CN104741153A - Device for preparing photocatalysts with visible-light response and preparation method thereof - Google Patents
Device for preparing photocatalysts with visible-light response and preparation method thereof Download PDFInfo
- Publication number
- CN104741153A CN104741153A CN201510074297.0A CN201510074297A CN104741153A CN 104741153 A CN104741153 A CN 104741153A CN 201510074297 A CN201510074297 A CN 201510074297A CN 104741153 A CN104741153 A CN 104741153A
- Authority
- CN
- China
- Prior art keywords
- illumination reaction
- photochemical catalyst
- preparation
- visible light
- reaction device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Catalysts (AREA)
Abstract
The invention discloses a device for preparing photocatalysts with visible-light response and a preparation method thereof. The device comprises an illumination reaction box, a glass-pipeline system, a carrier-gas collecting system and a vacuum device. The preparation method comprises the following steps of: in operation 1, vacuumizing the system, turning on a light source to carry out illumination reaction, and continuously vacuumizing in the reaction process; in operation 2, turning off the vacuum pump and valves, switching on nitrogen gas (carrier gas), opening the valve 8, opening the valve 6 and the valve 7 after the system is full filled with the nitrogen gas, turning on the light source to carry out illumination reaction, and continuously introducing the nitrogen gas in the reaction process; and finally, carrying out centrifugation on the solution left after reaction, drying by a baking oven and grinding, thus obtaining two noble-metal-loaded catalysts with visible-light response. The device and the preparation method disclosed by the invention have the advantages that the switching between the two conditions of vacuum and carrier gas is realized, the response of the photocatalysts to the visible light is improved, and the selective oxidation effect for organic matters is improved.
Description
Technical field
The present invention relates to catalysis material technical field, particularly relate to a kind of sealing photochemical catalyst that is good, preparation visible light-responded better, to the effective catalyst preparing device and method of organic matter selective oxidation.
Background technology
By a kind of reaction of organic substrates high selectivity to target product, commercial synthesis and laboratory synthesis are all had great importance.Along with environmental problem and resource problem day by day become the major issue of restriction social development, how to make the carrying out of industrial production green economy more, become the important directions of research now.How to replace costliness conventional at present and poisonous noble metal catalyst, transition metal complex catalyst, avoid a large amount of strong acid and strong bases conventional in course of reaction, and use the molecular oxygen of inexpensive clean to replace ClO
-, Cl
2etc. poisonous strong oxidizer, realizing the selective oxidation of the organic substrates of eco-friendly, economical and efficient, is the significant problem that researcher both domestic and external warmheartedness solves.
With the photochemical catalyst that titanium dioxide (TiO2) and carbonitride (C3N4) etc. are representative, all receive in pollutant process, photocatalytic water, solar cell etc. and pay attention to widely and study.By there is being separated of electronics and hole after ultraviolet excitation in titanium dioxide, its valence band hole has the oxidizing potential up to 2.7 eV, can the most organic matter of oxidation Decomposition; But under the effect of the hydroxyl radical free radical derived in the hole of strong oxidizing property and hole, most organic matter is all oxidizing to water and carbon dioxide by what cannot suppress, and this limits titanium dioxide greatly in very many-sided application; And the excitation wavelength of titanium dioxide is only accounting for the ultraviolet region of solar spectrum less than 3%, and this constrains the application of titanium dioxide at the energy and economic angle.How to utilize this green oxidation technology of photocatalysis, use photochemical catalyst to replace noble metal/transition metal complex catalyst, replace ClO with the molecular oxygen of inexpensive clean
-, Cl
2, Cr (VI) etc. makes oxidant, realizing the high-selectivity oxidation of alcohol in a mild condition, is the target that domestic and international researcher pursues always.
By photocatalyst modified with noble metals, the activity of photochemical catalyst and visible light-responded can be improved.The method that carried noble metal is conventional mainly contains: sodium borohydride reduction, logical nitrogen deoxidizing etc., wherein, and NaHB
4easily residual, and then affect the oxidability of photochemical catalyst; Logical nitrogen deoxygenation is not easy to operate.In addition, vacuum environment also can realize the load of noble metal, but mutually deserved device is few, and conventional vacuum device utilizes difficulty.
