CN104437575A - Fluorine and nitrogen co-doped bismuth phosphate-nickel oxide compound photocatalyst and preparation method thereof - Google Patents
Fluorine and nitrogen co-doped bismuth phosphate-nickel oxide compound photocatalyst and preparation method thereof Download PDFInfo
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- CN104437575A CN104437575A CN201410613402.9A CN201410613402A CN104437575A CN 104437575 A CN104437575 A CN 104437575A CN 201410613402 A CN201410613402 A CN 201410613402A CN 104437575 A CN104437575 A CN 104437575A
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Abstract
The invention discloses a fluorine and nitrogen co-doped bismuth phosphate-nickel oxide compound photocatalyst. The fluorine and nitrogen co-doped bismuth phosphate-nickel oxide compound photocatalyst is composed of fluorine and nitrogen co-doped bismuth phosphate and nickel oxide, wherein the mol ratio of fluorine and nitrogen co-doped bismuth phosphate to nickel oxide is 1 to (0.2-1). The invention further discloses a preparation method of the fluorine and nitrogen co-doped bismuth phosphate-nickel oxide compound photocatalyst. The preparation method comprises the following steps: dispersing fluorine and nitrogen co-doped bismuth phosphate powder into a nickel salt solution; dropwise adding a sodium hydroxide solution and transferring the solution into a hydrothermal reaction kettle to carry out microwave hydrothermal treatment; naturally cooling to room temperature; and centrifugally separating, washing, drying and calcining the obtained product to obtain the fluorine and nitrogen co-doped bismuth phosphate-nickel oxide compound photocatalyst. Non-metal fluorine and nitrogen ions are co-doped so that the capability of capturing electrons of a bismuth phosphate semiconductor interface is effectively improved, and the migration efficiency of electron holes is enhanced; and the oxygen vacancy concentration of a bismuth phosphate semiconductor is increased so that the photocatalytic activity of photocatalysis of bismuth phosphate is improved.
Description
Technical field
The invention belongs to inorganic environment-friendly catalysis material technical field, be specifically related to a kind of fluorine, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, the invention still further relates to the preparation method of this composite photo-catalyst.
Background technology
There is high-quantum efficiency, the preparations and applicatio of the Photocatalytic material with high activity of solar energy can be made full use of, become the hot subject of materialogy, chemistry, the energy and environmental science extensive concern and research.Two key issues in catalysis material research improve the activity of photochemical catalyst and the absorbing wavelength expanding photochemical catalyst, the mentality of designing of thus all novel photocatalysis systems, all carry out for this two problems, from this purpose, novel photocatalysis systems most at present mainly concentrates on composite metal oxide and sulphur, nitrogen substituted compound based on this.The report relating to phosphate catalysis material is little, and phosphate has many characteristics being beneficial to catalytic activity, as phosphate structure good stability, higher relative to its Lacking oxygen Formation energy of metal oxide in light-catalyzed reaction system, this just causes Lacking oxygen defect in phosphate crystal little, namely complex centre quantity is few, and electronics is easily separated with hole, is conducive to the carrying out forming light-catalyzed reaction.Meanwhile, all can there is cavitation corrosion (ZnO, CdS and MoS in most catalysis material
2) and electrical corrosion (GaP, Cu
2o and GaN), and phosphate anion is high-valence state is difficult to be chemically reduced, not easily by photoetch, if the metal ion in phosphate is stable equally, just there is photoetch in this photochemical catalyst under light illumination hardly.And phosphate has larger negative electrical charge, very large inductive effect can be produced, thus be conducive to the transmission of light induced electron.In addition, phosphate surface and water have strong interaction, and according to thermodynamic principles, surface phosphoric acid root, when with hydrone effect, can produce strong effect with the proton in water, and then be conducive to the generation hydroxyl that dissociates of hydrone.
