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Preparation method of tubular carbon nitride

A carbon nitride, tubular technology, applied in nitrogen and non-metallic compounds, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problems of specific surface area decrease, large grain size, small specific surface area, etc., Achieve the effects of controllable shape, large specific surface area and wide application prospects

Inactive Publication Date: 2016-01-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] C prepared by traditional thermal polycondensation method 3 N 4 Most of them are arranged in lamellar stacks, and there is a phenomenon of easy agglomeration, which leads to problems such as a decrease in their specific surface area, and the C prepared by traditional thermal condensation polymerization 3 N 4 The material has a larger grain size and a smaller specific surface area, which also limits the C 3 N 4 Applications in the above aspects

Method used

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  • Preparation method of tubular carbon nitride
  • Preparation method of tubular carbon nitride

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Experimental program
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Effect test

Embodiment 1

[0021] 1) Add 100 grams of halloysite clay to 500 grams of hydrochloric acid solution with a hydrogen ion concentration of 0.5 mol / L, and stir and activate it for 1 hour at a temperature of 60° C. to obtain a silicate clay slurry. Add 120 grams of dicyandiamide The amine was added to the above silicate clay slurry, ultrasonically dispersed for 60 minutes: part of the water was evaporated to prepare the halloysite clay composite slurry.

[0022] 2) Transfer the halloysite clay composite slurry obtained in step 1 into a crucible, place it in a tube furnace at a heating rate of 8°C per minute, raise the temperature to 580°C, and keep it warm for 2 hours to obtain halloysite / C 3 N 4 Complex.

[0023] Halloysite / C will then be produced 3 N 4 The complex was added to a 10% hydrogen fluoride solution by mass percentage, allowed to stand for 12 hours, filtered and washed until the filtrate pH = 6, and dried at 80°C for 6 hours to obtain tubular C 3 N 4 .

Embodiment 2

[0025] 1) Add 90 grams of attapulgite clay to 300 grams of sulfuric acid solution with a hydrogen ion concentration of 3 mol / L, stir and activate for 4 hours at a temperature of 85°C to obtain a silicate clay slurry, and add 45 grams of melamine to the The attapulgite clay slurry was ultrasonically dispersed for 30 minutes; then part of the water was evaporated to prepare the attapulgite clay composite slurry.

[0026] 2) Transfer the attapulgite clay composite slurry obtained in step 1 into a crucible, place it in a tube furnace at a heating rate of 0.5°C per minute, raise the temperature to 450°C, and keep it warm for 5 hours to obtain attapulgite / C 3 N 4 Complex.

[0027] Then the prepared attapulgite / C 3 N 4 Add the complex to a 5% hydrogen fluoride solution by mass, let it stand for 24 hours, filter, wash until the filtrate pH=7, and dry at 80°C for 2 hours to obtain tubular C 3 N 4 .

Embodiment 3

[0029] 1) Add 80 grams of sepiolite clay to 200 grams of sulfuric acid mixed solution with a hydrogen ion concentration of 5 mol / L, stir and activate for 3 hours at a temperature of 75°C to obtain a silicate clay slurry, and add 160 grams of urea to the In the above sepiolite clay slurry, ultrasonically disperse for 45 minutes; then evaporate part of the water to prepare sepiolite clay composite slurry.

[0030] 2) Transfer the sepiolite clay composite slurry obtained in step 1 into a crucible, place it in a tube furnace at a heating rate of 15°C per minute, raise the temperature to 550°C, and keep it warm for 7 hours to obtain sepiolite / C 3 N 4 Complex.

[0031] Sepiolite / C will then be prepared 3 N 4 The complex was added to a 20% ammonium bifluoride solution by mass, allowed to stand for 18 hours, filtered and washed until the filtrate pH = 6.5, and vacuum-dried at 80°C for 10 hours to obtain a hollow tubular C 3 N 4 .

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Abstract

The invention belongs to the field of preparation of nano functional materials and particularly relates to a method of preparing tubular-structured carbon nitride with natural rod-like silicate clay as a template. The method includes the steps of adding the rod-like silicate clay to an acidic solution and performing stirring activation to obtain silicate clay slurry; adding a raw material being rich in carbon and nitrogen, performing ultrasonic dispersion to obtain silicate clay composite slurry; and treating the silicate clay composite slurry at 450-580 DEG C with temperature maintenance for 2-7 h to obtain a silicate clay / C3N4 composition; and finally adding the silicate clay / C3N4 composition into a hydrogen fluoride or an ammonium bifluoride solution, allowing the mixture to stand, and filtering, washing and drying the mixture to obtain the tubular carbon nitride.

Description

technical field [0001] The invention belongs to the field of preparation of nanometer functional materials, and in particular relates to a method for preparing tubular carbon nitride by using natural rod-shaped silicate clay as a template. Background technique [0002] Carbon Nitride (C 3 N 4 ) has a unique graphite-like layered stacking structure and sp 2 The hybrid π-conjugated electronic band structure has a variety of incomparable physical and chemical properties, and has broad application prospects in the fields of materials, catalysis, electronics, and optics. [0003] C prepared by traditional thermal polycondensation method 3 N 4 Most of them are arranged in lamellar stacks, and there is a phenomenon of easy agglomeration, which leads to problems such as a decrease in their specific surface area, and the C prepared by traditional thermal condensation polymerization 3 N 4 The material has a larger grain size and a smaller specific surface area, which also limits...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/082B82Y30/00B82Y40/00
Inventor 姚超李俊乾左士祥刘文杰吴凤芹李霞章
Owner CHANGZHOU UNIV
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