Chinese patent publication No. CN102962078A, date of publication on March 13rd, 2013, name is called a kind of visible light-responded photochemical catalyst and preparation method thereof, this application case discloses a kind of visible light-responded photochemical catalyst and preparation method thereof, by analytically pure silver nitrate, cupric oxide, niobium pentaoxide, tantalum pentoxide according to AgCuNb
1-xta
xo
4(wherein 0≤x≤1) is put in autoclave after weighing, and take potassium hydroxide as mineralizer, adopts hydro-thermal synthesis process to obtain the composite oxides with good visible-light photocatalyst characteristic.Its weak point is, the photochemical catalyst electron transmission difficulty of preparation.
Summary of the invention
The object of the invention is to the defect in order to solve existing preparation photocatalyst oxidizes ability preparation method difficulty and the device providing a kind of vacuum, carrier gas dual-purpose, achieve catalyst vacuumizing, seal is good, the device of the photochemical catalyst light induced electron utilizing device to prepare and the visible light-responded photochemical catalyst of the preparation of hole good separating effect.
Another object of the present invention utilizes this device to prepare visible light-responded height to provide, the preparation method of effective to organic selective oxidation, selective high photochemical catalyst.
To achieve these goals, the present invention is by the following technical solutions:
A kind of device preparing visible light-responded photochemical catalyst, comprise illumination reaction case, glass piping system, carrier gas gas gathering system, vacuum plant, described glass piping system comprises glass piping, valve, condenser pipe, reactor, and condenser pipe, illumination reaction device, xenon lamp, magnetic stirring apparatus, lifting platform are arranged in illumination reaction case, and described carrier gas gas gathering system comprises carrier gas bottle, pressure-reducing valve, gas bottle; Described vacuum plant comprises vacuum meter, vavuum pump; Carrier gas bottle connects glass piping one end, illumination reaction device bottom arm respectively, glass piping system is formed by connecting by glass piping, valve, condenser pipe, illumination reaction device successively, it is outside that horizontal glass piping is positioned at illumination reaction case, its end connects vavuum pump, gas bottle respectively, it is equipped with some valves and vacuum meter.
As preferably, the top of described illumination reaction case is provided with visual window, and visual window is provided with anti glare anti static coatings glass, and condenser pipe and illumination reaction case contact position are provided with sealing ring.
As preferably, xenon lamp, magnetic stirring apparatus, lifting platform are arranged in illumination reaction case, and xenon lamp and magnetic stirring apparatus are positioned on lifting platform, and xenon lamp lamp holder height, just a little more than illumination reaction device, stretches into above illumination reaction device, just right with illumination reaction device; Each one of xenon lamp, magnetic stirring apparatus, lifting platform has large and small two, and xenon lamp is positioned on large lifting platform, and magnetic stirring apparatus is positioned on little lifting platform, and faces and be placed in illumination reaction device bottom, magnetic stirring apparatus and illumination reaction device bottom distance 1 to 2 centimetre.
As preferably, illumination reaction device has orthogonal arm near bottom, and athwartship leg is equipped with valve, illumination reaction device is made up of suspension arm, quartz cover, glass, and described suspension arm has two, hollow symmetrical, upper end is hemispherical, connect with the condenser pipe on top, there is thin spiral glass tube described condenser pipe inside, and condensing water inlet is arranged at outer wall top, condensation-water drain is arranged at outer wall bottom, condenser pipe lower end, in hemisphere hull shape, connects with illumination reaction device.
A preparation method for visible light-responded photochemical catalyst, described preparation method's step is as follows:
A) distilled water will be dissolved in after raw mill, put into illumination reaction device, add chlorauric acid solution;
B) system is vacuumized, open light source, illumination reaction 1-9h, continue in course of reaction to vacuumize, obtain reaction solution;
C) reaction solution obtained after step b) is centrifugal, and then oven for drying grinds, and obtains photochemical catalyst.
As preferably, step b) replaces with vavuum pump, valve contract fully, opens carrier gas, No. 8 valve opens, be full of after nitrogen until system, open No. 6 and No. 7 valves, open light source, illumination reaction 1-9h, maintaining nitrogen purge in course of reaction, the dividing potential drop of logical nitrogen is 0.1-0.6MPa.
