CN105664913A - Preparation method of lead titanate nanoparticle/graphene composite catalyst - Google Patents
Preparation method of lead titanate nanoparticle/graphene composite catalyst Download PDFInfo
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- CN105664913A CN105664913A CN201610014541.9A CN201610014541A CN105664913A CN 105664913 A CN105664913 A CN 105664913A CN 201610014541 A CN201610014541 A CN 201610014541A CN 105664913 A CN105664913 A CN 105664913A
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- lead titanate
- graphene
- graphene composite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 34
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 239000003054 catalyst Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 24
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000008187 granular material Substances 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000005285 chemical preparation method Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 229910052719 titanium Inorganic materials 0.000 abstract 1
- 239000010936 titanium Substances 0.000 abstract 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 201000010260 leiomyoma Diseases 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention relates to a preparation method of a lead titanate nanoparticle/graphene composite catalyst. By adopting a wet chemical reaction technique, the method includes the steps of: taking titanium dioxide as a titanium source, adopting lead nitrate as a lead source, using potassium hydroxide as a mineralizer, employing a graphene oxide aqueous solution as the graphene preparation raw material, carrying out hydrothermal reaction to obtain lead titanate nanoparticle/grapheme powder. The method provided by the invention has the characteristics of simple process, easy control, no pollution and low cost, and the prepared lead titanate nanoparticle/graphene composite catalyst has high purity and good crystallinity.
Description
Technical field
The present invention relates to the preparation method of lead titanate nano particle/graphene composite catalyst, belong to field of inorganic nonmetallic material.
Background technology
Lead titanate is the ferroelectric oxide of a kind of typical perovskite structure, and structure is simple, and piezoelectricity and ferroelectricity are strong. Since the fifties finds, lead titanate is the leiomyoma cells of ferroelectric and piezoelectricity field research always, recognizes perovskite oxide piezoelectricity for people and ferroelectric electronics origin has very important meaning. About preparation and the research of lead titanate zero dimensional nanometer materials, and the application of its catalyzer aspect is still in the exploratory stage. Graphene is that one passes through sp by carbon atom2The two-dimentional carbon material of the monoatomic layer thickness of hydridization composition; It has and has superpower electron transport property simultaneously, is the ideal carrier of a kind of complex functionality semiconductors coupling catalystic material. At present, for the research of lead titanate nano particle and the composite catalyst of Graphene, it is showed no relevant report both at home and abroad.
Summary of the invention
It is an object of the invention to provide a kind of technique simple, process is easy to the preparation method of the lead titanate nano particle/graphene composite catalyst of control.
The preparation method of the lead titanate nano particle/graphene composite catalyst of the present invention, employing be wet-chemical reaction method, comprise the following steps:
1) by 0.25-0.5mmol nano TiO 2 powder, 1-20ml concentration is that 1.5g/L graphene oxide water solution adds in reactor in courage, adds 1g-3g potassium hydroxide subsequently, adds deionized water to reactor loading level 80%, and stirred at ambient temperature is 6h at least;
2) by 0.25-0.5mmol lead nitrate, what join step 1) is equipped with in the reactor of mixing solutions in courage, and stirred at ambient temperature is 1h at least;
3) it is placed in reactor by being configured with in the reactor of reaction mass courage, airtight, at 180-200oC insulation is after 8-20 hour, and Temperature fall, to room temperature, takes out reaction product, filters, uses sub-water, washes of absolute alcohol, dries, obtains lead titanate nano particle/Graphene composite granule.
In the present invention, described lead nitrate, potassium hydroxide, titanium dioxide 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.
Technological process of the present invention is simple, is easy to control, and pollution-free, cost is low; Obtained lead titanate nano particle/graphene composite catalyst, purity height, good crystallinity.
Accompanying drawing explanation
Fig. 1 is the TEM figure of lead titanate nano particle/graphene composite catalyst.
Fig. 2 is the ultraviolet-visible absorption figure of lead titanate nano particle/graphene composite catalyst visible light photocatalytic degradation methylene blue different time.
Fig. 3 is the XRD figure spectrum of lead titanate nano particle/graphene composite catalyst.
Fig. 4 is the SEM picture of lead titanate nano particle/graphene composite catalyst.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
1) by 0.5mmol nano TiO 2 powder, 10ml concentration is that 1.5g/L graphene oxide water solution adds in reactor in courage, adds 2.74g potassium hydroxide subsequently, adds deionized water to reactor loading level 80%, stirred at ambient temperature 6h;
2) by 0.5mmol lead nitrate, what join step 1) is equipped with in the reactor of mixing solutions in courage, stirred at ambient temperature 1h;
3) it is placed in reactor by being configured with in the reactor of reaction mass courage, airtight, 190oAfter C is incubated 12 hours, Temperature fall, to room temperature, takes out reaction product, filters, spends sub-water, washes of absolute alcohol, dries, obtains lead titanate nano particle/Graphene composite granule.
Its TEM schemes as shown in Figure 1, and the lead titanate nano particle diameter distribution at the graphene-based end is little.
