CN103691473A - Bentonite/graphite phase carbon nitride composite material and preparation method thereof - Google Patents
Bentonite/graphite phase carbon nitride composite material and preparation method thereof Download PDFInfo
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- CN103691473A CN103691473A CN201410000800.3A CN201410000800A CN103691473A CN 103691473 A CN103691473 A CN 103691473A CN 201410000800 A CN201410000800 A CN 201410000800A CN 103691473 A CN103691473 A CN 103691473A
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- phase carbonitride
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Abstract
The invention discloses a bentonite/graphite phase carbon nitride composite material and a preparation method thereof. The bentonite/graphite phase carbon nitride composite material is prepared by the following steps: mixing dicyandiamide aqueous liquor with bentonite; drying; crushing; calcining; and crushing. The composite material in a lamellar structure prepared by the method disclosed by the invention has the capability of catalytic degradation on organic pollutants by visible lights and good photocurrent response performance. The method disclosed by the invention is simple and feasible, low in product cost and easy for industrialized production, has very high application prospect and practical value, and can be applied to the field of photocatalytic degradation of environmental pollutants.
Description
Technical field
The invention belongs to Nano-composite materials and application, be specifically related to a kind of bentonite/graphite-phase carbonitride composite and preparation method thereof.
Background technology
Graphite-phase carbonitride (g-C
3n
4) be a kind of semi-conducting material, there is the layer structure of similar graphite, in molecule, there is the large ∏ key of conjugation, there is good chemical stability and heat endurance.Owing to thering is suitable energy gap, g-C
3n
4can photolysis water hydrogen under visible ray condition, degradable organic pollutant, initiation organic reaction etc., thereby be with a wide range of applications.Due to body phase g-C
3n
4light induced electron hole separative efficiency not high, cause its catalytic activity lower, so people adopt multiple method of modifying to improve g-C
3n
4photocatalytic activity.Wherein by pattern, control preparation nanometer g-C
3n
4a kind of effective approach, because the specific area of material increases the activated centre that is conducive to increase material.But current nanometer g-C
3n
4preparation there is inefficiency [S. Yang, Y. Gong, J. Zhang. et al. Adv. Mater. 2013,25,2452], or course of reaction need be introduced a large amount of concentrated sulfuric acids and the potential safety hazard [application number 201210370150.2] that causes.How by method simple, cheap, that be easy to industrialization production requirements, to prepare eco-friendly nanometer g-C
3n
4and compound becomes the focus of current research.
Summary of the invention
The object of the present invention is to provide a kind of bentonite/graphite-phase carbonitride composite and preparation method thereof, to improve visible light photocatalytic degradation of organic pollutants and photocurrent response performance.
Graphite-phase carbonitride, hereinafter to be referred as g-C
3n
4, bentonite/graphite-phase carbonitride composite is called again bentonite/g-C
3n
4composite.
A preparation method for bentonite/graphite-phase carbonitride composite, is characterized in that comprising the following steps:
Step 1, dicyandiamide is soluble in water, make mass percentage concentration and be 5～20% dicyandiamide solution;
Step 4, is transferred to described sample in crucible, adds a cover, and be placed in Muffle furnace and calcine, and insulation, then naturally cool to room temperature, obtain product;
In described step 2 solution one, the mass ratio of bentonite and dicyandiamide is 1:5～1:30.
In described step 3, the temperature of drying solution one is 70～90 ℃.
In described step 4, calcining heat is 520～550 ℃, and temperature retention time is at 3～6 h; During calcining, heating rate is 2～10 ℃/min.
Bentonite/graphite-phase carbonitride composite, is characterized in that: according to above-described preparation method's preparation, obtain, the percentage composition of bentonite accounts for 5%-30%.
the present invention has beneficial effect.The present invention is by the dicyandiamide aqueous solution is mixed with bentonite, dry, grinds, and calcining, pulverizes, and prepares the bentonite/g-C of lamellar structure
3n
4composite, makes it have good visible light photocatalytic degradation of organic pollutants performance and photocurrent response performance.The present invention is simple, and product cost is low, and environmental friendliness is easy to suitability for industrialized production, has very high application prospect and practical value.
Accompanying drawing explanation
Fig. 1 is control sample g-C
3n
4with bentonite/g-C of the present invention
3n
4the X-ray diffractogram of composite.
Fig. 2 is control sample g-C
3n
4with bentonite/g-C of the present invention
3n
4the transmission electron microscope picture of composite.