As preferably, raw material is the melamine after P25 or calcining, gets 0.5g and be dissolved in 50mL distilled water after grinding.
As preferably, when raw material is melamine, first get raw material 5g, at 400-600 DEG C, calcine 4-6h, get 0.5g after cooling grinding and be dissolved in 50mL distilled water.
As preferably, chlorauric acid solution is that 1g gold chloride is dissolved in 100mL, and the amount adding chlorauric acid solution is 0.1-2mL.
As preferably, described light source is xenon lamp, power 300W, operating voltage 14V, operating current 14-21A.
Core of the present invention provides a kind of vacuum, carrier gas dual-purpose apparatus for preparing visible light-responded photochemical catalyst, the switching of vacuum plant and carrier gas device can be realized, with the demand of satisfied preparation different catalysts, the photochemical catalyst of high visible response can be prepared simultaneously.
Beneficial effect of the present invention:
1) easy switching of vacuum plant and carrier gas device;
2) improve the effect of catalyst noble metal load;
3) vacuum and carrier gas two kinds operation can be provided;
4) preparation technology of the present invention is simple, environmentally friendly;
5) raw material availability of the present invention is high, saves the cost of preparation;
6) photochemical catalyst that prepared by the present invention has excellent photoelectrocatalysis ability, and its reason is that Au has good conductive capability and chemical stability, and therefore the carbon nitride material of Au parcel effectively can improve interface electron transmission ability, reduces reaction energy barrier; In addition, effectively suppress carbon monoxide Poisoning Phenomenon because Au has, therefore photochemical catalyst of the present invention also has antitoxin voltinism energy.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of the present invention.
In figure, 1-8, valve; 9, illumination reaction device bottom arm; 10, vacuum meter; 11, condensing water inlet; 12, condensation-water drain; 13, condenser pipe; 14, thin spiral glass tube; 15, illumination reaction device; 16, xenon lamp; 17, magnetic stirring apparatus; 18, lifting platform; 19, packing ring; 20, illumination reaction case; 21, carrier gas bottle; 22, vavuum pump; 23, gas bottle; 24, pressure-reducing valve.
Fig. 2 is the partial enlarged drawing of illumination reaction device.
Fig. 3 is embodiment of the present invention 1-3 and comparative example 1 selective oxidation phenmethylol effect contrast figure.
Fig. 4 is embodiment of the present invention 4-5 and comparative example 2 selective oxidation phenmethylol effect contrast figure.
Detailed description of the invention
Below by specific embodiment, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.
Method in following embodiment, if no special instructions, is the conventional method of this area.
As shown in Figure 1 and Figure 2, vacuum, the carrier gas dual-purpose apparatus preparing visible light responsive photocatalyst of the present invention, comprises illumination reaction case 20, glass piping system, carrier gas gas gathering system, vacuum plant etc.Described glass piping system comprises glass piping, valve, condenser pipe 13, reactor 15.In described illumination reaction case 20, contain the parts such as condenser pipe 13, illumination reaction device 15, xenon lamp 16, magnetic stirring apparatus 17, lifting platform 18.Described carrier gas gas gathering system, comprises carrier gas bottle 21, pressure-reducing valve 24, gas bottle 23.Described vacuum plant comprises vacuum meter 10, vavuum pump 22.Described carrier gas bottle 21, connects glass piping one end, illumination reaction device bottom arm 9 respectively.Described glass piping system, be formed by connecting by glass piping, valve (1-8), condenser pipe 13, illumination reaction device 15 successively, it is outside that horizontal glass piping is positioned at illumination reaction case 20, its end connects vavuum pump 22, gas bottle 23 respectively, valve totally 7 (1-7) it is equipped with, vacuum meter 1.
Described illumination reaction case 20, chamber door can be opened, and visual window is arranged at top, and preferably, visual window has anti glare anti static coatings glass.
Described xenon lamp 16, magnetic stirring apparatus 17, lifting platform 18 are also positioned at illumination reaction case 20, xenon lamp 16 and magnetic stirring apparatus 17 are positioned on lifting platform 18, xenon lamp 16 lamp holder height, just a little more than illumination reaction device 15, stretches into above illumination reaction device 15, just right with it.Each one of described xenon lamp 16, magnetic stirring apparatus 17, lifting platform 18 has large and small two, and xenon lamp 16 is positioned on large lifting platform, and magnetic stirring apparatus is positioned on little lifting platform, and faces and be placed in illumination reaction device 15 bottom.Magnetic stirring apparatus 17 and illumination reaction device 15 bottom distance 1 to 2 centimetre, to prevent dropping and the deformation of lifting platform 18 of illumination reaction device 15.
