CN103157477A - Nickel oxide doped sodium titanate-titanium dioxide composite photocatalyst and preparation method thereof - Google Patents
Nickel oxide doped sodium titanate-titanium dioxide composite photocatalyst and preparation method thereof Download PDFInfo
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- CN103157477A CN103157477A CN2013100996126A CN201310099612A CN103157477A CN 103157477 A CN103157477 A CN 103157477A CN 2013100996126 A CN2013100996126 A CN 2013100996126A CN 201310099612 A CN201310099612 A CN 201310099612A CN 103157477 A CN103157477 A CN 103157477A
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Abstract
The invention provides a nickel oxide doped sodium titanate-titanium dioxide composite photocatalyst and a preparation method thereof. The method comprises the following steps of: growing in situ a supported titanium dioxide nano film on a foamed nickel substrate by taking titanium salt as a precursor; drying and calcining, and immersing in a sodium hydroxide solution; and performing a hydrothermal reaction to grow a sodium titanate-titanium dioxide-nickel oxide composite film on the surface, wherein in the film, sodium titanate-titanium dioxide exists in the form of nanosheet or nanotube array, and nickel oxide nano particles are uniformly dispersed on the surface of the film. Since the sodium titanium is a lamellar structure with charges on the laminate and the p-type semiconductor nickel oxide is uniformly doped, the photocatalysis efficiency of the composite material is obviously improved. Meanwhile, the nano array type photocatalyst based on a foamed nickel substrate increases the specific surface area of the catalyst, reduces the mass transfer resistance, overcomes the shortcomings of easy agglomeration, easy loss and difficult recover of a powder photocatalyst, and facilitates the regeneration and utilization of the catalyst.
Description
Technical field
The present invention relates to the composite photo-catalyst technology of preparing, be specifically related to a kind of nickel oxide doped titanic acid sodium-titanium dioxide composite photocatalyst and preparation method thereof.
Technical background
Photocatalysis technology is an environmental friendliness technology, has a extensive future in depollution of environment field.Research at present photochemical catalyst the most widely is nano-TiO
2, because its preparation technology is simple, with low cost, have high activity, good chemical stability and characteristics such as heat endurance, safety non-toxic, be the environmental protection catalyst that has DEVELOPMENT PROSPECT.Layered titanic acid sodium material has crystal structure and the performance approximate with titanium dioxide simultaneously, and it also possesses special layer structure, laminate is with negative electrical charge, be a kind of important solid functional material, have broad application prospects at numerous areas such as catalysis, absorption, ion-exchange, separation and conduction.
At present, for TiO
2The preparation of powder photocatalyst and modification TiO
2The research of powder photocatalyst is comparative maturity, but because the trickle easy generation of titanium dioxide powder particle is reunited, easy and waste water formation suspension in photocatalytic process, cause separation difficulty, easily loss is difficult to reclaim, the regeneration and the recycling that are unfavorable for catalyst have limited titanium dioxide to a certain extent in industrial extensive utilization, for this reason a lot of research preparation loaded photocatalysts.Appl Surf Sci, in 2010,257,367-371, the employing magnetron sputtering method such as C.uinones is splashed to TiO with the Au/Pd bimetallic
2Prepared Au/Pd modification TiO on thin slice
2Catalysis material.Su Ying-ying etc. are at China Environ Sci, and choosing in 2009,29,1171-1176 and getting diatomite is carrier, take tetraisopropyl titanate as predecessor, adopt sol-gel process to prepare TiO
2/ diatomite photochemical catalyst.The people such as Negishi are at Sol-Gel Sci.Technol., in 2001,22,23-31 take isopropyl titanate as raw material, with sol-gel process in load on glass TiO
2Film, still, TiO
2After photochemical catalyst is fixed, with TiO
2Powder is compared photocatalysis efficiency in various degree reduction, and this is because the rear catalyst specific area that is fixed reduces to make its suction-operated and utilization rate to reduce, and has reduced TiO
2Photocatalytic activity.