Bismuth phosphate, as the constitutionally stable phosphate semi-conducting material of one, has many application in fields such as the selective catalytic oxidation of optics, alkane, the catalytic oxidations of ammonia.Nearly 2 years, the research relating to bismuth phosphate photocatalyst had been reported, and how to improve the separative efficiency of bismuth phosphate light induced electron, and then improved the application of its photocatalytic activity to bismuth phosphate catalysis material and have certain scientific meaning.
Summary of the invention
The object of this invention is to provide a kind of fluorine, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, there is higher photocatalytic activity.
Another object of the present invention is to provide the preparation method of a kind of fluorine, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst.
The technical solution adopted in the present invention is, fluorine, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, be made up of fluorine, nitrogen co-doped bismuth phosphate and nickel oxide, and wherein the mol ratio of fluorine, nitrogen co-doped bismuth phosphate and nickel oxide is 1:0.2 ~ 1.
Feature of the present invention is also,
In fluorine, nitrogen co-doped bismuth phosphate, the mol ratio of bismuth ion, fluorine ion and Nitrogen ion is 1:0.5 ~ 1:0.5 ~ 1, and wherein the mol ratio of fluorine ion and Nitrogen ion is 1:1.
Another technical scheme of the present invention is, the preparation method of fluorine, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, specifically comprises the following steps:
Step 1: it is in the salpeter solution of 65% that five water bismuth nitrates are dissolved in mass concentration, obtains solution A; Phosphate is soluble in water, obtain solution B; Solution A and solution B are mixed and obtains solution C; Ammonium fluoride is added solution C, obtains solution D; Solution D is transferred to hydrothermal reaction kettle, and be placed in microwave reactor and utilize heating using microwave to 150 ~ 250 DEG C microwave hydrothermal process 1 ~ 3h, room temperature is naturally cooled to after taking-up, by the product centrifugation obtained, deionized water washs 3 times, in 80 DEG C of dry 12h, obtain fluorine, nitrogen co-doped bismuth phosphate powder;
Step 2: it is in the nickel salt solution of 0.01 ~ 0.1mol/L that fluorine step 1 obtained, nitrogen co-doped bismuth phosphate powder are scattered in concentration, obtains suspension E; Be that the sodium hydroxide solution of 0.1 ~ 1mol/L dropwise adds suspension E by concentration, obtain solution F; Solution F is transferred to hydrothermal reaction kettle, and be placed in microwave reactor and utilize heating using microwave to 120 ~ 200 DEG C microwave hydrothermal process 1 ~ 3h, room temperature is naturally cooled to after taking-up, by the product centrifugation obtained, deionized water washs 3 times, after 80 DEG C of dry 12h, be placed in Muffle furnace in 300 ~ 500 DEG C of calcining 1 ~ 3h, obtain fluorine, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst.
Feature of the present invention is also,
In step 1, the mass ratio of five water bismuth nitrates and nitric acid is 1:5 ~ 10; The mass ratio of phosphate and water is 1:5 ~ 10; In solution C, the mol ratio of bismuth ion and phosphate anion is 1:1; The mol ratio of bismuth ion and ammonium fluoride is 1:0.5 ~ 1.
In step 1, phosphate is one or more combinations of sodium phosphate, dibastic sodium phosphate, sodium dihydrogen phosphate, potassium phosphate, potassium hydrogen phosphate or potassium dihydrogen phosphate.
In step 2, the mol ratio of bismuth atom and nickle atom is 1:0.2 ~ 1; The mol ratio of nickle atom and NaOH is 1:1 ~ 2.
In step 2, nickel salt is one or more combinations of six water nickel nitrates, six water Nickel Chlorides, nickelous sulfate or organic nickel.
The invention has the beneficial effects as follows,
1. fluorine of the present invention, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst have following characteristics: the capture ability that the first, effectively improve bismuth phosphate interface place electronics by nonmetal fluorine and Nitrogen ion codope, strengthen the transport efficiency of electron hole; The second, oxygen vacancy concentration in bismuth phosphate semiconductor can be increased by nonmetallic ion-doped, and then improve the light-catalysed photocatalytic activity of bismuth phosphate; Three, n-type semiconductor bismuth phosphate and p-type semiconductor nickel oxide can form the heterogeneous joint of p-n in interface, effectively promote the separation of photo-generated carrier, and then improve compound system photocatalytic activity.
