CN101670269B - Synthesis method of load type composite material of graphite oxide/hydroxyl bismuth subnitrate - Google Patents
Synthesis method of load type composite material of graphite oxide/hydroxyl bismuth subnitrate Download PDFInfo
- Publication number
- CN101670269B CN101670269B CN200910182647XA CN200910182647A CN101670269B CN 101670269 B CN101670269 B CN 101670269B CN 200910182647X A CN200910182647X A CN 200910182647XA CN 200910182647 A CN200910182647 A CN 200910182647A CN 101670269 B CN101670269 B CN 101670269B
- Authority
- CN
- China
- Prior art keywords
- graphite oxide
- bismuth subnitrate
- solvent
- bismuth
- load type
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a synthesis method of composite material of graphite oxide/load type hydroxyl bismuth subnitrate, the composite material of graphite oxide/load type hydroxyl bismuth subnitrate is prepared by the following steps: scattering graphite oxide and bismuth salt in a solvent respectively, stirring evenly by ultrasound, and mixing to form a mixture solution; putting the mixture solution obtained in the last step in an oven to evaporate to remove the solvent and water, drying and grinding to obtain the composite material of graphite oxide/load type hydroxyl bismuth subnitrate. The invention utilizes the abundant surface properties of the graphite oxide and the high specific surface of the graphite oxide to in-situ deposit load type hydroxyl bismuth subnitrate grains on the surface of the graphite oxide by chemical action, the formed composite graphite oxide reduces aggregation of the load type hydroxyl bismuth subnitrate, enlarges the surface area thereof, obviously improves absorption property and catalyzation property, and has better application prospect and economic benefit in aspects of catalytical reaction, solar cell, sewage treatment, etc.
Description
Technical field
The present invention relates to the synthetic technology of loaded with nano particle on graphite oxide, be specifically related to the synthetic method of a kind of support type graphite oxide/hydroxyl bismuth subnitrate composite.
Background technology
Graphite oxide is a kind of carbon materials, is that another the new discovery to the material with carbon element field has important scientific meaning after diamond-type, graphite mould, fullerene type and carbon cast material with carbon element.Owing to be rich in functional groups such as epoxy radicals, hydroxyl on the graphite oxide carbon-coating, give graphite oxide and had very superior performance, electronegative as the graphite oxide carbon-coating, can adsorb the cation that has positive electricity; Simultaneously, the hydrophily of oxygen-containing functional group on the graphite oxide carbon-coating helps improving the dispersive property of graphite oxide in water; The abundant chemical bond in graphite oxide surface can form chemical bond between graphite oxide and loaded particle in addition, forms the composite of the graphite oxide of stable performance, the composite of obtained performance excellence.Therefore, based on the research of graphite oxide more and more widely.
Graphite oxide has bigger specific area, can be used as the carrier of catalyst, adsorbent, and at present, this type of work is risen, existing relevant research work report, as Wang Xinjiao give lessons topic form merit at the graphite oxide area load Ag, Cu
2O, Co
3O
4Deng material, but do not see about the load of bismuthino material and report.In addition, Wang Z M etc. is with graphite oxide and catalysis material TiO
2Compound, utilize oxidized graphite flake when calcining, to realize parcel, form cavernous structure and improve its performance, but its effect is not satisfactory.
Summary of the invention
The objective of the invention is to: the synthetic method that a kind of support type graphite oxide/hydroxyl bismuth subnitrate composite is provided, this synthetic method is carried on the graphite oxide surface with hydroxyl bismuth subnitrate, obtain a kind of support type graphite oxide/hydroxyl bismuth subnitrate composite, improve absorption property, the catalytic performance of composite.
Technical solution of the present invention is that this synthetic method may further comprise the steps:
The first step: graphite oxide is dispersed in the solvent, and ultrasonic being uniformly dispersed gets the graphite oxide suspension;
Second step: bismuth salt is dissolved in the solvent with the first step, ultrasonic being uniformly dispersed, the bismuth salting liquid;
The 3rd step: with the graphite oxide suspension of first step gained bismuth salt solution mix, stir with the second step gained, must mixed liquor;
The 4th step: the mixed liquor of the 3rd step gained is placed Muffle furnace or baking oven evaporative removal solvent and corresponding moisture, puts into baking oven after the taking-up and dry, grind the graphite oxide of load hydroxyl bismuth subnitrate.
In the synthetic method of support type graphite oxide of the present invention/hydroxyl bismuth subnitrate composite, the weight ratio of bismuth salt and graphite oxide is (20～1): 1, solvent is (300～100) with the graphite oxide ratio: 1, solvent is (15～5) with bismuth salt ratio: 1, wherein bismuth salt and graphite oxide are in gram, and solvent is in milliliter.