There is thin spiral glass tube 14 described condenser pipe 13 inside, and condensing water inlet 11 is arranged at outer wall top, and condensation-water drain 12 is arranged at outer wall bottom, condenser pipe lower end, in hemisphere hull shape, connects with illumination reaction device 15.
Condenser pipe 13 and illumination reaction case 20 contact position are provided with packing ring 19.
Illumination reaction device 15 has orthogonal arm 9 near bottom, athwartship leg is equipped with valve 8, can to control in illumination reaction device liquid and flow out, and the passing into of carrier gas.Illumination reaction device 15, by suspension arm, quartz cover, glass forms.Described suspension arm has two, hollow, and symmetrical, upper end is hemispherical, connects with the condenser pipe on top.Described quartz cover, there is clockwise thread inside, described glass, and anti-clockwise thread is arranged at top, and the two connects and can screw, and both ensure that negative pressure when using vacuum system, in turn ensure that sealing when using carrier gas.
Embodiment 1
A preparation method for visible light responsive photocatalyst, step is as follows: by 5g melamine in Muffle furnace, constant temperature 520 DEG C, calcines 4 hours, obtains g-C
3n
4.After grinding, claim 0.5g to be dissolved in 50mL distilled water, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution, 1,2, No. 8 valve closing, all the other valve opens, after system being vacuumized, open light source, illumination reaction 3h, continues in course of reaction to vacuumize, the power 300W of xenon lamp, operating voltage 14V, operating current 14-21A are last, solution centrifugal after reacting, oven for drying, grinding, the photochemical catalyst Au/g-C prepared under obtaining vacuum condition
3n
4.
Embodiment 2
A preparation method for visible light responsive photocatalyst, step is as follows: by 5g melamine in Muffle furnace, constant temperature 520 DEG C, calcines 4 hours, obtains g-C
3n
4.After grinding, claim 0.5g to be dissolved in 50mL distilled water, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution.Vavuum pump, valve complete shut-down, open nitrogen (carrier gas), No. 8 valve opens, after system is full of nitrogen, opens 6, No. 7 valves, open light source, illumination reaction 3h, maintaining nitrogen purge in course of reaction.The power 300W of xenon lamp, operating voltage 14V, operating current 14-21A are last, solution centrifugal after reacting, oven for drying, grinding, the photochemical catalyst Au/g-C prepared under obtaining logical condition of nitrogen gas
3n
4.
Embodiment 3
A preparation method for visible light responsive photocatalyst, step is as follows: by 5g melamine in Muffle furnace, constant temperature 400 DEG C, calcines 5 hours, obtains g-C
3n
4.After grinding, claim 0.5g to be dissolved in 50mL distilled water, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution.Vavuum pump, valve complete shut-down, open nitrogen (carrier gas), No. 8 valve opens, after system is full of nitrogen, opens 6, No. 7 valves, open light source, illumination reaction 1h, maintaining nitrogen purge in course of reaction.The power 300W of xenon lamp, operating voltage 14V, operating current 14-21A are last, solution centrifugal after reacting, oven for drying, and grinding, obtains photochemical catalyst Au/g-C
3n
4.
Embodiment 4
A kind of preparation method of visible light responsive photocatalyst, step is as follows: claim 0.5gP25 to be dissolved in 50mL distilled water, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution, 1,2, No. 8 valve closing, all the other valve opens, after system being vacuumized, open light source, illumination reaction 9h, continue in course of reaction to vacuumize, the power 300W of xenon lamp, operating voltage 14V, operating current 14-21A is last, solution centrifugal after reacting, oven for drying, grinding, the photochemical catalyst Au/P25 prepared under obtaining vacuum condition.
