CN104324742A - Nickel carbonate-supported titanium dioxide ultraviolet light catalyst and preparation method thereof - Google Patents
Nickel carbonate-supported titanium dioxide ultraviolet light catalyst and preparation method thereof Download PDFInfo
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- CN104324742A CN104324742A CN201410642960.8A CN201410642960A CN104324742A CN 104324742 A CN104324742 A CN 104324742A CN 201410642960 A CN201410642960 A CN 201410642960A CN 104324742 A CN104324742 A CN 104324742A
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Abstract
The invention discloses a nickel carbonate-supported titanium dioxide ultraviolet light catalyst and a preparation method thereof. The light catalyst comprises the following raw materials in parts by weight: 1 part of titanium dioxide, 0.2-0.5 part of inorganic carbonate and 0.001-0.4 part of inorganic nickel salt. The method comprises the following steps: dissolving inorganic carbonate into water to obtain an inorganic carbonate water solution of which the molar concentration is 0.1-1.0mmol/L; dispersing titanium dioxide into the inorganic carbonate water solution to obtain a suspension; and finally, slowly adding the inorganic nickel salt into the suspension, stirring evenly, washing and standing, filtering by using filter paper, and drying in vacuum at 60-100 DEG C for 4-8 hours so as to obtain the nickel carbonate-supported titanium dioxide ultraviolet light catalyst. Compared with a traditional supporting technology that a supporter of a transition metal oxide needs to be calcined by using electric energy, the method does not have preparation cost and is free of electric energy] consumption; and the cost for preparing the light catalyst is increased by less than 1 yuan per 500g on the basis of the cost of titanium dioxide.
Description
Technical field
The present invention relates to ultraviolet light photocatalysis agent, refer to titanium dioxide ultraviolet photochemical catalyst of a kind of nickelous carbonate load and preparation method thereof particularly.
Background technology
Hydrogen Energy is clean, efficient, convenient stores the plurality of advantages such as transport, is described as " following oil ", is subject to showing great attention to of countries in the world.But traditional hydrogen production process needs to consume huge conventional energy resource, makes the Hydrogen Energy personal value too high, greatly limit applying of Hydrogen Energy.Until 1972, Fujishima and Honda
[1]find at titanium dioxide (TiO
2) phenomenon of photochemical catalyzing on electrode, make in the means developed in numerous Hydrogen Energy, utilize solar energy photocatalytic hydrogen production by water decomposition to become one of ideal, the most promising means.
Although Photocatalyzed Hydrogen Production experienced by the course of 40, report TiO
2, CdS, WO
3, Fe
2o
3, ZnO, ZnS, SnO
2deng tens kinds of photochemical catalysts, but TiO
2remain studied and the maximum photochemical catalyst of report, and P25 is as the TiO of industrial applications rank
2be widely used in the field such as chemical industry, environment therefore, around TiO
2modification, improve its solar energy conversion ratio, improve photocatalysis method and Photoreactor, improve photocatalysis efficiency, remain one of current study hotspot.But pure TiO
2during photocatalysis Decomposition aquatic products hydrogen, the product hydrogen activity that it shows under the irradiation of ultraviolet light is very low, does not almost produce hydrogen activity.Therefore need to utilize some means to suppress TiO
2the compound of photo-generated carrier, improves Charge transfer on interface speed and improves TiO
2photocatalysis performance.TiO
2the main method of modification has
[2,3]: load cocatalyst, metal cation and carbon, nitrogen, carbon etc. are anion doped, dye sensitization etc., and wherein load cocatalyst is considered to the most effective method of modifying.
Co-catalyst also becomes the emphasis of research efficiently in recent years, and co-catalyst selects noble metal (Pt, Pd, Ru, Au, Ag) or metal oxide containing precious metals such as NiO usually, effectively can improve TiO
2the efficiency of photocatalysis Decomposition aquatic products hydrogen, but noble metal is expensive and rareness has even exceeded the cost producing hydrogen.What the preparation method of load was in the news in addition mostly is: high-temperature calcination and long-time hydro-thermal, energy consumption is high.