2. the preparation method of fluorine of the present invention, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, adopt doping type bismuth phosphate/nickel oxide composite photo-catalyst, the photocatalytic activity of compound system effectively can be improved by fluorine, load that is nitrogen co-doped and nickel oxide, and its preparation method is simple, easy to operate.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
Fluorine of the present invention, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, be made up of fluorine, nitrogen co-doped bismuth phosphate and nickel oxide, and wherein the mol ratio of fluorine, nitrogen co-doped bismuth phosphate and nickel oxide is 1:0.2 ~ 1.
In fluorine, nitrogen co-doped bismuth phosphate, the mol ratio of bismuth ion, fluorine ion and Nitrogen ion is 1:0.5 ~ 1:0.5 ~ 1, and wherein the mol ratio of fluorine ion and Nitrogen ion is 1:1.
The preparation method of fluorine of the present invention, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, specifically comprises the following steps:
Step 1: five water bismuth nitrates being dissolved in mass concentration is (mass ratio of five water bismuth nitrates and nitric acid is 1:5 ~ 10) in the salpeter solution of 65%, obtains solution A; By (mass ratio of phosphate and water is 1:5 ~ 10) soluble in water for phosphate, obtain solution B; Solution A and solution B are mixed and obtains solution C (in solution C, the mol ratio of bismuth ion and phosphate anion is 1:1); Ammonium fluoride is added solution C (mol ratio of bismuth ion and ammonium fluoride is 1:0.5 ~ 1), obtain solution D; Solution D is transferred to hydrothermal reaction kettle, and be placed in microwave reactor and utilize heating using microwave to 150 ~ 250 DEG C microwave hydrothermal process 1 ~ 3h, room temperature is naturally cooled to after taking-up, by the product centrifugation obtained, deionized water washs 3 times, in 80 DEG C of dry 12h, obtain fluorine, nitrogen co-doped bismuth phosphate powder;
In step 1, phosphate is one or more combinations of sodium phosphate, dibastic sodium phosphate, sodium dihydrogen phosphate, potassium phosphate, potassium hydrogen phosphate or potassium dihydrogen phosphate;
Step 2: it is (mol ratio of bismuth atom and nickle atom is 1:0.2 ~ 1) in the nickel salt solution of 0.01 ~ 0.1mol/L that fluorine step 1 obtained, nitrogen co-doped bismuth phosphate powder are scattered in concentration, obtains suspension E; Be that the sodium hydroxide solution of 0.1 ~ 1mol/L dropwise adds suspension E (mol ratio of nickle atom and NaOH is 1:1 ~ 2) by concentration, obtain solution F; Solution F is transferred to hydrothermal reaction kettle, and be placed in microwave reactor and utilize heating using microwave to 120 ~ 200 DEG C microwave hydrothermal process 1 ~ 3h, room temperature is naturally cooled to after taking-up, by the product centrifugation obtained, deionized water washs 3 times, after 80 DEG C of dry 12h, be placed in Muffle furnace in 300 ~ 500 DEG C of calcining 1 ~ 3h, obtain fluorine, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst.
In step 2, nickel salt is one or more combinations of six water nickel nitrates, six water Nickel Chlorides, nickelous sulfate or organic nickel.
Fluorine of the present invention, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst have following characteristics: the capture ability that the first, effectively improve bismuth phosphate interface place electronics by nonmetal fluorine and Nitrogen ion codope, strengthen the transport efficiency of electron hole; The second, oxygen vacancy concentration in bismuth phosphate semiconductor can be increased by nonmetallic ion-doped, and then improve the light-catalysed photocatalytic activity of bismuth phosphate; Three, n-type semiconductor bismuth phosphate and p-type semiconductor nickel oxide can form the heterogeneous joint of p-n in interface, effectively promote the separation of photo-generated carrier, and then improve compound system photocatalytic activity.