Embodiment 5
A preparation method for visible light responsive photocatalyst, step is as follows: claim 0.5gP25 to be dissolved in 50mL distilled water, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution, join in illumination reaction device, screw quartz cover, add 1mL chlorauric acid solution.Vavuum pump, valve complete shut-down, open nitrogen (carrier gas), No. 8 valve opens, after system is full of nitrogen, opens 6, No. 7 valves, open light source, illumination reaction 9h, maintaining nitrogen purge in course of reaction.The power 300W of xenon lamp, operating voltage 14V, operating current 14-21A are last, solution centrifugal after reacting, oven for drying, grinding, the photochemical catalyst Au/P25 prepared under obtaining logical condition of nitrogen gas.
Comparative example 1
Sodium borohydride reduction prepares Au/g-C
3n
4: by g-C
3n
4(0.5g) be dissolved in 50mL distilled water, stir, add several perchloric acid, adjust pH to be less than 2, add 1mL chlorauric acid solution, stir, dropwise add NaHB
4solution (excessive), stirring reaction 2 hours, centrifugal, wash 5 times, remove residual, dry.
Comparative example 2
Sodium borohydride reduction prepares Au/P25: by P25(0.5g) be dissolved in 50mL distilled water, stir, add several perchloric acid, adjust pH to be less than 2, add 1mL chlorauric acid solution, stir, dropwise add NaHB
4solution (excessive), stirring reaction 2 hours, centrifugal, wash 5 times, remove residual, dry.
Under visible light, g-C is utilized
3n
4, NaHB
4au/g-C prepared by reducing process, embodiment 1-3
3n
4, carry out the Contrast on effect that selective oxidation phenmethylol is benzaldehyde.
Weigh the Au/g-C of 20mg
3n
4, pipette 2mL benzyl alcohol solution (20uL phenmethylol is dissolved in 20mL benzotrifluoride), join in reaction bulb, stir 5min, leave standstill, with gas chromatograph, test sample 3 times, averages.Then, fill oxygen 10min(oxygen partial pressure 0.1MPa), under being positioned over xenon lamp (300W), visible ray (adding 420nm optical filter), reacts after 3 hours, test sample again, calculates conversion ratio.
Under visible light, with pure P25, NaHB
4au/P25 prepared by reducing process, embodiment 4-5, selective oxidation phenmethylol is benzaldehyde, contrast effect.
G-C
3n
4for yellow, fine powder, easily bond, Au/P25 is Dark grey.In general, due to g-C
3n
4for yellow, its absorption to visible ray, response more weak, selective oxidation organic matter poor effect under visible ray.The Au/g-C of Dark grey
3n
4, because color is comparatively dark, good response should be able to be had to visible ray.
Fig. 3 is the selective oxidation phenmethylol effect contrast figure of embodiment of the present invention 1-2 and comparative example 1.
As can be seen from the figure, under visible ray, g-C
3n
4selective oxidation phenmethylol is the conversion ratio of benzaldehyde is 18.68%, conventional NaHB
4au/g-C prepared by reducing process
3n
4, to the selective oxidation poor effect of phenmethylol, after carrying gold, effect does not obviously promote.But, Au/g-C prepared by carrier gas system
3n
4, phenmethylol conversion ratio improves obviously, can reach 56.58%, and knows that the selective of benzaldehyde is 99% according to calibration curve calculating.This illustrates the use of this device, especially under logical condition of nitrogen gas, helpful for the response of raising photochemical catalyst to visible ray.
P25 is pure white, fine powder, and Au/P25 is royal purple.In general, because P25 is pure white, its absorption to visible ray, response more weak, effect of disposing of sewage under visible ray is very undesirable.Mauve Au/P25, because color is comparatively dark, should be able to have good response to visible ray.
Fig. 4 is the selective oxidation phenmethylol effect contrast figure of embodiment of the present invention 3-4 and comparative example 2.
As can be seen from the figure, under visible ray, P25 selective oxidation phenmethylol is the conversion ratio of benzaldehyde is 21.35%, conventional NaHB
4au/P25 prepared by reducing process, to the selective oxidation poor effect of phenmethylol.But Au/P25 prepared by carrier gas system, phenmethylol conversion ratio improves obviously, can reach 72.86%, and knows that the selective of benzaldehyde is 99% according to calibration curve calculating.This illustrates the use of this device, for photocatalyst noble metal, improves that it is visible light-responded, thus to improve its selective oxidation phenmethylol be the effect of benzaldehyde.