Summary of the invention
Technical problem to be solved by this invention is just to provide titanium dioxide ultraviolet photochemical catalyst of a kind of nickelous carbonate load and preparation method thereof.The invention solves co-catalyst (Pt, Pd, Ru, Au, Ag) costliness and the problem of rareness, reduce cost of material.
For solving the problems of the technologies described above, the titanium dioxide ultraviolet photochemical catalyst of a kind of nickelous carbonate load provided by the invention, described photochemical catalyst comprises 1 part of titanium dioxide, the inorganic carbonate of 0.2 ~ 0.5 part, the inorganic nickel of 0.001 ~ 0.4 part by the ratio of weight and number of raw material.
Further, described inorganic nickel be nickelous sulfate and nickel nitrate any one.Described inorganic carbonate be in sodium carbonate and potash any one.
Again further, described in state photochemical catalyst and be made up of nickelous carbonate and titanium dioxide, described nickelous carbonate load is on the surface of titanium dioxide.
Again further, in described photochemical catalyst, the percentage by weight that nickelous carbonate accounts for photochemical catalyst is 0.09 ~ 28.5%.
Present invention also offers a kind of preparation method of titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load, comprise the following steps:
1) titanium dioxide, inorganic carbonate, inorganic nickel is taken according to above-mentioned weight fraction than meter, for subsequent use;
2) by step 1) inorganic carbonate that obtains is soluble in water, obtains the inorganic carbonate saline solution that molar concentration is 0.1 ~ 1.0mmol/L;
3) titanium dioxide is dispensed into step 2) in the inorganic carbonate saline solution that obtains, obtain suspension;
4) inorganic nickel slowly being added step 3) in the suspension that obtains, stir, after washing leaves standstill, with Filter paper filtering, vacuum drying 4 ~ 8h under temperature is 60 ~ 100 DEG C of conditions, namely obtains the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load.
Beneficial effect of the present invention is:
(1) titanium dioxide optical catalyst of the method just obtainable nickelous carbonate load in 20 minutes is used
(2) this co-catalyst is found to have the effect of co-catalyst first as transition metal salt material, and can substitute noble metal promoted agent, and its load is at TiO
2on Photocatalyzed Hydrogen Production activity to reach as high as 0.5mmol/h be pure TiO
2produce more than 39 times of hydrogen activity, higher than the TiO of other transition metal oxide and noble-metal-supported
2, compared with the Pt-TiO2 of H2-producing capacity the best, hydrogen output hourly only differs from 78 μm of ol, and continues 10h without deactivation phenomenom.
(3) compared with traditional load technology, the load of transition metal oxide all goes calcining with electric energy, and this method does not have preparation cost, without the need to using electric energy consumption.The cost preparing this photochemical catalyst be titanium dioxide cost on every 500g increase cost less than 1 yuan.
Accompanying drawing explanation
Fig. 1 is the product hydrogen activity comparison diagram of embodiment sample, TiO2 and prior art;
Fig. 2 is transmission electron microscope TEM image (a) and high-resolution transmission HRTEM image (b) of embodiment 2
Detailed description of the invention
In order to explain the present invention better, illustrate main contents of the present invention further below in conjunction with specific embodiment, but content of the present invention is not only confined to following examples.
Embodiment 1
A preparation method for the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load, comprises the following steps:
1) take the nickel nitrate of the titanium dioxide of 1g, the sodium carbonate of 0.2g and 0.002g than meter according to above-mentioned weight fraction, for subsequent use;
2) by step 1) sodium carbonate that obtains is soluble in water, obtains the aqueous sodium carbonate that molar concentration is 0.1 ~ 1.0mmol/L;
3) titanium dioxide is dispensed into step 2) in the aqueous sodium carbonate that obtains, obtain suspension;
4) nickel nitrate slowly being added step 3) in the suspension that obtains, stir, after washing leaves standstill, with Filter paper filtering, vacuum drying 4 ~ 8h under temperature is 60 ~ 100 DEG C of conditions, namely obtains the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load; Wherein, described nickelous carbonate load is on the surface of titanium dioxide, and the percentage by weight that nickelous carbonate accounts for photochemical catalyst is 0.2%.
