CN105126803A - Preparation method of strontium titanate/graphene composite nanometer catalyst - Google Patents
Preparation method of strontium titanate/graphene composite nanometer catalyst Download PDFInfo
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- CN105126803A CN105126803A CN201510526251.8A CN201510526251A CN105126803A CN 105126803 A CN105126803 A CN 105126803A CN 201510526251 A CN201510526251 A CN 201510526251A CN 105126803 A CN105126803 A CN 105126803A
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Abstract
The invention relates to a preparation method of strontium titanate/graphene composite nanometer catalyst. According to the preparation method disclosed by the invention, a wet chemical reaction method is adopted. The preparation comprises the steps of: using oxyhydroxide of titanium as a titanium source, using strontium nitrate as a strontium source, using ethanolamine as a solvent, using potassium hydroxide as a mineralizer, and thoroughly mixing the oxyhydroxide of the titanium, the strontium nitrate, the ethanolamine, the potassium hydroxide and an oxidized graphene aqueous solution so as to obtain a mixture; and performing a hydrothermal reaction to obtain strontium titanate/graphene nanometer powder. The preparation method disclosed by the invention is simple in technology process, easy to control, free from pollution and low in cost. The prepared strontium titanate/graphene composite nanometer catalyst is high in purity and good in crystallinity.
Description
Technical field
The present invention relates to the preparation method of strontium titanates/Graphene composite nano-catalyst, belong to field of inorganic nonmetallic material.
Background technology
Strontium titanates is a kind of metal oxide of typical perovskite structure, and its energy gap is 3.2eV, is a kind of semiconductor light-catalyst material with larger application potential.Graphene is that one passes through sp by carbon atom
2the Two-dimensional Carbon material of the monoatomic layer thickness of hydridization composition; It has superpower electric conductivity, thermal conductance, electron transport property simultaneously, is a kind of ideal carrier forming functional semiconductor catalytic composite material.At present, for the research of the composite catalyst of strontium titanates and Graphene, be still in the exploratory stage, be showed no relevant report both at home and abroad.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, process is easy to the preparation method of the strontium titanates/Graphene composite nano-catalyst controlled.
The preparation method of strontium titanates/graphene composite nano material of the present invention, employing be wet-chemical reaction method, comprise following processing step:
1) butyl titanate is dissolved in EGME and is configured to the solution that butyl titanate concentration is 0.02-0.2mol/L, then the ammoniacal liquor instilling mass concentration 30% all precipitates to titanium ion, filter the oxyhydroxide precipitation obtaining titanium;
Concentration is 0.5-1.5g/L graphene oxide water solution and monoethanolamine 1:1 mixing by volume by 2, again by step 1) the oxyhydroxide precipitation of the titanium that obtains and above-mentioned mixed solution be join in reactor inner bag together with 1:2 by volume, stirred at ambient temperature at least 6h;
3) by with step 1) in the strontium nitrate of butyl titanate equimolar amounts join step 2) reactor inner bag in, add potassium hydroxide solid again, controlling its concentration in mixed solution is 1.25-5g/L, and gained mixed solution is at room temperature stirred at least 1h;
4) the reactor inner bag being configured with reaction mass is placed in reactor, airtight, 160-200 DEG C of insulation after 3-12 hour, Temperature fall, to room temperature, takes out product, filters, by washed with de-ionized water, dry, obtain strontium titanates/Graphene composite nano-catalyst.
In the present invention, described strontium nitrate, butyl titanate, EGME, potassium hydroxide, monoethanolamine and graphene oxide purity are all not less than chemical pure.
In the present invention, described reactor is polytetrafluoroethylliner liner, the reactor that stainless steel external member is airtight.
Preparation method's technical process of the present invention is simple, is easy to control, and pollution-free, cost is low; Obtained strontium titanates/graphene composite nano material, purity is high, good crystallinity.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscopic picture of strontium titanates/Graphene composite nano-catalyst.
Fig. 2 is the ultraviolet-ray visible absorbing figure of strontium titanates/Graphene composite nano-catalyst visible light photocatalytic degradation methylene blue different time.
Fig. 3 is the XRD collection of illustrative plates of strontium titanates/Graphene composite nano-catalyst.
Fig. 4 is the transmission electron microscope picture of strontium titanates/Graphene composite nano-catalyst.
Detailed description of the invention
Below in conjunction with embodiment, the inventive method is described in further detail.