Claims (10)
1. prepare the device of visible light-responded photochemical catalyst for one kind, it is characterized in that, comprise illumination reaction case (20), glass piping system, carrier gas gas gathering system, vacuum plant, described glass piping system comprises glass piping, valve (1-8), condenser pipe (13), reactor (15), condenser pipe (13), illumination reaction device (15), xenon lamp (16), magnetic stirring apparatus (17), lifting platform (18) are arranged in illumination reaction case (20), and described carrier gas gas gathering system comprises carrier gas bottle (21), pressure-reducing valve (24), gas bottle (23); Described vacuum plant comprises vacuum meter (10), vavuum pump (22); Carrier gas bottle (21) connects glass piping one end, illumination reaction device bottom arm (9) respectively, glass piping system is formed by connecting by glass piping, valve (1-8), condenser pipe (13), illumination reaction device (15) successively, it is outside that horizontal glass piping is positioned at illumination reaction case (20), its end connects vavuum pump (22), gas bottle (23) respectively, it is equipped with some valves and vacuum meter (10).
2. a kind of device preparing visible light-responded photochemical catalyst according to claim 1, it is characterized in that, the top of described illumination reaction case (20) is provided with visual window, visual window is provided with anti glare anti static coatings glass, and condenser pipe (13) and illumination reaction case (20) contact position are provided with sealing ring (19).
3. a kind of device preparing visible light-responded photochemical catalyst according to claim 1, it is characterized in that, xenon lamp (16), magnetic stirring apparatus (17), lifting platform (18) are arranged in illumination reaction case (20), xenon lamp (16) and magnetic stirring apparatus (17) are positioned on lifting platform (18), xenon lamp (16) lamp holder height is just a little more than illumination reaction device (15), stretch into illumination reaction device (15) top, just right with illumination reaction device (15); Each one of xenon lamp (16), magnetic stirring apparatus (17), lifting platform (18) has large and small two, xenon lamp (16) is positioned on large lifting platform (18), magnetic stirring apparatus (17) is positioned on little lifting platform (18), and face and be placed in illumination reaction device (15) bottom, magnetic stirring apparatus (17) and illumination reaction device (15) bottom distance 1 to 2 centimetre.
4. a kind of device preparing visible light-responded photochemical catalyst according to claim 1 or 2 or 3, it is characterized in that, illumination reaction device (15) has orthogonal arm (9) near bottom, valve (8) athwartship leg is equipped with, illumination reaction device (15) is by suspension arm, quartz cover, glass forms, described suspension arm has two, hollow symmetrical, upper end is hemispherical, connect with the condenser pipe (13) on top, there is thin spiral glass tube (14) described condenser pipe (13) inside, condensing water inlet (11) is arranged at outer wall top, condensation-water drain (12) is arranged at outer wall bottom, condenser pipe lower end, in hemisphere hull shape, connect with illumination reaction device (15).
5. a preparation method for visible light-responded photochemical catalyst, is characterized in that, described preparation method's step is as follows:
A) distilled water will be dissolved in after raw mill, put into illumination reaction device (20), add chlorauric acid solution;
B) system is vacuumized, open light source, illumination reaction 1-9h, continue in course of reaction to vacuumize, obtain reaction solution;
C) reaction solution obtained after step b) is centrifugal, and then oven for drying grinds, and obtains photochemical catalyst.
6. the preparation method of a kind of visible light-responded photochemical catalyst according to claim 5, it is characterized in that, step b) replaces with vavuum pump (22), valve (1-8) contract fully, opens carrier gas, No. 8 valve opens, be full of after nitrogen until system, open No. 6 and No. 7 valves, open light source, illumination reaction 1-9h, maintaining nitrogen purge in course of reaction, the dividing potential drop of logical nitrogen is 0.1-0.6MPa.
7. the preparation method of a kind of visible light-responded photochemical catalyst according to claim 5, is characterized in that, raw material is P25 or the melamine after calcining, and gets 0.5g and be dissolved in 50mL distilled water after grinding.
8. the preparation method of a kind of visible light-responded photochemical catalyst according to claim 5 or 7, is characterized in that, when raw material is melamine, first gets raw material 5g, at 400-600 DEG C, calcines 4-6h, gets 0.5g and be dissolved in 50mL distilled water after cooling grinding.
