CN104401948A - Preparation method for single-layer graphite-type carbon nitride nanosheet solution - Google Patents

Preparation method for single-layer graphite-type carbon nitride nanosheet solution Download PDF

Info

Publication number
CN104401948A
CN104401948A CN201410653994.7A CN201410653994A CN104401948A CN 104401948 A CN104401948 A CN 104401948A CN 201410653994 A CN201410653994 A CN 201410653994A CN 104401948 A CN104401948 A CN 104401948A
Authority
CN
China
Prior art keywords
solution
carbon nitride
graphite type
ultrasonic
nitride powder
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.)
Pending
Application number
CN201410653994.7A
Other languages
Chinese (zh)
Inventor
阎鑫
郭豪彦
赵佳伟
王慧
陶婧颖
王轩
赵鹏
艾涛
苏兴华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changan University
Original Assignee
Changan University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Changan University filed Critical Changan University
Priority to CN201410653994.7A priority Critical patent/CN104401948A/en
Publication of CN104401948A publication Critical patent/CN104401948A/en
Pending legal-status Critical Current

Links

Landscapes

  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a preparation method for a single-layer graphite-type carbon nitride nanosheet solution. The preparation method comprises the following steps: selecting tripolycyanamide or urea or bipolydicyanamide as a precursor, and performing pyrolytic reaction to obtain graphite-type carbon nitride powder; weighing carbon nitride powder, putting the carbon nitride powder into a ball milling jar with an aqueous solution of a polar solvent or a surfactant, and putting into a jar mill for ball milling; after ball milling for a certain time, pouring out a suspension, performing ultrasonic exfoliation by using an ultrasonic dispersion instrument, and centrifuging the obtained solution; taking a supernatant, namely the single-layer graphite-type carbon nitride nanosheet solution. Compared with the prior art that the single-layer graphite-type carbon nitride nanosheet solution is obtained by using a high-power ultrasonic exfoliation instrument, the preparation method provided by the invention has the advantages as follows: after ball milling pretreatment, the ultrasonic exfoliation on the carbon nitride powder is carried out, so that energy consumption is lower in the preparation process, and the prepared graphite-type carbon nitride nanosheet solution is higher in concentration and relatively low in cost.