Embodiment 2
The present embodiment is substantially identical with the preparation method of embodiment 1, and difference is:
The titanium dioxide ultraviolet photochemical catalyst 2 of nickelous carbonate load, described photochemical catalyst comprises 1 part of titanium dioxide, the potash of 0.5 part, the nickelous sulfate of 0.01 part by the ratio of weight and number of raw material.The percentage by weight that nickelous carbonate accounts for photochemical catalyst is 0.9%.
Embodiment 3
The present embodiment is substantially identical with the preparation method of embodiment 1, and difference is:
The titanium dioxide ultraviolet photochemical catalyst 3 of nickelous carbonate load, described photochemical catalyst comprises 1 part of titanium dioxide, the sodium carbonate of 0.3 part, the nickel nitrate of 0.015 part by the ratio of weight and number of raw material.The percentage by weight that nickelous carbonate accounts for photochemical catalyst is 1.5%.
Embodiment 4
The present embodiment is substantially identical with the preparation method of embodiment 1, and difference is:
The titanium dioxide ultraviolet photochemical catalyst 4 of nickelous carbonate load, described photochemical catalyst comprises 1 part of titanium dioxide, the sodium carbonate of 0.4 part, the nickel nitrate of 0.06 part by the ratio of weight and number of raw material.The percentage by weight that nickelous carbonate accounts for photochemical catalyst is 5.6%.
Embodiment 5
The present embodiment is substantially identical with the preparation method of embodiment 1, and difference is:
The titanium dioxide ultraviolet photochemical catalyst 5 of nickelous carbonate load, described photochemical catalyst comprises 1 part of titanium dioxide, the potash of 0.2 part, the nickel nitrate of 0.09 part by the ratio of weight and number of raw material.The percentage by weight that nickelous carbonate accounts for photochemical catalyst is 8.3%.
Embodiment 6
The present embodiment is substantially identical with the preparation method of embodiment 1, and difference is:
The titanium dioxide ultraviolet photochemical catalyst 6 of nickelous carbonate load, described photochemical catalyst comprises 1 part of titanium dioxide, the potash of 0.5 part, the nickel nitrate of 0.4 part by the ratio of weight and number of raw material.The percentage by weight that nickelous carbonate accounts for photochemical catalyst is 9.5%.
Embodiment 7
The present embodiment is substantially identical with the preparation method of embodiment 1, and difference is:
The titanium dioxide ultraviolet photochemical catalyst 7 of nickelous carbonate load, described photochemical catalyst comprises 1 part of titanium dioxide, the potash of 0.2 part, the nickel nitrate of 0.001 part by the ratio of weight and number of raw material.The percentage by weight that nickelous carbonate accounts for photochemical catalyst is 5.5%.
Performance evaluation is carried out to the titanium dioxide ultraviolet photochemical catalyst of the nickelous carbonate load that embodiment 1 ~ 5 obtains:
Photocatalyzed Hydrogen Production activity photochemical catalyst having been prepared by embodiment 1 ~ 5 adopts advanced online automatic detection hydrogen output device, the content of gas-chromatography (GC7890-II) hydrogen of Shanghai Techcomp Instrument Ltd. utilizes high pure nitrogen propelling method to test, testing conditions is: 5A molecular sieve column chromatography post, setting column temperature 45 DEG C, the detected temperatures that arranges of conductance cell (TCD) detector is 120 DEG C, injector temperature is 120 DEG C, and bridge stream is 100mA.The device of simulated solar irradiation is the 350WXe lamp (model: PLS-SXE350/3500UV) that Beijing Bo Feilai Science and Technology Ltd. produces.
The method of the product hydrogen activity of test sample product is: weigh and prepare sample 50mg, be dispersed in 80mL ethylene glycol solution (volume fraction is the ethylene glycol solution of 5wt%).Sample fully infiltrates ultrasonic disperse 2h after a period of time, by the reaction system after catalyst hydrophily is adsorbed and be ultrasonic, seal after loading quartz glass reactor, and connect with detection system, after last keeping system vacuumizes 25min, under the condition of Keep agitation, gaseous product (H
2) carry out on-line checkingi by the detector TCD of gas chromatograph, gathered every one hour and once produce hydrogen activity data, whole system adopts circulation condensation device and air-conditioning to control temperature of reactor.
