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Preparation method of nano-structure carbon nitride

A nanostructure, carbon nitride technology, applied in nanotechnology, nitrogen and non-metallic compounds, etc., can solve the problems of difficulty in obtaining, long-term peeling, low yield, etc., achieving low cost, short production cycle, and simple operation. Effect

Active Publication Date: 2016-06-22
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Currently, g-C 3 N 4 There are three main methods for exfoliation of layered materials, namely oxidative exfoliation, solvent exfoliation and intercalation exfoliation. However, there are also many problems, such as ultrasonic exfoliation requires a long time to exfoliate, and the yield is low; oxidative exfoliation requires high pressure or supercritical, And it is difficult to obtain g-C with good water solubility that can increase the contact area with the rest of the reactants during application. 3 N 4

Method used

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  • Preparation method of nano-structure carbon nitride
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  • Preparation method of nano-structure carbon nitride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Grind dicyandiamine, put it into a porcelain boat after passing through a 500-mesh sieve, and place it in a tube furnace, feed nitrogen at a flow rate of 5mL / min, and then raise the temperature to 550°C at a rate of 10°C / min , and kept warm for 2h, cooled to room temperature with the furnace, light yellow solid g-C 3 N 4 ;

[0040] (2) The light yellow solid g-C obtained in step (1) 3 N 4 Grind, pass through a 500-mesh sieve, and then take 100mg of sieved g-C 3 N 4 Add it into 20mL of potassium hydroxide aqueous solution with a concentration of 3mol / L, heat and condense to reflux at 80°C, stir for 24h, cool to room temperature, then sonicate the sample for 30min, and then use a dialysis bag with a molecular weight of 1500 to dialyze the filtrate for 3d to neutral , to obtain 20mL carbon nitride nano flake aqueous solution;

[0041] (3) Freeze-dry the carbon nitride nanobelt aqueous solution obtained in step (2) at -25°C for 72 hours to constant weight to obtai...

Embodiment 2

[0046] The difference between this embodiment and embodiment 1 is only:

[0047] In step (2), the reflux stirring time is 18h; the final product is carbon nitride nanoflakes, marked as g-C 3 N 4 -water-2. The rest are the same as embodiment 1.

[0048] After testing, the specific surface area of ​​carbon nitride nanosheets obtained in this example is 280m 2 g -1 , and the yield also reached 100wt%. Nanosheets with few layers of thickness can be obtained. The width of the obtained nanosheets is about 0.8-3.3 μm, and the sheets are much larger than those obtained in Example 1, resulting in a solution that is not as clear as in Example 1. g-C 3 N 4 -Water-2 After standing for a month, a very small amount of precipitation occurs at the bottom of the bottle, and the stability is not as good as that of g-C 3 N 4- Water1.

Embodiment 3

[0050] The difference between this embodiment and embodiment 1 is only:

[0051] In step (2), the reflux stirring time is 12h, marked as g-C 3 N 4 -water-3. The rest are the same as embodiment 1. After testing, the specific surface area of ​​carbon nitride nanosheets obtained in this example is 235m 2 g -1 , the width of the obtained nanosheets is about 1.2-3.6 μm, and the yield is 75wt%. The aqueous solution obtained in this embodiment is light milky white, and a small amount of precipitation occurs at the bottom of the bottle after standing for a week.

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Abstract

The invention relates to a preparation method of nano-structure carbon nitride. The method comprises the following steps: (1) grinding dicyanodiamine, screening, putting in a heater, introducing nitrogen, heating to 400-700 DEG C, keeping the temperature for 1-2 hours, and carrying out furnace cooling to room temperature, thereby obtaining a light yellow solid g-C3N4; (2) grinding the g-C3N4 obtained in the step (1), screening, adding into a potassium hydroxide or sodium hydroxide water or alcohol solution, carrying out heating and condensation under reflux, stirring, cooling to room temperature, carrying out ultrasonic treatment on the sample for 10-60 minutes, filtering to obtain a filtrate and a filter residue, and dialyzing the filtrate to obtain a nano-structure carbon nitride water solution; and (3) carrying out freeze-drying on the nano-structure carbon nitride water solution to constant weight, thereby obtaining the nano-structure carbon nitride. The nano-structure carbon nitride prepared by the method has the advantages of various shapes, favorable peeling degree, high specific area (up to 320 m<2>g<-1>), high water solubility and high stability. The method is simple, and has the advantages of mild reaction conditions, short production cycle and low cost.

Description

technical field [0001] The invention relates to a preparation method of nanostructured carbon nitride. Background technique [0002] Nanomaterials are a research hotspot in recent years. It has some special effects, such as surface effect, small size effect, quantum size effect, macroscopic quantum tunneling effect, etc. Performance, electrical properties, and chemical and catalytic properties, etc., have unparalleled characteristics of other materials. [0003] Carbon nitride is composed of two elements, carbon and nitrogen. It has abundant reserves, wide sources, simple synthesis method, good economy and easy access. Graphite carbon nitride (g-C 3 N 4 ) is a narrow bandgap semiconductor with a bandgap width of about 2.7eV, non-toxic, and metal-free; at the same time, g-C 3 N 4 It has a certain absorption of visible light, anti-acid, alkali and light corrosion, good stability, easy to control the structure and performance, and has good photocatalytic performance; g-C ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/082B82Y40/00
CPCC01B21/082C01P2004/01C01P2004/03C01P2004/04C01P2004/61C01P2004/62C01P2004/64C01P2006/12
Inventor 楚增勇邹贤帅费俊杰王春华蒋振华李公义李效东
Owner NAT UNIV OF DEFENSE TECH
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