In the synthetic method of support type graphite oxide of the present invention/hydroxyl bismuth subnitrate composite, solvent is n-butanol or n-hexyl alcohol.
In the synthetic method of support type graphite oxide of the present invention/hydroxyl bismuth subnitrate composite, bismuth salt is five water bismuth nitrates.
In the synthetic method of support type graphite oxide of the present invention/hydroxyl bismuth subnitrate composite, ultrasound condition is the ultrasonic 30min of 25kHz room temperature.
In the synthetic method of support type graphite oxide of the present invention/hydroxyl bismuth subnitrate composite, evaporation conditions is 130～150 ℃ of temperature, time 5～15h, and bake out temperature is 50～70 ℃.
The present invention compared with prior art, its advantage is as follows: 1) utilize the active group on the oxidized graphite flake, act on its surface deposition hydroxyl bismuth subnitrate by chemical bonding, obtained the oxidized graphite composite material of stable performance; 2) because the graphite oxide thin slice has higher specific surface area, effectively suppressed the reunion between the particle, the oxidized graphite composite material dispersive property of acquisition is good, specific surface is big; 3) oxidized graphite composite material of the present invention is functional, has application promise in clinical practice in sewage disposal and energy source use field; 4) this synthetic method is easy to operate, cost is low, for the preparation oxidized graphite composite material provides a new way.
Description of drawings
Fig. 1 is the X-ray diffraction spectrogram of graphite oxide and the compound front and back of hydroxyl bismuth subnitrate, (a) graphite oxide wherein, (b) hydroxyl bismuth subnitrate, (c) the combined oxidation graphite of load hydroxyl bismuth subnitrate
Fig. 2 is the infrared spectrum of graphite oxide and the compound front and back of hydroxyl bismuth subnitrate, (a) hydroxyl bismuth subnitrate wherein, (b) the combined oxidation graphite of load hydroxyl bismuth subnitrate, (c) graphite oxide
The electromicroscopic photograph of the combined oxidation graphite of Fig. 3 load hydroxyl bismuth subnitrate, wherein (a) is transmission electron microscope photo, (b) is stereoscan photograph
The specific embodiment
According to technical scheme of the present invention, introduce the synthetic method of support type graphite oxide/hydroxyl bismuth subnitrate composite in conjunction with the embodiments, these embodiment should not be construed as the restriction to technical scheme.
Example 1: the synthesis step of support type graphite oxide/hydroxyl bismuth subnitrate composite is as follows:
The first step in the beaker of dried and clean, is got the 50mg graphite oxide, is distributed to the 10mL n-butanol, the ultrasonic 30min of 25kHz room temperature;
In second step, in the beaker of another dried and clean, get 0.7gBi (NO
3)
35H
2O is dissolved in the 7mL n-butanol then, the ultrasonic 30min of 25kHz room temperature;
The 3rd step, with the solution mixing of second step and the 3rd step gained, on magnetic stirring apparatus, stir 30min, it is mixed;
The 4th step placed 140 ℃ Muffle furnace to evaporate 10h above-mentioned mixed solution, took out the baking oven of putting into 60 ℃ and dried, and ground.
Fig. 1 is the XRD spectra of graphite oxide (GO) and the compound front and back of hydroxyl bismuth subnitrate, as can be seen, and with Bi
6O
5(OH)
3(NO
3)
52H
2(001) crystal face diffraction maximum (2 θ=9.8 °) of graphite oxide disappeared (Fig. 1 c) after O was compound, and that present is Bi substantially
6O
5(OH)
3(NO
3)
52H
2The diffraction maximum of O is with the Bi of pure phase
6O
5(OH)
3(NO
3)
52H
2O diffraction peak-to-peak similar (Fig. 1 b) illustrates the compound Bi afterwards with GO
6O
5(OH)
3(NO
3)
52H
2The crystal phase structure of O does not have significant change, and the layer structure of graphite oxide is at Bi
6O
5(OH)
3(NO
3)
52H
2Destroyed in the deposition process of O, formed the GO monolithic layer; Because GO is difficult to be stripped from the n-butanol solvent, the possible cause that occurs this phenomenon so is exactly that oxygen-containing functional group on the GO carbon-coating makes graphite oxide be elecrtonegativity, the Bi of positively charged
6O
5(OH)
3 5+Be deposited on the GO lamella by Electrostatic Absorption, and then the decomposition reaction that has produced original position causes Bi
6O
5(OH)
3(NO
3)
52H
2The O crystal destroys, peels off until the GO interlayer structure in the growth of GO interlayer, deposition.