Therefore, we adopt the larger nickel foam of specific area as substrate, at its superficial growth sodium titanate-titanium dioxide nanoplate or nano-tube array formula composite construction, surface uniform is dispersed with nickel oxide nanoparticle, in formation, the p-n hetero-junctions not only can be expanded by sensibilization the wave-length coverage of wide band gap semiconducter, and it is compound to suppress carrier by built in field, increases substantially the catalysis material performance of material.
Summary of the invention
The purpose of this invention is to provide a kind of nickel oxide doped titanic acid sodium-titanium dioxide composite photocatalyst and preparation method thereof.
Nickel oxide doped titanic acid sodium-titanium dioxide composite photocatalyst provided by the invention is: take nickel foam as substrate, at its superficial growth sodium titanate-titanium dioxide-nickel oxide laminated film, this film is that sodium titanate-titanium dioxide exists with nanometer sheet or nano-tube array form, and its surface uniform is dispersed with nickel oxide nanoparticle, this composite has advantages of the structure homogeneous, has catalytic activity used as photochemical catalyst high, stable, segregative characteristics.
The preparation method of nickel oxide doped titanic acid sodium-titanium dioxide composite photocatalyst provided by the invention is:
A. nickel foam sheet pretreatment
The nickel foam sheet is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry rises to 400-600 ℃ of calcining with the heating rate of 5 ℃/min and carried out pre-oxidation in 10-30 minute in air atmosphere.
B. carried titanium dioxide on nickel substrate
Dose volume stirs in reactor than for the alcohol of 8-10:4-5:1, acid, butyl titanate mixed solution join, put into the pretreated nickel foam sheet of steps A, sealing, in 100-140 ℃ of heating 5-15 hour, the nature cooling down, take out oven dry, the heating rate with 2 ℃/min in air atmosphere rises to 400-600 ℃ of calcining 30-60 minute, obtains foamed nickel supported titanium dioxide nano-film; Described alcohol is: a kind of in ethanol, propyl alcohol, butanols or ethylene glycol; Acid is: a kind of in acetic acid or propionic acid;
C. load sodium titanate-titanium dioxide on nickel foam
The sodium hydroxide solution of preparation 5-15mol/L adds the foamed nickel supported titanium dioxide nano-film of putting into step B preparation after stirring in reactor, in 100-160 ℃ of heating 2-24 hour, after natural cooling down, takes out, with deionized water washing, oven dry; Obtain nickel oxide doped titanic acid sodium-composite titania material, this material can be used as photochemical catalyst.
Fig. 1, Fig. 2 is embodiment 1 SEM (SEM) photograph that obtains sample and transmission electron microscope (TEM) photograph that scrapes rear sample from nickel substrate, composite construction is grown in the nickel foam substrate with sodium titanate-titanium dioxide nanoplate array format as seen from the figure, and its surface uniform is dispersed with nickel oxide nanoparticle.
Fig. 3, Fig. 4 is embodiment 2 SEM (SEM) photograph that obtains sample and transmission electron microscope (TEM) photograph that scrapes rear sample from nickel substrate, composite construction is grown in the nickel foam substrate with sodium titanate-Nano tube array of titanium dioxide form as seen from the figure, and its surface uniform is dispersed with nickel oxide nanoparticle.
Fig. 5 is high resolution transmission electron microscopy (HRTEM) photograph that obtains sample, can find out that spacing of lattice is 0.8nm, and the spacing of lattice of sodium titanate is complementary; The spacing of lattice that diameter is about the nano particle about 10nm is 0.35nm, and the spacing of lattice of titanium dioxide is complementary; The spacing of lattice that diameter is about the nano particle of about 3nm is 0.2nm, and the spacing of lattice of nickel oxide is complementary, and further proves the structure of composite.
The photoactivation degradation of dye is a kind of important method of Fast Evaluation photochemical catalyst catalytic effect.Fig. 6 is that the sample photocatalytic degradation 100mL concentration with embodiment 1 is the photocatalysis effect figure of 1.1mg/L rhodamine B (RhB) and malachite green (MG).This material is due to the ingenious special construction that combines the good electron transport ability of nickel substrate and lamellar compound, make this array composite construction at the dye molecule (RhB of positively charged, MG) the light degradation field shows catalytic performance preferably, as to the photocatalytic degradation efficiency of rhodamine B more than 99%, catalytic effect is better than TiO
2, and have good structural stability.