Following data can be read: in the present invention, the product hydrogen activity of embodiment 1 is 351.0 μm of o/h by Fig. 1, the product hydrogen activity of embodiment 2 is 525.2 μm of o/h, the product hydrogen activity of embodiment 3 is 240.9 μm of o/h, the product hydrogen activity of embodiment 4 is 91.6 μm of o/h, the product hydrogen activity of embodiment 5 is 58.5 μm of o/h, pure TiO
2product hydrogen activity be 13.6 μm of o/h, in contrast test, Pt load TiO
2product hydrogen activity be 600.08 μm of o/h, prior art report transition metal oxide load TiO
2after product hydrogen activity be: 278.1 μm of o/h.Therefore the product hydrogen activity size of sample puts in order and is followed successively by: Pt-TiO
2> embodiment 2 > implements the pure TiO of 1 > prior art > embodiment 3 > embodiment 4 > embodiment 5 >
2.It is worth mentioning that: the product hydrogen activity of embodiment 2 is than pure TiO
2product hydrogen activity high 39 times.
The product hydrogen activity of comparative example 1, example 2, example 3, example 4, example 5 can draw following rule: work as NiCO
3load capacity when being increased to 8.3% from 0.1%, along with NiCO
3the increase of content, the product hydrogen activity of photochemical catalyst increases.Work as NiCO
3mass percentage content when reaching 0.9%, the product hydrogen activity of this sample reaches the highest, but NiCO
3content continue to increase, the product hydrogen activity of sample reduces, and this is due to too much NiCO
3load is at TiO
2the surface of photochemical catalyst, has the effect that is in the light, and also can cause the scattering of light in addition, will be reduced by the incident light of reaction system, and the photon numbers that such photochemical catalyst produces falls sharply.The reason that another one is possible is: due to too much NiCO
3be present in TiO
2in can block TiO
2adsorption, and define new electronics and hole recombination centers, make light induced electron also not migrate to TiO
2surface just there occurs compound, rare is compared with the product hydrogen activity of existing base metal co-catalyst load, still exceeds 100 μm of ol/h.Compared with existing best co-catalyst precious metals pt, active difference 74 μm of ol/h, the replacement Pt that can realize to a certain extent become efficient co-catalyst.
The transmission electron microanalysis (TEM) of sign material composition and high-resolution transmission electron microscope (HRTEM) carry out on the TJEM-2100F type transmission electron microscope of Japanese vender company, and the accelerating potential of Electronic Speculum is 200kV; By the 0.9%NiCO of 10mg
3/ TiO
2ultrasonic disperse, in the ethanol of 5ml, then sends into the composition that JEM-2100F type transmission electron microscope carries out observing sample.
By Fig. 2, we can find: as can be seen from Fig. 2 (a), TiO
2nano particle presents aggregating state, sample NiCO
3/ TiO
2in contain size greatly about the nano particle of 20 ~ 60nm, wherein 40 ~ 60nm crystal grain correspond to rutile TiO
2, the crystal grain of 20 ~ 40nm corresponds to Detitanium-ore-type TiO
2, further observe the high-resolution TEM image of enlargement ratio as can be seen from Fig. 2 (b), have much little NiCO
3what nano-cluster was uneven is dispersed in TiO
2the surface of nano particle, these NiCO
3bunch size be approximately 1 ~ 2nm.
Other unspecified part is prior art.Although above-described embodiment is to invention has been detailed description; but it is only the present invention's part embodiment; instead of whole embodiment, people can also obtain other embodiments according to the present embodiment under without creative prerequisite, and these embodiments all belong to scope.
1、Fujishima A,Honda K.Electrochemical photolysis of water at a semiconductor electrode[J].Nature,1972,238:37-38.