9. the preparation method of a kind of visible light-responded photochemical catalyst according to claim 5 or 6 or 7, is characterized in that, chlorauric acid solution is that 1g gold chloride is dissolved in 100mL, and the amount adding chlorauric acid solution is 0.1-2mL.
10. the preparation method of a kind of visible light-responded photochemical catalyst according to claim 5 or 6 or 7, is characterized in that, described light source is xenon lamp, power 300W, operating voltage 14V, operating current 14-21A.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510074297.0A CN104741153B (en) | 2015-02-12 | 2015-02-12 | A kind of device and preparation method for preparing visible light-responded photochemical catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510074297.0A CN104741153B (en) | 2015-02-12 | 2015-02-12 | A kind of device and preparation method for preparing visible light-responded photochemical catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104741153A true CN104741153A (en) | 2015-07-01 |
| CN104741153B CN104741153B (en) | 2017-10-24 |
Family
ID=53581740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510074297.0A Expired - Fee Related CN104741153B (en) | 2015-02-12 | 2015-02-12 | A kind of device and preparation method for preparing visible light-responded photochemical catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104741153B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107754837A (en) * | 2017-09-21 | 2018-03-06 | 浙江工商大学 | Single-layer silicon nitride carbon nanosheet and bismuth plasma combined modification type bismuth oxide base electrode and its preparation and application |
| CN109456160A (en) * | 2017-09-06 | 2019-03-12 | 中国科学院大连化学物理研究所 | A kind of method of photochemical catalytic oxidation fracture lignin model compound |
| CN114392739A (en) * | 2022-03-25 | 2022-04-26 | 烟台沃泰特新材料科技有限责任公司 | Catalyst for degrading VOC (volatile organic compounds) in matt catalysis manner, preparation process and preparation device |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011068095A1 (en) * | 2009-12-01 | 2011-06-09 | 住友化学株式会社 | Method for producing liquid dispersion of noble metal-supporting photocatalyst particles, liquid dispersion of noble metal-supporting photocatalyst particles, hydrophilizing agent, and photocatalytic functional product |
| CN102120184A (en) * | 2011-01-25 | 2011-07-13 | 中国科学院山西煤炭化学研究所 | Noble metal-carrying titanium dioxide catalyst and preparation method and use thereof |
| CN102151534A (en) * | 2011-01-30 | 2011-08-17 | 西北大学 | Multifunctional photocatalytic reaction device |
| CN102718253A (en) * | 2012-06-20 | 2012-10-10 | 中国科学院福建物质结构研究所 | Brookite titanium dioxide nanocrystalline and preparation method and application thereof |
| CN203216914U (en) * | 2013-01-05 | 2013-09-25 | 江南大学 | Multipurpose photocatalytic performance assessment device |
| CN104028308A (en) * | 2014-06-20 | 2014-09-10 | 中国科学院新疆理化技术研究所 | Nanometer photo-catalyst used in producing hydrogen by decomposing water under visible light response and application of nanometer photo-catalyst |
-
2015
- 2015-02-12 CN CN201510074297.0A patent/CN104741153B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011068095A1 (en) * | 2009-12-01 | 2011-06-09 | 住友化学株式会社 | Method for producing liquid dispersion of noble metal-supporting photocatalyst particles, liquid dispersion of noble metal-supporting photocatalyst particles, hydrophilizing agent, and photocatalytic functional product |
| CN102120184A (en) * | 2011-01-25 | 2011-07-13 | 中国科学院山西煤炭化学研究所 | Noble metal-carrying titanium dioxide catalyst and preparation method and use thereof |
| CN102151534A (en) * | 2011-01-30 | 2011-08-17 | 西北大学 | Multifunctional photocatalytic reaction device |
| CN102718253A (en) * | 2012-06-20 | 2012-10-10 | 中国科学院福建物质结构研究所 | Brookite titanium dioxide nanocrystalline and preparation method and application thereof |
| CN203216914U (en) * | 2013-01-05 | 2013-09-25 | 江南大学 | Multipurpose photocatalytic performance assessment device |