Description

A kind of preparation method of mono-layer graphite type azotized carbon nano sheet solution
Technical field
The invention belongs to field of nanometer material technology, be specifically related to a kind of preparation method of mono-layer graphite type azotized carbon nano sheet solution.
Background technology
Graphite phase carbon nitride is because of its chemical heat good stability, the nontoxic and performance that raw material is easy to get, containing metal etc. is unexcellent and be subject to the extensive concern of countries in the world researcher.Particularly Late Cambrian graphite phase carbon nitride has excellent photocatalytic hydrogen production by water decomposition performance and causes the dense research interest of people especially in recent years.Graphite phase carbon nitride is laminate structure, be strong chemical bond in layer, interlayer is extremely weak Van der Waals force, can obtain single-layer silicon nitride carbon nanosheet by the Van der Waals force between breakable layer, the azotized carbon nano sheet of this two-dirnentional structure is with a wide range of applications in fields such as nanoelectronics, friction, catalysis, the energy and high performance matrix materials.The method preparing mono-layer graphite phase carbon nitride nanometer sheet at present has hot etching method, liquid phase stripping method.Hot etching method preparation amount is less, and processing parameter is difficult to control, and is difficult to meet industrial requirement.Liquid phase of comparing stripping method can obtain the individual layer nanometer sheet product of high yield, and liquid phase stripping process is easy and other metallic compound forms nano composite material, greatly promote the performance and application field (SunYanjuan etc. of single-layer silicon nitride carbon, Growth of BiOBr nanosheets on C3N4nanosheetsto construct two-dimensional nanojunctions with enhanced photoreactivity for NO removal, Journalof Colloid and Interface Science, 2014,418:317-323; Cao Shao-Wen etc., In-situ growth of CdSquantum dots on g-C3N4nanosheets for highly efficient photocatalytic hydrogen generation undervisible light irradiation, International Journal o f Hydrogen Energy, 2013,38:1258-1266).Current liquid phase stripping means is all directly adopt carbonitride powder to obtain (Zhang Xiaodong etc. in the ultrasonic stripping of different solvents, Enhancedphotoresponsive ultrathin g-C3N4nanosheets for bioimaging, Journal of the American ChemicalSociety, 2012,135:18-21; Yang Shubin etc., Exfoliated Graphitic Carbon Nitride Nanosheets asEfficient Catalysts for Hydrogen Evolution Under Visible Light, Advanced Materials, 2013,25,2452-2456).The cycle in reaction times of carbonitride powder direct ultrasonic stripping is in a solvent longer, and energy consumption is higher, is unfavorable for suitability for industrialized production.The solvent species adopted in simultaneous reactions is fewer, and this makes when preparing single-layer silicon nitride carbon nanosheet and other metal forms nano composite material, needs more complicated technique.In addition, the concentration of the mono-layer graphite phase carbon nitride nanometer sheet solution using liquid phase stripping means to prepare at present is only 0.15mg/mL.Therefore, study a kind of technique simple, the with low cost and method tool with the mono-layer graphite phase carbon nitride nanometer sheet solution of high density is of great significance.
Summary of the invention
The object of the invention is to solve the problems of the prior art, provide a kind of preparation method of mono-layer graphite type azotized carbon nano sheet solution, its technique is simple, with low cost, is easy to industrialization.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for mono-layer graphite type azotized carbon nano sheet solution, comprises the following steps:
1) choosing trimeric cyanamide, urea or dimerization dicyanamide is presoma, obtains graphite type carbon nitride powder by heat polymerization; Choose the aqueous solution of a kind of polar solvent or tensio-active agent, graphite type carbon nitride powder is added in the aqueous solution of selected polar solvent or tensio-active agent, obtain solution A, then solution A is put into ball grinder, and be placed on jar mill and carry out ball milling 12 ~ 24h, obtain carbonitride suspension solution; Wherein, in solution A, the concentration of carbonitride powder is 2.5 ~ 5mg/mL;
2) take out the carbonitride suspension solution after ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, interim, ultrasonic power 100 ~ 200w, ultrasonic time 0.5 ~ 1h;
3) solution after ultrasonic stripping is carried out centrifugal treating 0.5 ~ 1h, centrifuge speed 3000 ~ 4000rpm, get supernatant liquid and namely obtain mono-layer graphite type azotized carbon nano sheet solution.
The present invention further improves and is, step 1) in, the polar solvent selected in ball milling is the one in water, aqueous ethanolic solution, N-Methyl pyrrolidone or the N-Methyl pyrrolidone aqueous solution.
The present invention further improves and is, in the polar solvent aqueous ethanolic solution selected in ball milling, the volume ratio of water and ethanol is (1 ~ 10): 1; In the N-Methyl pyrrolidone aqueous solution, the volume ratio of water and N-Methyl pyrrolidone is (1 ~ 5): 1.
The present invention further improves and is, the tensio-active agent selected in ball milling is the one in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium laurylsulfonate or Sodium cholic acid.
The present invention further improves and is, the concentration of aqueous solution of tensio-active agent is 0.75 ~ 1.5mg/mL.
