve immediately.
2. start analytical sampling, analyze duration 10 min.
3. after reaction in 8 hours terminates, close gas-chromatography, close argon gas steel cylinder.
The curve obtained is carried out integration, with 1.01%H
2calibrating gas carries out conversion and obtains hydrogen production potential.Experimental result is shown in Table 1.
As can be seen from Table 1, the compound titanium dioxide nanosheet photocatalyst using the present invention to obtain produces hydrogen as photocatalytic water splitting, with C
3n
4compare with P25, hydrogen-producing speed is all significantly improved.
Claims (9)
1. a compound titanium dioxide nanosheet photocatalyst, it is characterized in that for carbon quantum dot, carbonitride and titanium dioxide composite photocatalyst, the weight percentage of described carbon quantum dot, carbonitride and titanium dioxide is: carbon quantum dot 0.01 ~ 0.02%, carbonitride 39.44 ~ 70.73%, titanium dioxide 29.25 ~ 60.55%.
2. a preparation method for compound titanium dioxide nanosheet photocatalyst, is characterized in that comprising the steps:
1) titanium dioxide nanoplate of two-dimensional sheet structure is prepared
Concentrated hydrochloric acid and isopropyl titanate mix by a in flask, stir the yellow solution that 15-20min obtains clarifying;
B configures P
123with absolute ethyl alcohol mixed liquor, this mixed liquor is added in the yellow solution of the clarification that step a) obtains, stir 28-32min, obtain mixed solution;
C, by the mixed solution in step b) and ethylene glycol mixing, after stirring, puts into autoclave;
The autoclave of step c) is placed in air dry oven and places 20h at 120 DEG C by d, and the absolute ethanol washing 3 ~ 5 times of the reactant in reactor, puts into vacuum drying chamber 78-82 DEG C, and 2.5-3.5h is dried, and obtains preliminary solid product;
E) by the solid product that tentatively the obtains tube furnace roasting 2h at 500 ~ 550 DEG C, then Temperature fall is to room temperature, obtains the carbon dioxide nanometer sheet of white two-dimensional sheet structure;
2) carbon quantum dot of dilute with water 10g/L obtains the carbon quantum dot solution of 10 ~ 20mg/L;
3) titanium dioxide nanoplate and the melamine of getting the two-dimensional sheet structure of step 1) take mass ratio as 1:1 ~ 10 mixed liquors that obtain soluble in water, the carbon quantum dot solution of mixed liquor and 10 ~ 20mg/L is mixed with the volume ratio of 3 ~ 4:1, stirs 5-7h at 60 ~ 70 DEG C;
4) solution that step 3) obtains is placed in revolve steam instrument, 80 ~ 83 DEG C revolve steaming, then put into air dry oven and dry 10-15h at 100 DEG C, obtain white powder;
5) dried white powder in step 4) is scraped, be placed in silica crucible, compacting, put into tube furnace, air flow is 10 ~ 15 ml/min, 550 DEG C, roasting 10 ~ 30min, naturally be down to room temperature, obtain the compound titanium dioxide nanosheet photocatalyst of khaki one, wherein the content of titanium dioxide is 29.25 ~ 60.55%.
3. the preparation method of a kind of compound titanium dioxide nanosheet photocatalyst according to claim 2, is characterized in that the volume ratio of concentrated hydrochloric acid and isopropyl titanate in step 1) is 1:3 ~ 4.
4. the preparation method of a kind of compound titanium dioxide nanosheet photocatalyst according to claim 2, is characterized in that P in step 1)
123be 1:14 ~ 16 with the mass ratio of absolute ethyl alcohol.
5. the preparation method of a kind of compound titanium dioxide nanosheet photocatalyst according to claim 2, is characterized in that the mixed solution of the step b) in step 1) and ethylene glycol volume ratio are 1:8 ~ 10.
6. the preparation method of a kind of compound titanium dioxide nanosheet photocatalyst according to claim 2, is characterized in that the carbon dioxide nanometer sheet of the two-dimensional sheet structure described in step 3) and the mass ratio that feeds intake of melamine are 1:1 ~ 10.
7. the preparation method of a kind of compound titanium dioxide nanosheet photocatalyst according to claim 2, it is characterized in that the carbon dioxide nanometer sheet of the two-dimensional sheet structure described in step 3) and the carbon quantum dot liquor capacity ratio of melamine mixed liquor and 10 ~ 20mg/L are 3 ~ 4:1, mixing time is 6h.
8. the preparation method of a kind of compound titanium dioxide nanosheet photocatalyst according to claim 2, it is characterized in that putting in step 4) air dry oven drying time is 12h.
9. the application of compound titanium dioxide nanosheet photocatalyst in treatment of Organic Wastewater and photodissociation aquatic products hydrogen.
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| CN107837817A (en) * | 2017-11-21 | 2018-03-27 | 华中农业大学 | A kind of carbon point/carbonitride/composite titania material and its preparation method and application |
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