2、Bak T,Nowotony J,Rekas M,et al.Photoelectrochemical hydrogen generation from water using solar energy[J].Int.J.Hydrogen Energy,2002,27:991-1022.
3、Asahi R,Morikawa T,Ohwaki T,et al.Visible-light photocatalysis in nitrogen-doped titanium oxides[J].Science,2001,293:269-271.
Claims (6)
1. a titanium dioxide ultraviolet photochemical catalyst for nickelous carbonate load, is characterized in that: described photochemical catalyst comprises 1 part of titanium dioxide, the inorganic carbonate of 0.2 ~ 0.5 part, the inorganic nickel of 0.001 ~ 0.4 part by the ratio of weight and number of raw material.
2. the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load according to claim 1, is characterized in that: described inorganic nickel be in nickelous sulfate and nickel nitrate any one.
3. the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load according to claim 1 or 2, is characterized in that: described inorganic carbonate be in sodium carbonate and potash any one.
4. the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load according to claim 1 or 2, is characterized in that: described in state photochemical catalyst and be made up of nickelous carbonate and titanium dioxide, described nickelous carbonate load is on the surface of titanium dioxide.
5. according to claim 1 or 2, have the tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, it is characterized in that: in described photochemical catalyst, the percentage by weight that nickelous carbonate accounts for photochemical catalyst is 0.09 ~ 28.5%.
6. a preparation method for the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load described in claim 1, is characterized in that: comprise the following steps:
1) titanium dioxide, inorganic carbonate, inorganic nickel is taken according to above-mentioned weight fraction than meter, for subsequent use;
2) by step 1) inorganic carbonate that obtains is soluble in water, obtains the inorganic carbonate saline solution that molar concentration is 0.1 ~ 1.0mmol/L;
3) titanium dioxide is dispensed into step 2) in the inorganic carbonate saline solution that obtains, obtain suspension;
4) inorganic nickel slowly being added step 3) in the suspension that obtains, stir, after washing leaves standstill, with Filter paper filtering, vacuum drying 4 ~ 8h under temperature is 60 ~ 100 DEG C of conditions, namely obtains the titanium dioxide ultraviolet photochemical catalyst of nickelous carbonate load.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115888676A (en) * | 2022-09-28 | 2023-04-04 | 电子科技大学长三角研究院(湖州) | Composition for inhibiting decomposition of nitrate and preparation method thereof |
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| GB834460A (en) * | 1956-03-29 | 1960-05-11 | Standard Oil Co | Method of desulfurizing hydrocarbon oil |
| CN101502792A (en) * | 2009-02-19 | 2009-08-12 | 北京化工大学 | Inorganic sensitized visible-light responsive photocatalyst and preparation method thereof |
| CN103342386A (en) * | 2013-07-12 | 2013-10-09 | 河南大学 | Preparation method of anatase titanium dioxide nanotubes |
| CN103990463A (en) * | 2014-05-21 | 2014-08-20 | 东华大学 | Preparation method of NiO/gamma-Al2O3 composite ceramic nanofiber photocatalytic material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB834460A (en) * | 1956-03-29 | 1960-05-11 | Standard Oil Co | Method of desulfurizing hydrocarbon oil |
| CN101502792A (en) * | 2009-02-19 | 2009-08-12 | 北京化工大学 | Inorganic sensitized visible-light responsive photocatalyst and preparation method thereof |
| CN103342386A (en) * | 2013-07-12 | 2013-10-09 | 河南大学 | Preparation method of anatase titanium dioxide nanotubes |
| CN103990463A (en) * | 2014-05-21 | 2014-08-20 | 东华大学 | Preparation method of NiO/gamma-Al2O3 composite ceramic nanofiber photocatalytic material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115888676A (en) * | 2022-09-28 | 2023-04-04 | 电子科技大学长三角研究院(湖州) | Composition for inhibiting decomposition of nitrate and preparation method thereof |
| CN115888676B (en) * | 2022-09-28 | 2024-05-14 | 电子科技大学长三角研究院(湖州) | Composition for inhibiting nitrate decomposition and preparation method thereof |
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