Fig. 3 is control sample g-C
3n
4with bentonite/g-C of the present invention
3n
4the infrared spectrogram of composite.
Fig. 4 is control sample g-C
3n
4with bentonite/g-C of the present invention
3n
4the performance map of composite catalytic degradation methylene blue under visible ray.
Fig. 5 is control sample g-C
3n
4, bentonite and bentonite/g-C of the present invention
3n
4composite is photocurrent response performance map under visible ray.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, technical scheme of the present invention is described in further detail.
In following embodiment, material used, reagent etc., if no special instructions, all can obtain from commercial channels.
Calcining preparation g-C
3n
4: take 5.0 g dicyandiamides and be placed in 50 mL crucibles, add a cover, be placed in Muffle furnace, the heating that heats up in air atmosphere, heating rate is 5 ℃/min, is warming up to 530 ℃, then at 530 ℃ of insulation 4 h, naturally cooling after, obtain g-C
3n
4solid, grind stand-by, sample in contrast.
embodiment 1
Take 5 g dicyandiamides and be dissolved in 20 g water, make 20% dicyandiamide solution; Under stirring, 0.167 g bentonite is dispersed in dicyandiamide solution; By this solution, in 70 ℃ of oven dry, gained solid grinds; Sample after grinding is transferred in 50 mL crucibles, adds a cover, be placed in Muffle furnace, heating heats up in air atmosphere, heating rate is 2 ℃/min, is warming up to 550 ℃, then at 550 ℃ of insulation 3 h, naturally cool to room temperature, product is ground, obtain described bentonite/g-C
3n
4composite.The present embodiment gained bentonite/g-C
3n
4composite and control sample g-C
3n
4x-ray diffractogram as shown in Figure 1.
Take 5 g dicyandiamides and be dissolved in 45 g water, make 10% dicyandiamide solution; Under stirring, 0.5 g bentonite is dispersed in dicyandiamide solution; By this solution, in 80 ℃ of oven dry, gained solid grinds; Sample after grinding is transferred in 50 mL crucibles, adds a cover, be placed in Muffle furnace, heating heats up in air atmosphere, heating rate is 5 ℃/min, is warming up to 530 ℃, then at 530 ℃ of insulation 5 h, naturally cool to room temperature, product is ground, obtain described bentonite/g-C
3n
4composite, its transmission electron microscope picture as shown in Figure 2, control sample g-C wherein
3n
4for the solid particle of reuniting, and composite is lamellar structure.
Take 5 g dicyandiamides and be dissolved in 75 g water, make 6.5% dicyandiamide solution; Under stirring, 0.7 g bentonite is dispersed in dicyandiamide solution; By this solution, in 90 ℃ of oven dry, gained solid grinds; Sample after grinding is transferred in 50 mL crucibles, adds a cover, be placed in Muffle furnace, heating heats up in air atmosphere, heating rate is 7 ℃/min, is warming up to 520 ℃, then at 520 ℃ of insulation 6 h, naturally cool to room temperature, product is ground, obtain described bentonite/g-C
3n
4composite.Gained bentonite/g-C
3n
4composite and control sample g-C
3n
4infrared spectrogram as shown in Figure 3.
embodiment 4
Take 5 g dicyandiamides and be dissolved in 95 g water, make 5% dicyandiamide solution; Under stirring, 1.0 g bentonite are dispersed in dicyandiamide solution; By this solution, in 80 ℃ of oven dry, gained solid grinds; Sample after grinding is transferred in 50 mL crucibles, adds a cover, be placed in Muffle furnace, heating heats up in air atmosphere, heating rate is 10 ℃/min, is warming up to 530 ℃, then at 530 ℃ of insulation 5 h, naturally cool to room temperature, product is ground, obtain described bentonite/g-C
3n
4composite.
Bentonite/g-C
3n
4the photocatalysis performance evaluation of composite: compound concentration is 6.25 * 10
-5molL
-1methylene blue solution 100 mL, add 0.100 g
the bentonite that embodiment 2 is prepared/ g-C
3n
4composite, lucifuge magnetic agitation 30 min are to system adsorption equilibrium, and the 300 W xenon lamps of take are light source, install 420 nm optical filters additional, and the absorbance of measuring methylene blue solution at 663 nm wavelength places with ultraviolet-visible spectrophotometer, carries out light degradation experiment, with C/C
0the mapping of～time, the photocatalytic activity of exosyndrome material, wherein C
0, C is respectively the concentration of methylene blue before and after photocatalytic degradation.Under similarity condition, carry out g-C
3n
4light degradation experiment, result as shown in Figure 4, visible bentonite/g-C
3n
4composite has the g-C of ratio
3n
4better Photocatalytic activity.