| CN104028308A (en) * | 2014-06-20 | 2014-09-10 | 中国科学院新疆理化技术研究所 | Nanometer photo-catalyst used in producing hydrogen by decomposing water under visible light response and application of nanometer photo-catalyst |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109456160A (en) * | 2017-09-06 | 2019-03-12 | 中国科学院大连化学物理研究所 | A kind of method of photochemical catalytic oxidation fracture lignin model compound |
| CN107754837A (en) * | 2017-09-21 | 2018-03-06 | 浙江工商大学 | Single-layer silicon nitride carbon nanosheet and bismuth plasma combined modification type bismuth oxide base electrode and its preparation and application |
| CN114392739A (en) * | 2022-03-25 | 2022-04-26 | 烟台沃泰特新材料科技有限责任公司 | Catalyst for degrading VOC (volatile organic compounds) in matt catalysis manner, preparation process and preparation device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104741153B (en) | 2017-10-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Research advances towards large-scale solar hydrogen production from water | |
| Das et al. | A review on advances in photocatalysts towards CO 2 conversion | |
| Halmann et al. | Photoassisted carbon dioxide reduction on aqueous suspensions of titanium dioxide | |
| CN106362729B (en) | A kind of in-situ preparation method of oxygen-containing vacancy defect photochemical catalyst strontium bismuth niobium oxygen | |
| Rockafellow et al. | Selenium-modified TiO2 and its impact on photocatalysis | |
| CN104258886B (en) | A kind of silver orthophosphate/oxygen vacancies type titanium dioxide composite photocatalyst and preparation method | |
| CN106799222B (en) | A kind of preparation method of titanium dioxide/niobium acid tin composite nano materials | |
| Jia et al. | Enhanced visible-light active C and Fe co-doped LaCoO3 for reduction of carbon dioxide | |
| CN104741153A (en) | Device for preparing photocatalysts with visible-light response and preparation method thereof | |
| Yu et al. | Fabrication of heterostructured CdS/TiO2 nanotube arrays composites for photoreduction of U (VI) under visible light | |
| Chen et al. | Effect of reaction atmosphere on photodeposition of Pt nanoparticles and photocatalytic hydrogen evolution from SrTiO3 suspension system | |
| Chen et al. | Three-Dimensional Ordered Macroporous gC 3 N 4-Cu 2 O-TiO 2 Heterojunction for Enhanced Hydrogen Production | |
| CN106423223B (en) | A kind of pie porous structure MoSe2@TiO2 photochemical catalyst and preparation method thereof | |
| CN105664995A (en) | Multi-element co-doped nano titanium dioxide photocatalytic material | |
| CN105080553B (en) | A kind of preparation method of stanniferous double-perovskite type Photocatalytic Degradation of Phenol catalyst | |
| CN105536843A (en) | Preparation method of highly visible light electron transfer g-C3N4/ Au/TiO2 Z type photocatalyst | |
| CN109748894A (en) | A method of producing 2,5- furans dicarbaldehyde | |
| CN107486213A (en) | A kind of hollow BiVO4The preparation method of micron film photochemical catalyst | |
| Liu et al. | CoNi bimetallic alloy cocatalyst-modified TiO2 nanoflowers with enhanced photocatalytic hydrogen evolution | |
| CN107469822A (en) | Efficent electronic transfer Cu modifications C/TiO2The preparation method of photo catalytic reduction material | |
| CN100503034C (en) | Titanium dichloride load method when in use for preparing catalyst, and dual functional catalyst for recovering sulfur prepared by using the method | |
| CN107149931A (en) | The preparation method of Zinc oxide quantum dot potassium niobate photochemical catalyst and the purposes of the catalyst | |
| CN107899569A (en) | A kind of preparation method of platinum modified nano-titanium dioxide | |
| CN103506104B (en) | Carbon-doped TiO2 visible light-responding catalytic film on glass carrier and preparation method thereof | |
| CN115999614B (en) | Ultraviolet-visible-near infrared light responsive carbon dioxide reduction photocatalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Qi Inventor after: Shi Xiaodong Inventor before: Wang Qi Inventor before: Shi Xiaodong Inventor before: Zhu Naxin Inventor before: Hu Jingtao Inventor before: Wang Chunchun Inventor before: Zhou Tiantian Inventor before: Liu Yanqiu Inventor before: Zhang Die |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20171024 Termination date: 20180212 |