Fig. 2 is Bi
6O
5(OH)
3(NO
3)
52H
2The FT-IR spectrogram of the compound front and back of O and graphite oxide (GO) by Fig. 2 a as can be seen, is positioned at 3300cm
-1Near have absworption peak, from the deformation vibration of surperficial adsorbed water; Be positioned at 1369cm
-1About locate also to exist NO
3 -Strong absworption peak; 575cm
-1And 815cm
-1About absworption peak, corresponding to the vibration of Bi-O and Bi-O-Bi; 1600cm
-1Near have absworption peak, owing to Bi
2O
3The flexural vibrations of surface O-H; By Fig. 2 c as can be seen, be positioned at 3200～3800cm
-1The spectrum peak of the broad that occurs in the scope comes from the adsorbed hydrone of stretching vibration and surface thereof of graphite oxide surface-OH; Be positioned at 1600cm
-1Near absworption peak is corresponding to the flexural vibrations of O-H; Be positioned at 1030cm
-1Near absworption peak is the absorption of vibrations of C-O-C, and these presentation of results graphite oxide surfaces have the chemical bond than horn of plenty; Fig. 2 b is GO-Bi
6O
5(OH)
3(NO
3)
52H
2As can be seen, not only there is the absworption peak of GO in the infrared spectrum of O, and has Bi in the composite
6O
5(OH)
3(NO
3)
52H
2The absworption peak of O illustrates that composite has GO and Bi simultaneously
6O
5(OH)
3(NO
3)
52H
2The character of O; By relatively finding with the infrared spectrum of pure phase material, the position of the infrared absorption peak of combination product is blue shift to some extent all, and the maximum wave number of blue shift is about 12cm
-1, compound GO and Bi afterwards are described
6O
5(OH)
3(NO
3)
52H
2Certain interaction has taken place between the O, and therefore, this composite has stronger stability.
Fig. 3 is the electromicroscopic photograph of the combined oxidation graphite of load hydroxyl bismuth subnitrate, oxidized plumbago single slice layer structural integrity as can be seen, and its area load the hydroxyl bismuth subnitrate of whisker shape, and better dispersed, coincide with structure common in the document; Explanation thus, synthetic method of the present invention can obtain the combined oxidation graphite of load hydroxyl bismuth subnitrate, and simple, the easy row of technology, realizes suitability for industrialized production easily.
Example 2: the synthetic method of support type graphite oxide/hydroxyl bismuth subnitrate composite:
The first step in the beaker of dried and clean, is got the 100mg graphite oxide, is distributed to the 30mL n-butanol, the ultrasonic 30min of 25kHz room temperature;
In second step, in the beaker of another dried and clean, get 0.1gBi (NO
3)
35H
2O is dissolved in the 1.5mL butanol solution, the ultrasonic 30min of 25kHz room temperature;
The 3rd step, with the solution mixing of second step and the 3rd step gained, on magnetic stirring apparatus, stir 30min, solution is mixed;
The 4th step placed 130 ℃ Muffle furnace to evaporate 5h above-mentioned mixed solution, took out the baking oven of putting into 50 ℃ and dried, and ground.
Example 3: the synthetic method of support type graphite oxide/hydroxyl bismuth subnitrate composite:
The first step is got the 200mg graphite oxide in the beaker of dried and clean, be distributed to the 20mL n-hexyl alcohol, the ultrasonic 30min of 25kHz room temperature;
In second step, in the beaker of another dried and clean, get 4g Bi (NO
3)
35H
2O is scattered in the 20mL n-hexyl alcohol solution, the ultrasonic 30min of 25kHz room temperature;
The 3rd step, with the solution mixing of second step and the 3rd step gained, on magnetic stirring apparatus, stir 30min, solution is mixed;
The 4th step placed 150 ℃ Muffle furnace to evaporate 15h above-mentioned mixed solution, took out the baking oven of putting into 70 ℃ and dried, and ground.
Claims (3)
1. the synthetic method of support type graphite oxide/hydroxyl bismuth subnitrate composite is characterized in that this synthetic method may further comprise the steps: the first step: graphite oxide is dispersed in the solvent, ultrasonic being uniformly dispersed, the graphite oxide suspension; Second step: bismuth salt is dissolved in the solvent with the first step, ultrasonic being uniformly dispersed, the bismuth salting liquid; The 3rd step: the solution of the first step, the second step gained is mixed, stir, get mixed liquor; The 4th step: the mixed liquor of the 3rd step gained is placed baking oven evaporative removal solvent and corresponding moisture, takes out and to put into baking oven and dries, grind the combined oxidation graphite of load hydroxyl bismuth subnitrate; Wherein, solvent is n-butanol or n-hexyl alcohol; Wherein, bismuth salt is five water bismuth nitrates; Wherein, evaporation conditions is 130～150 ℃ of temperature, time 5～15h, 50～70 ℃ of baking temperatures.