The preparation method of fluorine of the present invention, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, adopt doping type bismuth phosphate/nickel oxide composite photo-catalyst, the photocatalytic activity of compound system effectively can be improved by fluorine, load that is nitrogen co-doped and nickel oxide, and its preparation method is simple, easy to operate.
Embodiment 1
It is in the salpeter solution of 65% that 4.85g five water bismuth nitrate is dissolved in 24.25g concentration, obtains solution A; 1.64g sodium phosphate is dissolved in 8.2g water, obtains solution B; Solution A and solution B are mixed and obtains solution C, 0.185g ammonium fluoride is added in solution C to stir obtain solution D; Solution D is transferred to hydrothermal reaction kettle, is placed in microwave reactor and utilizes heating using microwave to 150 DEG C microwave hydrothermal process 1h, after taking-up, naturally cool to room temperature, by the product centrifugation obtained, deionized water washs 3 times, in 80 DEG C of dry 12h, obtains fluorine, nitrogen co-doped bismuth phosphate powder;
By 3.04g fluorine, it is obtain suspension E in the six water nickel nitrate solutions of 0.01mol/L that nitrogen co-doped bismuth phosphate powder is scattered in 200mL concentration, be that the sodium hydroxide solution of 0.1mol/L dropwise joins in suspension E by 20mL concentration, solution F is obtained after stirring, solution F is transferred to hot water reaction still, and be placed in microwave reactor and utilize heating using microwave to 120 DEG C microwave hydrothermal process 1h, room temperature is naturally cooled to after taking-up, the product centrifugation obtained is washed 3 times, after 80 DEG C of dry 12h, be placed in Muffle furnace again in 300 DEG C of calcining 1h, obtain fluorine, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst.
Prepared by fluorine to embodiment 1, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst carries out light degradation experiment, selection methyl orange is target contaminant, above-mentioned for 0.02g composite photocatalyst material is added the methyl orange solution that 100mL concentration is 10mg/L, after 50min UV-irradiation (300W mercury lamp), methyl orange degradation efficiency is greater than 90%.
Embodiment 2
It is in the salpeter solution of 65% that 4.85g five water bismuth nitrate is dissolved in 48.5g concentration, obtains solution A; 1.64g sodium phosphate is dissolved in 16.4g water, obtains solution B; Solution A and solution B are mixed and obtains solution C, 0.37g ammonium fluoride is added in solution C to stir obtain solution D; Solution D is transferred to hydrothermal reaction kettle, is placed in microwave reactor and utilizes heating using microwave to 250 DEG C microwave hydrothermal process 3h, after taking-up, naturally cool to room temperature, by the product centrifugation obtained, deionized water washs 3 times, in 80 DEG C of dry 12h, obtains fluorine, nitrogen co-doped bismuth phosphate powder;
By 3.04g fluorine, it is obtain suspension E in the six water nickel nitrate solutions of 0.1mol/L that nitrogen co-doped bismuth phosphate powder is scattered in 100mL concentration, be that the sodium hydroxide solution of 1mol/L dropwise joins in suspension E by 20mL concentration, solution F is obtained after stirring, solution F is transferred to hot water reaction still, and be placed in microwave reactor and utilize heating using microwave to 200 DEG C microwave hydrothermal process 3h, room temperature is naturally cooled to after taking-up, the product centrifugation obtained is washed 3 times, after 80 DEG C of dry 12h, be placed in Muffle furnace again in 500 DEG C of calcining 3h, obtain fluorine, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst.
Prepared by fluorine to embodiment 2, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst carries out light degradation experiment, selection methyl orange is target contaminant, above-mentioned for 0.02g composite photocatalyst material is added the methyl orange solution that 100mL concentration is 10mg/L, after 50min UV-irradiation (300W mercury lamp), methyl orange degradation efficiency is greater than 90%.