Embodiment 2
1) by 0.45mmol nano TiO 2 powder, 20ml concentration is that 1.5g/L graphene oxide water solution adds in reactor in courage, adds 3g potassium hydroxide subsequently, adds deionized water to reactor loading level 80%, stirred at ambient temperature 8h;
2) by 0.45mmol lead nitrate, what join step 1) is equipped with in the reactor of mixing solutions in courage, stirred at ambient temperature 3h;
3) it is placed in reactor by being configured with in the reactor of reaction mass courage, airtight, 180oAfter C is incubated 20 hours, Temperature fall, to room temperature, takes out reaction product, filters, spends sub-water, washes of absolute alcohol, dries, obtains lead titanate nano particle/Graphene composite granule.
The UV-Visible absorption figure of its degradation of methylene blue different time under visible ray (λ >=420nm) illumination is as shown in Figure 2. As seen from the figure, the major absorbance peak of methylene blue, at 664nm place, after visible light source illumination 40min, about has the methylene blue dye of 46% to be degraded. This demonstrate lead titanate nano particle/graphene composite catalyst and there is very high visible light catalytic performance.
Embodiment 3
1) by 0.25mmol nano TiO 2 powder, 1ml concentration is that 1.5g/L graphene oxide water solution adds in reactor in courage, adds 1g potassium hydroxide subsequently, adds deionized water to reactor loading level 80%, stirred at ambient temperature 10h;
2) by 0.25mmol lead nitrate, what join step 1) is equipped with in the reactor of mixing solutions in courage, stirred at ambient temperature 2h;
3) it is placed in reactor by being configured with in the reactor of reaction mass courage, airtight, 200oAfter C is incubated 8 hours, Temperature fall, to room temperature, takes out reaction product, filters, spends sub-water, washes of absolute alcohol, dries, obtains lead titanate nano particle/Graphene composite granule.
Its corresponding SEM figure and XRD composes line such as Fig. 3, and shown in 4, gained sample crystallization degree is good, purity height, and the lead titanate nano particle diameter distribution at the graphene-based end is little.
Claims (3)
1. the preparation method of lead titanate nano particle/graphene composite catalyst, it is characterised in that comprise the following steps:
1) by 0.25-0.5mmol nano TiO 2 powder, 1-20ml concentration is that 1.5g/L graphene oxide water solution adds in reactor in courage, adds 1g-3g potassium hydroxide subsequently, adds deionized water to reactor loading level 80%, and stirred at ambient temperature is 6h at least;
2) by 0.25-0.5mmol lead nitrate, what join step 1) is equipped with in the reactor of mixing solutions in courage, and stirred at ambient temperature is 1h at least;
3) it is placed in reactor by being configured with in the reactor of reaction mass courage, airtight, at 180-200oC insulation is after 8-20 hour, and Temperature fall, to room temperature, takes out reaction product, filters, uses sub-water, washes of absolute alcohol, dries, obtains lead titanate nano particle/Graphene composite granule.
2. the preparation method of lead titanate nano particle/Graphene composite granule according to claim 1, it is characterised in that described lead nitrate, potassium hydroxide, titanium dioxide and graphene oxide purity are all not less than chemical pure.
3. the preparation method of lead titanate nano particle/Graphene according to claim 1, it is characterised in that described reactor is polytetrafluoroethylliner liner, the reactor that stainless steel external member is airtight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610014541.9A CN105664913A (en) | 2016-01-11 | 2016-01-11 | Preparation method of lead titanate nanoparticle/graphene composite catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610014541.9A CN105664913A (en) | 2016-01-11 | 2016-01-11 | Preparation method of lead titanate nanoparticle/graphene composite catalyst |
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| Publication Number | Publication Date |
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| CN105664913A true CN105664913A (en) | 2016-06-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610014541.9A Pending CN105664913A (en) | 2016-01-11 | 2016-01-11 | Preparation method of lead titanate nanoparticle/graphene composite catalyst |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006205006A (en) * | 2005-01-26 | 2006-08-10 | Ichimura Fukuyo | Catalyst material for waste gas purification, and waste gas purification apparatus having this material fixed to it |
| CN102847529A (en) * | 2012-02-09 | 2013-01-02 | 江苏大学 | Graphene/titanate nanometer composite visible-light activated photocatalyst and preparation method thereof |
-
2016
- 2016-01-11 CN CN201610014541.9A patent/CN105664913A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006205006A (en) * | 2005-01-26 | 2006-08-10 | Ichimura Fukuyo | Catalyst material for waste gas purification, and waste gas purification apparatus having this material fixed to it |
| CN102847529A (en) * | 2012-02-09 | 2013-01-02 | 江苏大学 | Graphene/titanate nanometer composite visible-light activated photocatalyst and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李永宇等: "温度和pH值对水热制备的 PbTiO3的催化性能的影响", 《中国化学会第29届学术年会会议论文集》 * |
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Application publication date: 20160615 |
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