Compared with prior art, the present invention adopts and graphite type carbon nitride powder is carried out pre-treatment by ball-milling technology, under ball-milling technology condition, grinding medium fully contacts with graphite type carbon nitride powder, grinding medium produces two kinds of physical force to graphite type carbon nitride, one is shearing force, can carry out thinning from graphite type carbon nitride body structure surface; Secondly squeeze, can carry out thinning from graphite type carbon nitride structural edge.The net result of (accompanying drawing 1 is shown in by schematic diagram) two kinds of reactive forces is by thinning for graphite type carbon nitride multilayered structure, thus interlamellar spacing is widened, the model ylid bloom action power between further reducing layer.And in whole mechanism, the two-dimensional surface texture of carbonitride is not damaged, also can not introduce other impurity.By graphite type carbon nitride after ball milling pretreatment, then carry out ultrasonic stripping.Under ultrasonication, graphite type carbon nitride powder after ball milling pretreatment is easy to come off into mono-layer graphite type azotized carbon nano sheet, substantially increase the efficiency of ultrasonic stripping graphite type carbon nitride like this, thus improve mono-layer graphite type azotized carbon nano sheet content in the solution.
Using graphite type carbon nitride powder directly to carry out ultrasonic stripping with prior art obtains compared with mono-layer graphite type azotized carbon nano sheet solution, the present invention carries out ball-milling processing by ball-milling technology to graphite phase carbon nitride powder, graphite phase carbon nitride is in the solvent chosen or tensio-active agent, by grinding medium to the shearing of graphite phase carbon nitride powder and extruding physical action, thus making graphite phase carbon nitride interlayer thinning, reactive force reduces.Again through ultrasonic stripping, can obtain mono-layer graphite phase carbon nitride nanometer sheet solution, its preparation technology is simple, and energy consumption is low, and the mono-layer graphite type azotized carbon nano sheet concentration obtained is high.
Accompanying drawing explanation
Fig. 1 is the mechanism of action figure of ball-milling technology of the present invention to graphite type carbon nitride powder.
Fig. 2 is the XRD figure of powder after the mono-layer graphite type azotized carbon nano sheet solution drying that obtains of the present invention.
Fig. 3 is transmission electron microscope (TEM) shape appearance figure of the mono-layer graphite type azotized carbon nano sheet solution that the present invention obtains.
Fig. 4 is the concentration map of azotized carbon nano sheet solution obtained under embodiment 1-embodiment 13 condition.
Embodiment
Below in conjunction with the drawings and specific embodiments, particular content of the present invention is described in further detail.
Embodiment 1
First prepare graphite type carbon nitride powder, the trimeric cyanamide taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.5g graphite type carbon nitride powder and be placed in the ball grinder that 200ml water is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 2.5mg/mL, is placed in by ball grinder on jar mill ball milling 24h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 200w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 1h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 1.5mg/mL.
Embodiment 2
First prepare graphite type carbon nitride powder, the trimeric cyanamide taking 15g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 1g graphite type carbon nitride powder and be placed in the ball grinder that 200ml water/ethanol (volume ratio is 10/1) is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 5mg/mL, is placed in by ball grinder on jar mill ball milling 12h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 100w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 0.5h, centrifuge speed 3000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.65mg/mL.
Embodiment 3
First prepare graphite type carbon nitride powder, the dimerization dicyanamide taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.8g graphite type carbon nitride powder and be placed in the ball grinder that 200ml water/ethanol (volume ratio is 6/1) is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 4mg/mL, is placed in by ball grinder on jar mill ball milling 20h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 120w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 1h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.6mg/mL.
Embodiment 4
First prepare graphite type carbon nitride powder, the trimeric cyanamide taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.6g graphite type carbon nitride powder and be placed in the ball grinder that 200ml water/ethanol (volume ratio is 1/1) is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 3mg/mL, is placed in by ball grinder on jar mill ball milling 18h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 200w, ultrasonic time 0.7h; Solution through ultrasonic stripping is carried out centrifugal treating 0.6h, centrifuge speed 3000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.7mg/mL.
Embodiment 5
First prepare graphite type carbon nitride powder, the urea taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 1g graphite type carbon nitride powder and be placed in the ball grinder that 200ml N-Methyl pyrrolidone is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 5mg/mL, is placed in by ball grinder on jar mill ball milling 24h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 200w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 1h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 1.4mg/mL.
Embodiment 6
First prepare graphite type carbon nitride powder, the trimeric cyanamide taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.8g graphite type carbon nitride powder and be placed in the ball grinder that 200ml water/N-Methyl pyrrolidone (volume ratio is 1/1) is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 4mg/mL, is placed in by ball grinder on jar mill ball milling 14h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 160w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 0.5h, centrifuge speed 3000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.5mg/mL.
Embodiment 7