Embodiment 1
1) butyl titanate is dissolved in EGME and is configured to the solution that butyl titanate concentration is 0.02mol/L, then the ammoniacal liquor instilling mass concentration 30% all precipitates to titanium ion;
2) concentration is graphene oxide water solution and the mixing of monoethanolamine equal-volume of 0.5g/L, by step 1) the oxyhydroxide precipitation of the titanium that obtains joins in reactor inner bag together with above-mentioned mixed liquor, wherein the oxyhydroxide of titanium and the volume ratio of mixed solution are 1:2, stirred at ambient temperature 6h;
3) by with step 1) in the strontium nitrate of butyl titanate equimolar amounts join step 2) reactor inner bag in, then add potassium hydroxide solid, controlling its concentration in mixed solution is 1.25g/L, stirred at ambient temperature 1h;
4) the reactor inner bag being configured with reaction mass is placed in reactor, airtight, 160 DEG C of insulations after 3 hours, Temperature fall, to room temperature, takes out product, filters, and by washed with de-ionized water, dries, obtains composite nano powder.
Its scanning electron microscopic picture as shown in Figure 1.
Embodiment 2
1) butyl titanate is dissolved in EGME and is configured to the solution that butyl titanate concentration is 0.05mol/L, then the ammoniacal liquor instilling mass concentration 30% all precipitates to titanium ion;
2) by concentration be 1g/L graphene oxide water solution and the mixing of monoethanolamine equal-volume, by step 1) the oxyhydroxide precipitation of the titanium that obtains joins in reactor inner bag together with above-mentioned mixed liquor, wherein the oxyhydroxide of titanium and the volume ratio of mixed solution are 1:2, stirred at ambient temperature 8h;
3) by with step 1) in the strontium nitrate of butyl titanate equimolar amounts join step 2) reactor inner bag in, then add potassium hydroxide solid, controlling its concentration in mixed solution is 2.5g/L, stirred at ambient temperature 1.5h;
4) the reactor inner bag being configured with reaction mass is placed in reactor, airtight, 180 DEG C of insulations after 12 hours, Temperature fall, to room temperature, takes out product, filters, and by washed with de-ionized water, dries, obtains strontium titanates/Graphene composite nano powder.
The UV-Visible absorption figure of its degradation of methylene blue different time under visible ray (λ >400nm) illumination as shown in Figure 2.As seen from the figure, the major absorbance peak of methylene blue, at 664nm place, after illumination 40min, about has the methylene blue dye of 54% to be degraded, and indicates strontium titanates/Graphene composite nano-catalyst and has very high visible light catalytic performance.
Embodiment 3
1) butyl titanate is dissolved in EGME and is configured to the solution that butyl titanate concentration is 0.1mol/L, then the ammoniacal liquor instilling mass concentration 30% all precipitates to titanium ion;
2) by concentration be 1.5g/L graphene oxide water solution and the mixing of monoethanolamine equal-volume, by step 1) the oxyhydroxide precipitation of the titanium that obtains joins in reactor inner bag together with above-mentioned mixed liquor, wherein the oxyhydroxide of titanium and the volume ratio of mixed solution are 1:2, stirred at ambient temperature 6h;
3) by with step 1) in the strontium nitrate of butyl titanate equimolar amounts join step 2) reactor inner bag in, then add potassium hydroxide solid, controlling its concentration in mixed solution is 5g/L, stirred at ambient temperature 1h;
4) the reactor inner bag being configured with reaction mass is placed in reactor, airtight, 200 DEG C of insulations after 6 hours, Temperature fall, to room temperature, takes out product, filters, and by washed with de-ionized water, dries, obtains strontium titanates/Graphene composite nano powder.
Its corresponding transmission electron microscope picture and XRD spectral line are as Fig. 3, and shown in 4, gained sample crystallization degree is good, and purity is high, and Graphene suprabasil strontium titanate nanoparticles domain size distribution is little, good dispersion.
Claims (3)
1. a preparation method for strontium titanates/Graphene composite nano-catalyst, is characterized in that, comprises following processing step:
1) butyl titanate is dissolved in EGME and is configured to the solution that butyl titanate concentration is 0.02-0.2mol/L, then the ammoniacal liquor instilling mass concentration 30% all precipitates to titanium ion, filter the oxyhydroxide precipitation obtaining titanium;
Concentration is 0.5-1.5g/L graphene oxide water solution and monoethanolamine 1:1 mixing by volume by 2, then by step 1) the oxyhydroxide precipitation of titanium that obtains and above-mentioned mixed solution by volume 1:2 join in reactor inner bag, stirred at ambient temperature is 6h at least;
3) by with step 1) in the strontium nitrate of butyl titanate equimolar amounts join step 2) reactor inner bag in, add potassium hydroxide solid again, make its concentration in mixed solution be 1.25-5g/L, gained mixed solution is at room temperature stirred at least 1h;
4) the reactor inner bag being configured with reaction mass is placed in reactor, airtight, 160-200 DEG C of insulation after 3-12 hour, Temperature fall, to room temperature, takes out product, filters, by washed with de-ionized water, dry, obtain strontium titanates/Graphene composite nano-catalyst.