Beneficial effect of the present invention: the inventive method adopts the larger nickel foam of specific area as substrate, array sodium titanate-the titanium dioxide composite photocatalyst of preparation Y-oxides doping, complete under simple hydrothermal condition, its advantage is that synthetic method is simple, with low cost, good reproducibility, size uniform.The use of bigger serface substrate is conducive to molecular diffusion, improves load quality, and catalyst is disperseed equably; The Uniform Doped of p-type semiconductor oxide nickel and n-type semiconductor metatitanic acid sodium-titanium dioxide forms p-n junction, can stop the compound of light induced electron and hole, has improved significantly the photocatalysis efficiency of composite; The array architecture that forms at last increases specific area and the active site of catalyst, has reduced resistance to mass tranfer, makes the array optical catalyst be easy to separate, and realizes catalyst regeneration and recycling.
Description of drawings
Fig. 1 is the SEM picture of embodiment 1;
Fig. 2 is the TEM picture of embodiment 1;
Fig. 3 is the SEM picture of embodiment 2;
Fig. 4 is the TEM picture of embodiment 2;
Fig. 5 is the HRTEM picture of embodiment 1;
Fig. 6 is the photocatalysis effect figure of sample in embodiment 1.
The specific embodiment
Embodiment 1
A. nickel foam is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry.Heating rate with 5 ℃/min in air rises to 550 ℃ of calcining 10min pre-oxidation treatment.
B. with ethanol 20mL, acetic acid 10mL, butyl titanate 2mL joins in reactor and stirs, and puts into the nickel foam after processing of step A, sealing.Reactor, is dried after natural cooling down in 120 ℃ of heating 10h.Heating rate with 2 ℃/min rises to 550 ℃ of calcining 45min in air atmosphere again, obtains foamed nickel supported titanium dioxide nano-film.
C. prepare the sodium hydroxide solution of 10mol/L, put into the foamed nickel supported titanium dioxide nano-film sample that step B obtains, 100 ℃ of heating 9h.After reactor nature cooling down, take out, with the deionized water washing, oven dry obtains required sample.
A. nickel foam is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry.Heating rate with 5 ℃/min in air rises to 550 ℃ of calcining 10min pre-oxidation treatment.
B. with ethanol 20mL, acetic acid 10mL, butyl titanate 2mL joins in reactor and stirs, and puts into the nickel foam after processing of step A, sealing.Reactor, is dried after natural cooling down in 120 ℃ of heating 10h.Heating rate with 2 ℃/min rises to 550 ℃ of calcining 45min in air atmosphere again, obtains foamed nickel supported titanium dioxide nano-film.
C. prepare the sodium hydroxide solution of 10mol/L, put into the foamed nickel supported titanium dioxide nano-film sample that step B obtains, 160 ℃ of heating 9h.After reactor nature cooling down, take out, with the deionized water washing, oven dry obtains required sample.
Embodiment 3
A. nickel foam is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry.Heating rate with 5 ℃/min in air rises to 400 ℃ of calcining 10min pre-oxidation treatment.
B. with propyl alcohol 16mL, acetic acid 8mL, butyl titanate 2mL joins in reactor and stirs, and puts into the nickel foam after processing of step A, sealing.Reactor, is dried after natural cooling down in 100 ℃ of heating 15h.Heating rate with 2 ℃/min rises to 400 ℃ of calcining 30min in air atmosphere again, obtains foamed nickel supported titanium dioxide nano-film.
C. prepare the sodium hydroxide solution of 5mol/L, put into the foamed nickel supported titanium dioxide nano-film sample that step B obtains, 100 ℃ of heating 8h.After reactor nature cooling down, take out, with the deionized water washing, oven dry obtains required sample.
Embodiment 4
A. nickel foam is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry.Heating rate with 5 ℃/min in air rises to 450 ℃ of calcining 20min pre-oxidation treatment.