First prepare graphite type carbon nitride powder, the trimeric cyanamide taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.6g graphite type carbon nitride powder and be placed in the ball grinder that 200ml water/N-Methyl pyrrolidone (volume ratio is 3/1) is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 3mg/mL, is placed in by ball grinder on jar mill ball milling 16h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 120w, ultrasonic time 0.5h; Solution through ultrasonic stripping is carried out centrifugal treating 0.7h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.55mg/mL.
Embodiment 8
First prepare graphite type carbon nitride powder, the trimeric cyanamide taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.6g graphite type carbon nitride powder and be placed in the ball grinder that 200ml water/N-Methyl pyrrolidone (volume ratio is 5/1) is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 3mg/mL, is placed in by ball grinder on jar mill ball milling 18h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 140w, ultrasonic time 0.5h; Solution through ultrasonic stripping is carried out centrifugal treating 0.7h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.6mg/mL.
Embodiment 9
First prepare graphite type carbon nitride powder, the urea taking 15g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.8g graphite type carbon nitride powder to be placed in the ball grinder that 200ml concentration is 0.75mg/mL sodium dodecyl benzene sulfonate aqueous solution is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 4mg/mL, is placed in by ball grinder on jar mill ball milling 16h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 100w, ultrasonic time 0.5h; Solution through ultrasonic stripping is carried out centrifugal treating 0.7h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.7mg/mL.
Embodiment 10
First prepare graphite type carbon nitride powder, the dimerization dicyanamide taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 1g graphite type carbon nitride powder to be placed in the ball grinder that 200ml concentration is 1mg/mL lauryl sodium sulfate aqueous solution is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 5mg/mL, is placed in by ball grinder on jar mill ball milling 20h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 180w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 0.5h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 1.0mg/mL.
Embodiment 11
First prepare graphite type carbon nitride powder, the urea taking 10g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 0.9g graphite type carbon nitride powder to be placed in the ball grinder that 200ml concentration is 1.5mg/mL sodium dodecyl sulfate aqueous solution is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 4.5mg/mL, is placed in by ball grinder on jar mill ball milling 24h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 100w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 0.5h, centrifuge speed 4000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.75mg/mL.
Embodiment 12
First prepare graphite type carbon nitride powder, the dimerization dicyanamide taking 15g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 1g graphite type carbon nitride powder to be placed in the ball grinder that 200ml concentration is 1.25mg/mL sodium dodecyl sulfate aqueous solution is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 5mg/mL, is placed in by ball grinder on jar mill ball milling 20h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 100w, ultrasonic time 1h; Solution through ultrasonic stripping is carried out centrifugal treating 0.5h, centrifuge speed 3000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.6mg/mL.
Embodiment 13
First prepare graphite type carbon nitride powder, the dimerization dicyanamide taking 15g, in crucible, is placed in retort furnace, is warming up to 550 DEG C of thermal treatment 4h, for subsequent use after taking out grinding after cooling; Take 1g graphite type carbon nitride powder to be placed in the ball grinder that 200ml concentration is the 1mg/mL Sodium cholic acid aqueous solution is housed, it is 1mm zirconium white microballon that 500 diameters are wherein housed in grinding pot.The concentration of graphite type carbon nitride powder is 5mg/mL, is placed in by ball grinder on jar mill ball milling 12h (as shown in Figure 1); Take out the carbonitride suspension solution through ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, ultrasonic power 100w, ultrasonic time 0.7h; Solution through ultrasonic stripping is carried out centrifugal treating 0.5h, centrifuge speed 3000rpm, get supernatant liquid and can obtain mono-layer graphite type azotized carbon nano sheet solution, its concentration is 0.55mg/mL.
As shown in Figures 2 to 4, Fig. 2 is the XRD figure of powder after the mono-layer graphite type azotized carbon nano sheet solution drying that obtains of the present invention; Wherein, the X-ray diffraction equipment used is Rigaku Rigaku D/Max-2400 type X-ray diffractometer, and x-ray source is Cu target.Diffraction peaks all in figure is graphite type carbon nitride characteristic diffraction peak, does not have other dephasign composition.Fig. 3 is transmission electron microscope (TEM) shape appearance figure of the mono-layer graphite type azotized carbon nano sheet solution that the present invention obtains; Wherein, the transmission electron microscope equipment used is Dutch FEI Co. Tecnai F30 type transmission electron microscope, and acceleration voltage is 300kV.Can find out in figure that the azotized carbon nano sheet of preparation is single layer structure really.Fig. 4 is the concentration map of azotized carbon nano sheet solution obtained under embodiment 1-embodiment 13 condition.What X-coordinate represented is that sample specimens number (is respectively 1-13 from embodiment 1-embodiment 13,14 is document Zhang Xiaodong etc., Enhanced photoresponsive ultrathin g-C3N4nanosheets forbioimaging, Journal of the American Chemical Society, the ultrasonic stripping of 2012,135:18-21 obtains azotized carbon nano sheet solution example) ordinate zou represents is the concentration (unit is mg/mL) of azotized carbon nano sheet solution.As can be seen from the figure the present invention can obtain the concentration of the azotized carbon nano sheet solution of greater concn.