Embodiment 3
It is in the salpeter solution of 65% that 4.85g five water bismuth nitrate is dissolved in 38.8g concentration, obtains solution A; 1.64g sodium phosphate is dissolved in 12.3g water, obtains solution B; Solution A and solution B are mixed and obtains solution C, 0.259g ammonium fluoride is added in solution C to stir obtain solution D; Solution D is transferred to hydrothermal reaction kettle, is placed in microwave reactor and utilizes heating using microwave to 200 DEG C microwave hydrothermal process 2h, after taking-up, naturally cool to room temperature, by the product centrifugation obtained, deionized water washs 3 times, in 80 DEG C of dry 12h, obtains fluorine, nitrogen co-doped bismuth phosphate powder;
By 3.04g fluorine, it is obtain suspension E in the six water nickel nitrate solutions of 0.05mol/L that nitrogen co-doped bismuth phosphate powder is scattered in 10mL concentration, be that the sodium hydroxide solution of 0.5mol/L dropwise joins in suspension E by 20mL concentration, solution F is obtained after stirring, solution F is transferred to hot water reaction still, and be placed in microwave reactor and utilize heating using microwave to 150 DEG C microwave hydrothermal process 2h, room temperature is naturally cooled to after taking-up, the product centrifugation obtained is washed 3 times, after 80 DEG C of dry 12h, be placed in Muffle furnace again in 400 DEG C of calcining 2h, obtain fluorine, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst.
Prepared by fluorine to embodiment 3, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst carries out light degradation experiment, selection methyl orange is target contaminant, above-mentioned for 0.02g composite photocatalyst material is added the methyl orange solution that 100mL concentration is 10mg/L, after 50min UV-irradiation (300W mercury lamp), methyl orange degradation efficiency is greater than 90%.
Embodiment 4
It is in the salpeter solution of 65% that 4.85g five water bismuth nitrate is dissolved in 29.1g concentration, obtains solution A; 1.64g sodium phosphate is dissolved in 14.76g water, obtains solution B; Solution A and solution B are mixed and obtains solution C, 0.296g ammonium fluoride is added in solution C to stir obtain solution D; Solution D is transferred to hydrothermal reaction kettle, is placed in microwave reactor and utilizes heating using microwave to 175 DEG C microwave hydrothermal process 2.5h, after taking-up, naturally cool to room temperature, by the product centrifugation obtained, deionized water washs 3 times, in 80 DEG C of dry 12h, obtains fluorine, nitrogen co-doped bismuth phosphate powder;
By 3.04g fluorine, it is obtain suspension E in the six water nickel nitrate solutions of 0.1mol/L that nitrogen co-doped bismuth phosphate powder is scattered in 80mL concentration, be that the sodium hydroxide solution of 0.8mol/L dropwise joins in suspension E by 20mL concentration, solution F is obtained after stirring, solution F is transferred to hot water reaction still, and be placed in microwave reactor and utilize heating using microwave to 180 DEG C microwave hydrothermal process 2.5h, room temperature is naturally cooled to after taking-up, the product centrifugation obtained is washed 3 times, after 80 DEG C of dry 12h, be placed in Muffle furnace again in 450 DEG C of calcining 1.5h, obtain fluorine, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst.
Prepared by fluorine to embodiment 4, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst carries out light degradation experiment, selection methyl orange is target contaminant, above-mentioned for 0.02g composite photocatalyst material is added the methyl orange solution that 100mL concentration is 10mg/L, after 50min UV-irradiation (300W mercury lamp), methyl orange degradation efficiency is greater than 90%.
In embodiment 4, phosphate is sodium phosphate, and phosphate also can be one or more combinations of sodium phosphate, dibastic sodium phosphate, sodium dihydrogen phosphate, potassium phosphate, potassium hydrogen phosphate or potassium dihydrogen phosphate.