2. the synthetic method of support type graphite oxide according to claim 1/hydroxyl bismuth subnitrate composite, it is characterized in that: the amount ratio of bismuth salt and graphite oxide is (20～1): 1, solvent is (300～100) with the ratio of graphite oxide: 1, solvent is (15～5) with bismuth salt ratio: 1, wherein the consumption of bismuth salt and graphite oxide is in gram, and solvent load is in milliliter.
3. the synthetic method of support type graphite oxide according to claim 1/hydroxyl bismuth subnitrate composite is characterized in that: ultrasound condition is the ultrasonic 30min of 25kHz room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910182647XA CN101670269B (en) | 2009-09-18 | 2009-09-18 | Synthesis method of load type composite material of graphite oxide/hydroxyl bismuth subnitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910182647XA CN101670269B (en) | 2009-09-18 | 2009-09-18 | Synthesis method of load type composite material of graphite oxide/hydroxyl bismuth subnitrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101670269A CN101670269A (en) | 2010-03-17 |
| CN101670269B true CN101670269B (en) | 2011-05-11 |
Family
ID=42017812
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910182647XA Expired - Fee Related CN101670269B (en) | 2009-09-18 | 2009-09-18 | Synthesis method of load type composite material of graphite oxide/hydroxyl bismuth subnitrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101670269B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2011258067B2 (en) * | 2010-05-28 | 2013-10-24 | Graphea, Inc. | Carbocatalysts for chemical transformations |
| CN106391087B (en) * | 2016-10-19 | 2018-10-16 | 常州大学 | A kind of preparation method of novismuth compound phosphoric acid yttrium catalyst |
-
2009
- 2009-09-18 CN CN200910182647XA patent/CN101670269B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101670269A (en) | 2010-03-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106799251B (en) | A kind of composite photo-catalyst and preparation method thereof | |
| CN1803594A (en) | Large-area ultra-thin carbon nanotube film and its preparation process | |
| CN106179446B (en) | The method of cobalt/nitrating porous carbon composite and its preparation method and catalysis silane oxidation | |
| Li et al. | Controlled deposition of Au on (BiO) 2 CO 3 microspheres: the size and content of Au nanoparticles matter | |
| CN107262133A (en) | A kind of preparation method of the photochemical catalyst based on single dispersing bismuth with elementary and carbonitride | |
| CN114177891B (en) | Preparation method of biochar composite metal organic framework adsorbing material | |
| CN101811689A (en) | Three-dimensional network carbon nanofiber and preparation method and application thereof | |
| CN102658106A (en) | Method for preparing acidification stripped vermiculite supported TiO2 photocatalyst | |
| CN113149115B (en) | Multistage heterostructure membrane for photo-thermal seawater desalination and preparation method | |
| CN106268908A (en) | A kind of graphite-phase C removing removal organic polluter3n4doping TiO2float type ecological restoration material of load expanded perlite and preparation method thereof | |
| Fathy et al. | Synthesis of transparent amorphous carbon thin films from cellulose powder in rice straw | |
| CN106395802B (en) | Preparation method of graphene porous membrane | |
| CN102205238A (en) | Method for preparing MWCNTs/ZnO (multi-wall carbon nano tubes/zinc oxide) nanometer composite material | |
| CN101670269B (en) | Synthesis method of load type composite material of graphite oxide/hydroxyl bismuth subnitrate | |
| CN101279208B (en) | Method for preparing Y type molecular sieve film | |
| CN112934167A (en) | Titanium dioxide/layered double hydroxide non-carbon-based composite material and preparation method and application thereof | |
| CN106238080A (en) | The method that p-doped porous graphene and preparation method thereof aoxidizes with catalysis benzylamine | |
| CN106683909A (en) | In-situ preparation method for cubic copper oxide/graphene aerogel composite material | |
| CN114558595B (en) | Visible light catalyst for degrading antibiotic residues | |
| CN106532047A (en) | Silylene/graphene composite material, and preparation method and applications thereof | |
| CN114700065B (en) | Waste resin carbon sphere composite ozone catalyst and preparation method and application thereof | |
| CN108031481B (en) | Ultrathin bismuth oxyhalide nanosheet photocatalyst stripped by silver intercalation and preparation method thereof | |
| CN112892572B (en) | Au-PCN-CNT composite material and preparation method and application thereof | |
| CN115148506A (en) | Super capacitor electrode material and preparation method thereof | |
| CN114904558A (en) | Preparation method of hollow nitrogen-doped carbon-coated titanium dioxide photocatalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110511 Termination date: 20140918 |
|
| EXPY | Termination of patent right or utility model |