B. with butanols 18mL, propionic acid 10mL, butyl titanate 2mL joins in reactor and stirs, and puts into the nickel foam after processing of step A, sealing.Reactor, is dried after natural cooling down in 120 ℃ of heating 10h.Heating rate with 2 ℃/min rises to 450 ℃ of calcining 40min in air atmosphere again, obtains foamed nickel supported titanium dioxide nano-film.
C. prepare the sodium hydroxide solution of 8mol/L, put into the foamed nickel supported titanium dioxide nano-film sample that step B obtains, 120 ℃ of heating 12h.After reactor nature cooling down, take out, with the deionized water washing, oven dry obtains required sample.
Embodiment 5
A. nickel foam is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry.Heating rate with 5 ℃/min in air rises to 500 ℃ of calcining 30min pre-oxidation treatment.
B. with ethanol 16mL, acetic acid 8mL, butyl titanate 2mL joins in reactor and stirs, and puts into the nickel foam after processing of step A, sealing.Reactor, is dried after natural cooling down in 140 ℃ of heating 5h.Heating rate with 2 ℃/min rises to 500 ℃ of calcining 40min in air atmosphere again, obtains foamed nickel supported titanium dioxide nano-film.
C. prepare the sodium hydroxide solution of 15mol/L, put into the foamed nickel supported titanium dioxide nano-film sample that step B obtains, 140 ℃ of heating 20h.After reactor nature cooling down, take out, with the deionized water washing, oven dry obtains required sample.
Embodiment 6
A. nickel foam is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry.Heating rate with 5 ℃/min in air rises to 600 ℃ of calcining 10min pre-oxidation treatment.
B. with ethylene glycol 20mL, acetic acid 10mL, butyl titanate 2mL joins in reactor and stirs, and puts into the nickel foam after processing of step A, sealing.Reactor, is dried after natural cooling down in 140 ℃ of heating 10h.Heating rate with 2 ℃/min rises to 600 ℃ of calcining 30min in air atmosphere again, obtains foamed nickel supported titanium dioxide nano-film.
C. prepare the sodium hydroxide solution of 10mol/L, put into the foamed nickel supported titanium dioxide nano-film sample that step B obtains, 100 ℃ of heating 24h.After reactor nature cooling down, take out, with the deionized water washing, oven dry obtains required sample.
Claims (2)
1. the preparation method of a nickel oxide doped titanic acid sodium-titanium dioxide composite photocatalyst, concrete steps are as follows:
A. nickel foam sheet pretreatment
The nickel foam sheet is cut into different size and shapes on demand, processes with absolute ethyl alcohol, deionized water supersound washing and remove surface impurity, oven dry rises to 400-600 ℃ of calcining with the heating rate of 5 ℃/min and carried out pre-oxidation in 10-30 minute in air atmosphere;
B. carried titanium dioxide on nickel substrate
Dose volume stirs in reactor than for the alcohol of 8-10:4-5:1, acid, butyl titanate mixed solution join, put into the pretreated nickel foam sheet of steps A, sealing, in 100-140 ℃ of heating 5-15 hour, the nature cooling down, take out oven dry, the heating rate with 2 ℃/min in air atmosphere rises to 400-600 ℃ of calcining 30-60 minute, obtains foamed nickel supported titanium dioxide nano-film; Described alcohol is: a kind of in ethanol, propyl alcohol, butanols or ethylene glycol; Acid is: a kind of in acetic acid or propionic acid;
C. load sodium titanate-titanium dioxide on nickel foam
The sodium hydroxide solution of preparation 5-15mol/L adds the foamed nickel supported titanium dioxide nano-film of putting into step B preparation after stirring in reactor, in 100-160 ℃ of heating 2-24 hour, after natural cooling down, takes out, with deionized water washing, oven dry; Obtain nickel substrate sodium titanate-titania additive NiO composite, this material can be used as photochemical catalyst.