embodiment 6
Bentonite/g-C
3n
4the photocurrent response performance evaluation of composite: adopt CHI660B type electrochemical workstation working sample photoelectric current, adopt three-electrode system, tin indium oxide (ITO) glass-carbon electrode of usining is modified after sample as working electrode, Ag/AgCl (saturated KCl solution) is reference electrode, platinum filament is auxiliary electrode, electrolyte Na
2sO
4solution concentration is 0.1 mol/L.Visible light source is 300 W xenon lamps, installs 420 nm optical filters additional.Under similarity condition, carry out g-C
3n
4photocurrent response performance test with bentonite.Control sample g-C
3n
4, the bentonite/g-C in bentonite and embodiment 4
3n
4the photocurrent response performance of composite under visible ray as shown in Figure 5, visible bentonite/g-C
3n
4composite has the g-C of ratio when illumination
3n
4stronger photoelectric current.
Claims (6)
1. a preparation method for bentonite/graphite-phase carbonitride composite, is characterized in that comprising the following steps:
Step 1, dicyandiamide is soluble in water, make mass percentage concentration and be 5～20% dicyandiamide solution;
Step 2, under stirring, is dispersed in described dicyandiamide solution to obtain solution one by bentonite;
Step 3, dries described solution one, obtains solids, then grinds described solids and obtains sample;
Step 4, is transferred to described sample in crucible, adds a cover, and be placed in Muffle furnace and calcine, and insulation, then naturally cool to room temperature, obtain product;
Step 5, grinds described product, obtains described bentonite/graphite-phase carbonitride composite.
2. the preparation method of a kind of bentonite/graphite-phase carbonitride composite according to claim 1, is characterized in that: in described step 2 solution one, the mass ratio of bentonite and dicyandiamide is 1:5～1:30.
3. the preparation method of a kind of bentonite/graphite-phase carbonitride composite according to claim 1, is characterized in that: in described step 3, the temperature of drying solution one is 70～90 ℃.
4. the preparation method of a kind of bentonite/graphite-phase carbonitride composite according to claim 1, is characterized in that: in described step 4, calcining heat is 520～550 ℃, and temperature retention time is at 3～6 h.
5. the preparation method of a kind of bentonite/graphite-phase carbonitride composite according to claim 4, is characterized in that: during calcining, heating rate is 2～10 ℃/min.
6. bentonite/graphite-phase carbonitride composite, is characterized in that: according to the preparation method's preparation described in claim 1,2,3,4 or 5, obtain.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111174A (en) * | 2016-06-17 | 2016-11-16 | 中国矿业大学(北京) | G C3N4/ kaolinite composite photo-catalyst and preparation method thereof |
| CN110252379A (en) * | 2019-07-10 | 2019-09-20 | 西北师范大学 | A kind of preparation and application of palygorskite/graphite-phase carboritride composite material |
| CN112058290A (en) * | 2020-01-21 | 2020-12-11 | 中国石油大学(华东) | Application of photocatalytic modified material in removing ocean oil spill |
| CN112756008A (en) * | 2021-01-13 | 2021-05-07 | 合肥工业大学 | Iron-doped carbon nitride diatomite composite material and preparation method and application thereof |
-
2014
- 2014-01-02 CN CN201410000800.3A patent/CN103691473B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 黄立英等: ""无机化学实验WO3/g-C3N4杂化材料的制备及其光催化性能"", 《考试周刊》, no. 58, 31 December 2013 (2013-12-31), pages 152 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111174A (en) * | 2016-06-17 | 2016-11-16 | 中国矿业大学(北京) | G C3N4/ kaolinite composite photo-catalyst and preparation method thereof |
| CN110252379A (en) * | 2019-07-10 | 2019-09-20 | 西北师范大学 | A kind of preparation and application of palygorskite/graphite-phase carboritride composite material |
| CN112058290A (en) * | 2020-01-21 | 2020-12-11 | 中国石油大学(华东) | Application of photocatalytic modified material in removing ocean oil spill |
| CN112058290B (en) * | 2020-01-21 | 2023-05-26 | 中国石油大学(华东) | Application of photocatalysis modified material in removing marine spilled oil |
| CN112756008A (en) * | 2021-01-13 | 2021-05-07 | 合肥工业大学 | Iron-doped carbon nitride diatomite composite material and preparation method and application thereof |
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| CN103691473B (en) | 2015-10-28 |
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