Claims (5)

1. a preparation method for mono-layer graphite type azotized carbon nano sheet solution, is characterized in that: comprise the following steps:
1) choosing trimeric cyanamide, urea or dimerization dicyanamide is presoma, obtains graphite type carbon nitride powder by heat polymerization; Choose the aqueous solution of a kind of polar solvent or tensio-active agent, graphite type carbon nitride powder is added in the aqueous solution of selected polar solvent or tensio-active agent, obtain solution A, then solution A is put into ball grinder, and be placed on jar mill and carry out ball milling 12 ~ 24h, obtain carbonitride suspension solution; Wherein, in solution A, the concentration of carbonitride powder is 2.5 ~ 5mg/mL;
2) take out the carbonitride suspension solution after ball-milling processing, be placed in ultrasonic disperse instrument and carry out ultrasonic stripping, interim, ultrasonic power 100 ~ 200w, ultrasonic time 0.5 ~ 1h;
3) solution after ultrasonic stripping is carried out centrifugal treating 0.5 ~ 1h, centrifuge speed 3000 ~ 4000rpm, get supernatant liquid and namely obtain mono-layer graphite type azotized carbon nano sheet solution.
2. a kind of method preparing mono-layer graphite type azotized carbon nano sheet solution according to claim 1, it is characterized in that, step 1) in, the polar solvent selected in ball milling is the one in water, aqueous ethanolic solution, N-Methyl pyrrolidone or the N-Methyl pyrrolidone aqueous solution.
3. a kind of method preparing mono-layer graphite type azotized carbon nano sheet solution according to claim 2, it is characterized in that, in the polar solvent aqueous ethanolic solution selected in ball milling, the volume ratio of water and ethanol is (1 ~ 10): 1; In the N-Methyl pyrrolidone aqueous solution, the volume ratio of water and N-Methyl pyrrolidone is (1 ~ 5): 1.
4. a kind of method preparing mono-layer graphite type azotized carbon nano sheet solution according to claim 1, it is characterized in that, the tensio-active agent selected in ball milling is the one in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium laurylsulfonate or Sodium cholic acid.
5. a kind of method preparing mono-layer graphite type azotized carbon nano sheet solution according to claim 4, it is characterized in that, the concentration of aqueous solution of tensio-active agent is 0.75 ~ 1.5mg/mL.
CN201410653994.7A 2014-11-17 2014-11-17 Preparation method for single-layer graphite-type carbon nitride nanosheet solution Pending CN104401948A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410653994.7A CN104401948A (en) 2014-11-17 2014-11-17 Preparation method for single-layer graphite-type carbon nitride nanosheet solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410653994.7A CN104401948A (en) 2014-11-17 2014-11-17 Preparation method for single-layer graphite-type carbon nitride nanosheet solution