2. the preparation method of the strontium titanates according to claims 1/Graphene composite nano-catalyst, is characterized in that the purity of described strontium nitrate, butyl titanate, EGME, potassium hydroxide, monoethanolamine and graphene oxide is all not less than chemical pure.
3. the preparation method of the strontium titanates according to claims 1/Graphene composite nano-catalyst, is characterized in that described reactor is polytetrafluoroethylliner liner, the reactor that stainless steel external member is airtight.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105817217A (en) * | 2016-04-26 | 2016-08-03 | 武汉三江航天远方科技有限公司 | SrTiO3/graphene composite catalyst as well as preparation method and application thereof |
| CN106925248A (en) * | 2017-03-15 | 2017-07-07 | 天津大学 | The oxygen-containing vacancy strontium titanates catalysis material of hydroxyl modified and its preparation and application |
| CN107285698A (en) * | 2017-07-05 | 2017-10-24 | 汤始建华建材（苏州）有限公司 | Flame-retarding wave-absorbing functional concrete and preparation method thereof |
| CN109967098A (en) * | 2017-12-28 | 2019-07-05 | Tcl集团股份有限公司 | A kind of photochemical catalyst and the preparation method and application thereof |
| CN114345318A (en) * | 2021-12-03 | 2022-04-15 | 中北大学 | graphene-SrTiO3Material and method for the production thereof |
| CN116422323A (en) * | 2023-04-12 | 2023-07-14 | 江苏大学 | Preparation method of visible light driven graphene oxide/rhodium-strontium titanate composite full-hydrolysis photocatalyst |
Citations (3)
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| CN102847529A (en) * | 2012-02-09 | 2013-01-02 | 江苏大学 | Graphene/titanate nanometer composite visible-light activated photocatalyst and preparation method thereof |
| CN104402044A (en) * | 2014-11-14 | 2015-03-11 | 浙江大学 | Preparation method for barium titanate/graphene composite nanometer material |
| CN104477975A (en) * | 2014-12-04 | 2015-04-01 | 浙江大学 | Method for preparing hollow cubic strontium titanate |
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2015
- 2015-08-25 CN CN201510526251.8A patent/CN105126803A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102847529A (en) * | 2012-02-09 | 2013-01-02 | 江苏大学 | Graphene/titanate nanometer composite visible-light activated photocatalyst and preparation method thereof |
| CN104402044A (en) * | 2014-11-14 | 2015-03-11 | 浙江大学 | Preparation method for barium titanate/graphene composite nanometer material |
| CN104477975A (en) * | 2014-12-04 | 2015-04-01 | 浙江大学 | Method for preparing hollow cubic strontium titanate |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105817217A (en) * | 2016-04-26 | 2016-08-03 | 武汉三江航天远方科技有限公司 | SrTiO3/graphene composite catalyst as well as preparation method and application thereof |
| CN106925248A (en) * | 2017-03-15 | 2017-07-07 | 天津大学 | The oxygen-containing vacancy strontium titanates catalysis material of hydroxyl modified and its preparation and application |
| CN106925248B (en) * | 2017-03-15 | 2019-06-25 | 天津大学 | The oxygen-containing vacancy strontium titanates catalysis material of hydroxyl modified and its preparation and application |
| CN107285698A (en) * | 2017-07-05 | 2017-10-24 | 汤始建华建材（苏州）有限公司 | Flame-retarding wave-absorbing functional concrete and preparation method thereof |
| CN109967098A (en) * | 2017-12-28 | 2019-07-05 | Tcl集团股份有限公司 | A kind of photochemical catalyst and the preparation method and application thereof |
| CN114345318A (en) * | 2021-12-03 | 2022-04-15 | 中北大学 | graphene-SrTiO3Material and method for the production thereof |
| CN116422323A (en) * | 2023-04-12 | 2023-07-14 | 江苏大学 | Preparation method of visible light driven graphene oxide/rhodium-strontium titanate composite full-hydrolysis photocatalyst |
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