2. the nickel oxide doped titanic acid sodium-titanium dioxide composite photocatalyst of method according to claim 1 preparation: this catalyst is take nickel foam as substrate, at its superficial growth sodium titanate-titanium dioxide-nickel oxide laminated film, this film is that sodium titanate-titanium dioxide exists with nanometer sheet or nano-tube array form, and its surface uniform is dispersed with nickel oxide nanoparticle.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016532555A (en) * | 2013-09-06 | 2016-10-20 | 日東電工株式会社 | High surface area photocatalytic material and production method |
| CN107243353A (en) * | 2016-08-10 | 2017-10-13 | 山东大学 | A kind of titanium dioxide multi-level structure photochemical catalyst of Fluorin doped and preparation method thereof |
| CN108630812A (en) * | 2017-03-17 | 2018-10-09 | 中国科学院宁波材料技术与工程研究所 | Application of the rhodamine material in organic solar batteries |
| CN110013824A (en) * | 2019-04-24 | 2019-07-16 | 吉林师范大学 | Membranaceous two-dimensional nano thin layer sodium titanate covering silver oxide/titanium oxide heterojunction photocatalysis membrana layer material in ground and preparation method thereof |
| CN110773172A (en) * | 2019-11-20 | 2020-02-11 | 河南工程学院 | Nickel oxide @ titanium dioxide catalytic material with three-dimensional network core-shell structure and preparation method |
| CN112158853A (en) * | 2020-09-14 | 2021-01-01 | 宜兴国际环保城科技发展有限公司 | Tubular free radical oxidant and preparation method thereof |
| CN112675859A (en) * | 2021-01-28 | 2021-04-20 | 华南农业大学 | Foam nickel-based titanium dioxide nano composite material and preparation method and application thereof |
| CN112791726A (en) * | 2021-02-20 | 2021-05-14 | 华南农业大学 | Foamed nickel substrate in-situ loaded titanium dioxide nanowire array material and preparation method and application thereof |
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Cited By (11)
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|---|---|---|---|---|
| JP2016532555A (en) * | 2013-09-06 | 2016-10-20 | 日東電工株式会社 | High surface area photocatalytic material and production method |
| CN107243353A (en) * | 2016-08-10 | 2017-10-13 | 山东大学 | A kind of titanium dioxide multi-level structure photochemical catalyst of Fluorin doped and preparation method thereof |
| CN107243353B (en) * | 2016-08-10 | 2019-11-22 | 山东大学 | A kind of titanium dioxide multi-level structure photochemical catalyst of Fluorin doped and preparation method thereof |
| CN108630812A (en) * | 2017-03-17 | 2018-10-09 | 中国科学院宁波材料技术与工程研究所 | Application of the rhodamine material in organic solar batteries |
| CN110013824A (en) * | 2019-04-24 | 2019-07-16 | 吉林师范大学 | Membranaceous two-dimensional nano thin layer sodium titanate covering silver oxide/titanium oxide heterojunction photocatalysis membrana layer material in ground and preparation method thereof |
| CN110773172A (en) * | 2019-11-20 | 2020-02-11 | 河南工程学院 | Nickel oxide @ titanium dioxide catalytic material with three-dimensional network core-shell structure and preparation method |
| CN112158853A (en) * | 2020-09-14 | 2021-01-01 | 宜兴国际环保城科技发展有限公司 | Tubular free radical oxidant and preparation method thereof |
| CN112158853B (en) * | 2020-09-14 | 2023-05-23 | 宜兴国际环保城科技发展有限公司 | Tubular free radical oxidant and preparation method thereof |
| CN112675859A (en) * | 2021-01-28 | 2021-04-20 | 华南农业大学 | Foam nickel-based titanium dioxide nano composite material and preparation method and application thereof |
| CN112791726A (en) * | 2021-02-20 | 2021-05-14 | 华南农业大学 | Foamed nickel substrate in-situ loaded titanium dioxide nanowire array material and preparation method and application thereof |
| CN112791726B (en) * | 2021-02-20 | 2022-03-25 | 华南农业大学 | Foamed nickel substrate in-situ loaded titanium dioxide nanowire array material and preparation method and application thereof |
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