In embodiment 4, nickel salt is six water nickel nitrates, also can be one or more combinations of six water nickel nitrates, six water Nickel Chlorides, nickelous sulfate or organic nickel.
Claims (7)
1. fluorine, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, is characterized in that, is made up of fluorine, nitrogen co-doped bismuth phosphate and nickel oxide, and wherein the mol ratio of fluorine, nitrogen co-doped bismuth phosphate and nickel oxide is 1:0.2 ~ 1.
2. fluorine according to claim 1, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, it is characterized in that, in fluorine, nitrogen co-doped bismuth phosphate, the mol ratio of bismuth ion, fluorine ion and Nitrogen ion is 1:0.5 ~ 1:0.5 ~ 1, and wherein the mol ratio of fluorine ion and Nitrogen ion is 1:1.
3. the preparation method of fluorine according to claim 1, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, is characterized in that, specifically comprise the following steps:
Step 1: it is in the salpeter solution of 65% that five water bismuth nitrates are dissolved in mass concentration, obtains solution A; Phosphate is soluble in water, obtain solution B; Solution A and solution B are mixed and obtains solution C; Ammonium fluoride is added solution C, obtains solution D; Solution D is transferred to hydrothermal reaction kettle, and be placed in microwave reactor and utilize heating using microwave to 150 ~ 250 DEG C microwave hydrothermal process 1 ~ 3h, room temperature is naturally cooled to after taking-up, by the product centrifugation obtained, deionized water washs 3 times, in 80 DEG C of dry 12h, obtain fluorine, nitrogen co-doped bismuth phosphate powder;
Step 2: it is in the nickel salt solution of 0.01 ~ 0.1mol/L that fluorine step 1 obtained, nitrogen co-doped bismuth phosphate powder are scattered in concentration, obtains suspension E; Be that the sodium hydroxide solution of 0.1 ~ 1mol/L dropwise adds suspension E by concentration, obtain solution F; Solution F is transferred to hydrothermal reaction kettle, and be placed in microwave reactor and utilize heating using microwave to 120 ~ 200 DEG C microwave hydrothermal process 1 ~ 3h, room temperature is naturally cooled to after taking-up, by the product centrifugation obtained, deionized water washs 3 times, after 80 DEG C of dry 12h, be placed in Muffle furnace in 300 ~ 500 DEG C of calcining 1 ~ 3h, obtain fluorine, nitrogen co-doped bismuth phosphate/nickel oxide composite photo-catalyst.
4. the preparation method of fluorine according to claim 3, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, is characterized in that, in step 1, the mass ratio of five water bismuth nitrates and nitric acid is 1:5 ~ 10; The mass ratio of phosphate and water is 1:5 ~ 10; In solution C, the mol ratio of bismuth ion and phosphate anion is 1:1; The mol ratio of bismuth ion and ammonium fluoride is 1:0.5 ~ 1.
5. the preparation method of the fluorine according to claim 3 or 4, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, it is characterized in that, in step 1, phosphate is one or more combinations of sodium phosphate, dibastic sodium phosphate, sodium dihydrogen phosphate, potassium phosphate, potassium hydrogen phosphate or potassium dihydrogen phosphate.
6. the preparation method of fluorine according to claim 3, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, is characterized in that, in step 2, the mol ratio of bismuth atom and nickle atom is 1:0.2 ~ 1; The mol ratio of nickle atom and NaOH is 1:1 ~ 2.
7. the preparation method of the fluorine according to claim 3 or 6, nitrogen co-doped bismuth phosphate-nickel oxide composite photo-catalyst, is characterized in that, in step 2, nickel salt is one or more combinations of six water nickel nitrates, six water Nickel Chlorides, nickelous sulfate or organic nickel.
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| CN116713009A (en) * | 2023-06-06 | 2023-09-08 | 常州大学 | Preparation method and application of ZnCdS/NiO composite photocatalyst |
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