Publications (1)

Publication Number Publication Date
CN104401948A true CN104401948A (en) 2015-03-11

Family

ID=52639636

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410653994.7A Pending CN104401948A (en) 2014-11-17 2014-11-17 Preparation method for single-layer graphite-type carbon nitride nanosheet solution

Country Status (1)

Country Link
CN (1) CN104401948A (en)

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891460A (en) * 2015-05-29 2015-09-09 厦门大学 Method for preparing graphite-phase carbon nitride nanosheets by using solution phase
CN105195204A (en) * 2015-10-19 2015-12-30 合肥工业大学 Ultrafine g-C3N4 nano photocatalyst and preparation method thereof
CN105289684A (en) * 2015-09-29 2016-02-03 北京化工大学 Method for preparing porous flake-like graphite phase carbon nitride on large scale, and application thereof
CN105417507A (en) * 2015-12-10 2016-03-23 济南大学 Preparing method for carbon nitride nano particles and obtained product
CN105800571A (en) * 2016-02-26 2016-07-27 浙江大学 Preparation method for two-dimensional nanosheet carbon nitride material
CN106145069A (en) * 2016-06-29 2016-11-23 湖南大学 Graphite mould C3n4the preparation method of material, graphite mould C3n4material and application thereof
CN106752122A (en) * 2016-11-29 2017-05-31 东南大学 One kind nitridation carbon complex, its preparation method and application
CN106824190A (en) * 2017-03-03 2017-06-13 中国科学技术大学先进技术研究院 A kind of WO3‑xNanocatalyst and its preparation, application
CN107118575A (en) * 2017-04-14 2017-09-01 长安大学 Azotized carbon nano piece improves the application of pitch ageing resistace
CN107352517A (en) * 2017-07-21 2017-11-17 桂林理工大学 A kind of preparation method of the graphite phase carbon nitride nanometer bouquet with amorphous surface
CN108502856A (en) * 2018-06-14 2018-09-07 中国科学院兰州化学物理研究所 A kind of green economy preparation method of two dimension carbonitride
CN109668864A (en) * 2018-12-14 2019-04-23 福建中医药大学 Azotized carbon nano piece couples the ochratoxin A fluorescence detection method of aptamers sensing
CN109734060A (en) * 2019-02-18 2019-05-10 东南大学 Azotized carbon nano material and its preparation method and application
CN109847785A (en) * 2019-02-25 2019-06-07 牟富书 A kind of preparation method nitrogenizing carbon colloid
CN109908937A (en) * 2019-03-25 2019-06-21 黄河三角洲京博化工研究院有限公司 A kind of preparation method of nanoscale visible light catalyst
CN110479099A (en) * 2019-07-23 2019-11-22 福建农林大学 A kind of bionical nanofiltration membrane of high throughput and preparation method thereof based on lamellar graphite phase carbon nitride nanometer sheet
CN111234785A (en) * 2020-03-19 2020-06-05 中国石油天然气集团有限公司 Nano plugging agent for water-based drilling fluid, preparation method of nano plugging agent and water-based drilling fluid
CN112499604A (en) * 2020-11-20 2021-03-16 中国科学院深圳先进技术研究院 Graphite-like phase carbon nitride material with nitrogen vacancy density and preparation method thereof
CN112537770A (en) * 2020-12-07 2021-03-23 齐鲁工业大学 Preparation method of nitrogen-doped two-dimensional carbon nanosheet
CN115678124A (en) * 2022-11-28 2023-02-03 中国重汽集团济南动力有限公司 Natural rubber composite material for rubber support of heavy truck leaf spring and application thereof
CN115888790A (en) * 2022-11-14 2023-04-04 南京先进生物材料与过程装备研究院有限公司 Method for preparing carbon nitride nanosheet by using microchannel
CN116139927A (en) * 2023-02-20 2023-05-23 安徽农业大学 Organic micromolecule modified nano carbon nitride, preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103254200A (en) * 2013-05-22 2013-08-21 福州大学 C3N4 nanosheet with molecular-scale thickness as well as preparation method and application thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103254200A (en) * 2013-05-22 2013-08-21 福州大学 C3N4 nanosheet with molecular-scale thickness as well as preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LU HUA LI ET AL.: "Large-scale mechanical peeling of boron nitride nanosheets by low-energy ball milling", 《JOURNAL OF MATERIALS CHEMISTRY》, vol. 21, 31 December 2011 (2011-12-31), pages 11862 - 11866 *

Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104891460A (en) * 2015-05-29 2015-09-09 厦门大学 Method for preparing graphite-phase carbon nitride nanosheets by using solution phase
CN105289684A (en) * 2015-09-29 2016-02-03 北京化工大学 Method for preparing porous flake-like graphite phase carbon nitride on large scale, and application thereof
CN105195204A (en) * 2015-10-19 2015-12-30 合肥工业大学 Ultrafine g-C3N4 nano photocatalyst and preparation method thereof
CN105417507B (en) * 2015-12-10 2018-03-06 济南大学 A kind of preparation method and products obtained therefrom of azotized carbon nano particle
CN105417507A (en) * 2015-12-10 2016-03-23 济南大学 Preparing method for carbon nitride nano particles and obtained product
CN105800571A (en) * 2016-02-26 2016-07-27 浙江大学 Preparation method for two-dimensional nanosheet carbon nitride material
CN106145069A (en) * 2016-06-29 2016-11-23 湖南大学 Graphite mould C3n4the preparation method of material, graphite mould C3n4material and application thereof
CN106752122B (en) * 2016-11-29 2019-02-05 东南大学 A kind of nitridation carbon complex, preparation method and application
CN106752122A (en) * 2016-11-29 2017-05-31 东南大学 One kind nitridation carbon complex, its preparation method and application
CN106824190A (en) * 2017-03-03 2017-06-13 中国科学技术大学先进技术研究院 A kind of WO3‑xNanocatalyst and its preparation, application
CN106824190B (en) * 2017-03-03 2023-12-29 中国科学技术大学先进技术研究院 WO (WO) 3-x Nanometer catalyst and its preparation and application
CN107118575A (en) * 2017-04-14 2017-09-01 长安大学 Azotized carbon nano piece improves the application of pitch ageing resistace
CN107118575B (en) * 2017-04-14 2019-08-13 长安大学 The application of azotized carbon nano piece raising pitch anti-aging property
CN107352517A (en) * 2017-07-21 2017-11-17 桂林理工大学 A kind of preparation method of the graphite phase carbon nitride nanometer bouquet with amorphous surface
CN108502856A (en) * 2018-06-14 2018-09-07 中国科学院兰州化学物理研究所 A kind of green economy preparation method of two dimension carbonitride
CN109668864A (en) * 2018-12-14 2019-04-23 福建中医药大学 Azotized carbon nano piece couples the ochratoxin A fluorescence detection method of aptamers sensing
CN109734060A (en) * 2019-02-18 2019-05-10 东南大学 Azotized carbon nano material and its preparation method and application
CN109734060B (en) * 2019-02-18 2020-12-25 东南大学 Carbon nitride nano material and preparation method and application thereof
CN109847785A (en) * 2019-02-25 2019-06-07 牟富书 A kind of preparation method nitrogenizing carbon colloid
CN109908937A (en) * 2019-03-25 2019-06-21 黄河三角洲京博化工研究院有限公司 A kind of preparation method of nanoscale visible light catalyst
CN110479099A (en) * 2019-07-23 2019-11-22 福建农林大学 A kind of bionical nanofiltration membrane of high throughput and preparation method thereof based on lamellar graphite phase carbon nitride nanometer sheet
CN110479099B (en) * 2019-07-23 2021-02-02 福建农林大学 High-flux bionic nanofiltration membrane based on layered graphite phase carbon nitride nanosheets and preparation method thereof
CN111234785A (en) * 2020-03-19 2020-06-05 中国石油天然气集团有限公司 Nano plugging agent for water-based drilling fluid, preparation method of nano plugging agent and water-based drilling fluid
CN111234785B (en) * 2020-03-19 2022-03-18 中国石油天然气集团有限公司 Nano plugging agent for water-based drilling fluid, preparation method of nano plugging agent and water-based drilling fluid
CN112499604A (en) * 2020-11-20 2021-03-16 中国科学院深圳先进技术研究院 Graphite-like phase carbon nitride material with nitrogen vacancy density and preparation method thereof
CN112537770A (en) * 2020-12-07 2021-03-23 齐鲁工业大学 Preparation method of nitrogen-doped two-dimensional carbon nanosheet
CN115888790A (en) * 2022-11-14 2023-04-04 南京先进生物材料与过程装备研究院有限公司 Method for preparing carbon nitride nanosheet by using microchannel
CN115678124A (en) * 2022-11-28 2023-02-03 中国重汽集团济南动力有限公司 Natural rubber composite material for rubber support of heavy truck leaf spring and application thereof
CN115678124B (en) * 2022-11-28 2024-01-26 中国重汽集团济南动力有限公司 Natural rubber composite material for heavy-duty truck spring rubber support and application thereof
CN116139927A (en) * 2023-02-20 2023-05-23 安徽农业大学 Organic micromolecule modified nano carbon nitride, preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN104401948A (en) Preparation method for single-layer graphite-type carbon nitride nanosheet solution
Hu et al. Rapid preparation, thermal stability and electromagnetic interference shielding properties of two-dimensional Ti3C2 MXene
Peng et al. A hydrothermal etching route to synthesis of 2D MXene (Ti3C2, Nb2C): Enhanced exfoliation and improved adsorption performance
CN108385124B (en) Preparation method of transition metal/carbon tube/graphene electrocatalyst for hydrogen evolution reaction
Gao et al. Preparation of MXene-Cu2O nanocomposite and effect on thermal decomposition of ammonium perchlorate
CN103934004B (en) A kind of stannic disulfide/graphene composite photocatalyst and preparation method thereof
CN105126876B (en) A kind of flower-shaped carbon load MoS2Composite of nano particle and preparation method thereof
CN109286009B (en) Preparation method of nano-sheet self-assembled three-dimensional nano-flower tin sulfide/graphitized carbon nitride lithium ion battery cathode material
CN103232458A (en) Method for preparing graphite phase carbon nitride material with monatomic layer structure
CN102153077A (en) Method for preparing single-layer graphene with high carbon-oxygen ratio
Ma et al. Microwave synthesis of cellulose/CuO nanocomposites in ionic liquid and its thermal transformation to CuO
CN105776154A (en) Preparation method of tungsten diselenide nanosheet
CN105600779B (en) The method that the full carbon three-dimensional grapheme of self assembly is prepared with black liquid
Wang et al. Hydrothermal synthesis and electrochemical performance of NiO microspheres with different nanoscale building blocks
CN104773720A (en) Method for preparing single-layer molybdenum disulfide flake doped graphene composite film
CN102891008A (en) Nickel hydroxide nanosheet thin-film material as well as preparation method and application thereof
CN104174422A (en) High nitrogen doped graphene and fullerene-like molybdenum selenide hollow-ball nanocomposite and preparation method thereof
CN103130276B (en) Preparation method of cadmium vanadate nanorods
CN102698774A (en) Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material
CN106058206A (en) Composite material of flower-like carbon-loaded MoS2 nanoparticles and preparation method and application thereof
CN103951916A (en) RGO (Reduced Graphene oxide)/ferric oxide-filled polyvinylidene fluoride composite wave-absorbing material and preparation method thereof
CN103693693A (en) Preparation method for synthesizing molybdenum sulfide nanospheres by microwave-assisted liquid phase deposition
CN104891485A (en) Method for preparing nano graphite sheet
CN107731550A (en) A kind of metal oxide/graphene composite material and its preparation method and application
CN105688969A (en) Preparation method of catalyst for photo-catalytically splitting water to produce hydrogen

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20150311