CN105217596A - A kind of cobalt-chloride catalyst prepares the preparation method of carbon nanotube - Google Patents

Abstract

The invention discloses a method for preparing carbon nanotubes with a cobalt chloride catalyst. The carbon nanotubes are obtained by using glucose, melamine and cobalt chloride as raw materials through steps of mixing, drying, roasting, pickling and the like. The length is 5-30 microns and the tube diameter is 200-300 nanometers. The preparation process of the carbon nanotube disclosed by the invention has the advantages of simplicity, safety, low cost, easy operation and controllability.

Description

A kind of preparation method that cobalt chloride catalyst prepares carbon nanotube

technical field

The invention relates to a chemical reaction method, in particular to a method for preparing carbon nanotubes using cobalt chloride as a catalyst and glucose as a raw material.

Background technique

Carbon nanomaterials are widely used in various technological and energy-related fields due to their excellent electronic properties and mechanical stability. In particular, carbon nanotubes are hailed as a rapidly rising star material due to the advantages that they can be regarded as rolled from graphitic carbon layers, have a one-dimensional lumen structure, and have lumen sizes ranging from one to several hundred nanometers, Therefore, it can be used as a nanoreactor or filled with other nanomaterials into the lumen to synthesize nanocomposites with novel properties, making it widely used in fuel cells, biological probes and chemical catalysis.

Generally, the preparation methods of carbon nanotubes mainly include arc discharge method, laser ablation method and chemical vapor deposition method. Although the carbon nanotubes prepared by arc discharge method and laser ablation method are very thin, both methods have certain limitations in controlling the length of carbon nanotubes and other unnecessary deposition by-products. Currently, the most widely used technique is chemical vapor deposition. Compared with arc discharge method and laser ablation method, chemical vapor deposition method can produce a large number of carbon nanotubes with controlled size and growth. However, for the above methods, in terms of the use of carbon sources, small molecular compounds that are easy to gasify are mainly used, such as benzene, acetylene, ethylene, and isopropanol. Therefore, it is necessary to find a simple, safe, controllable and low-cost method for synthesizing carbon nanotubes.

At present, biomass sources are extensive and renewable. If biomass raw materials can be directly prepared into carbon nanotubes and their composite nanocatalysts, it is of great significance in the synthesis of new materials and the development of new reaction processes.

In the application of the present invention, through the pyrolysis of glucose, melamine and cobalt chloride, a one-step synthesis of carbon nanotubes has been realized (see accompanying drawings 1 and 2)

Contents of the invention

Due to the complex process in the current synthesis process of carbon nanotubes, the need for expensive equipment, the high price of raw materials, and the unevenness of the prepared product; A simple method for preparing carbon nanotubes, the present invention is achieved through the following technical solutions:

The invention discloses a method for preparing carbon nanotubes using cobalt chloride as a catalyst and glucose as a raw material. The main raw materials used are glucose, melamine and cobalt chloride. The specific preparation steps are as follows:

1), glucose, melamine, cobalt chloride and distilled water are mixed and ground into a uniform mixture, the mass ratio of glucose, melamine and cobalt chloride is controlled to be 1:1:1, and the quality of distilled water is 1-2 times that of glucose, The above mixture was dried at 80°C for 12 hours to obtain a pink solid;

2), the above-mentioned pink solid is ground into powder and then transferred to a high-temperature tube furnace, heated to 700-800 degrees Celsius in flowing nitrogen, and maintained at 700-800 degrees Celsius for 4 hours to obtain a black solid;

3), the above-mentioned black solid substance is cooled to room temperature, transferred to a glass beaker, washed with HCl solution of 10% hydrochloric acid for 6 hours, controlling the quality of the hydrochloric acid solution to be 10-20 times that of the black solid;

4) After the above-mentioned solid matter washed with hydrochloric acid is suction-filtered with a microporous membrane, it is washed with distilled water until neutral, and the obtained solid matter is vacuum-dried at 50 degrees Celsius for 10 hours to obtain a carbon nanotube catalyst.

As a further improvement, the obtained carbon nanotubes described in the present invention have a length of 5-30 microns and a diameter of 200-300 nanometers.

As a further improvement, the glucose of the present invention is 3 grams, the melamine is 3 grams, the cobalt chloride is 3 grams; the distilled water is 5 milliliters.

The beneficial effects of the present invention are as follows:

The invention discloses a method for preparing carbon nanotubes. The carbon nanotubes use glucose, melamine and cobalt chloride as raw materials, and the length of the obtained nanotubes is 5-30 Micron, tube diameter of 200-300 nanometers, the preparation process of carbon nanotubes disclosed in the present invention has the advantages of simplicity, safety, low cost, easy operation and controllability.

Description of drawings

Fig. 1 is the scanning electron micrograph of the carbon nanotube that the present invention obtains;

Fig. 2 is a transmission electron microscope image of carbon nanotubes obtained in the present invention.

detailed description

Fig. 1 is the scanning electron micrograph of the carbon nanotube that the present invention obtains, in the electron micrograph after magnifying 5 thousand times, can observe clearly adopting the prepared carbon nanotube product of the present invention, these carbon nanotube lengths are in 5- 30 microns, uniform arrangement, diameter of about 200-300 nanometers.

Fig. 2 is a transmission electron microscope picture of the carbon nanotube obtained in the present invention, and in the electron microscope picture enlarged by 50,000 times, a single carbon nanotube and its internal contour can be clearly observed.

The technical scheme of the present invention will be further described below by specific examples:

Example 1

3 grams of glucose, 3 grams of melamine, 3 grams of cobalt chloride and 5 milliliters of distilled water were mixed and ground into a uniform mixture, and the above mixture was dried at 80 degrees Celsius for 12 hours to obtain a pink solid; after the above pink solid was ground into a powder Transfer to the high-temperature tube furnace, heat up to 700 degrees Celsius in flowing nitrogen, and maintain 700 degrees Celsius for 4 hours to obtain a black solid; the above-mentioned black solid is cooled to room temperature, transferred to a glass beaker, and 50 milliliters of HCl is added with a content of 10 % (mass percent) hydrochloric acid solution, stirred and dissolved for 6 hours; after the above-mentioned solid matter washed with hydrochloric acid was suction-filtered with a microporous membrane, washed to neutrality with 2000 milliliters of distilled water, and then rinsed with 50 milliliters of acetone, The obtained solid matter was vacuum-dried at 50° C. for 10 hours to obtain the product (about 1.72 g).

Example 2

3 grams of glucose, 3 grams of melamine, 3 grams of cobalt chloride and 5 milliliters of distilled water were mixed and ground into a uniform mixture, and the above mixture was dried at 80 degrees Celsius for 12 hours to obtain a pink solid; after the above pink solid was ground into a powder Transfer to the high-temperature tube furnace, heat up to 750 degrees Celsius in flowing nitrogen, and maintain 750 degrees Celsius for 4 hours to obtain a black solid; the above-mentioned black solid substance is cooled to room temperature, transferred to a glass beaker, and 50 milliliters of HCl is added with a content of 10 % (mass percent) hydrochloric acid solution, stirred and dissolved for 6 hours; after the above-mentioned solid matter washed with hydrochloric acid was suction-filtered with a microporous membrane, washed to neutrality with 2000 milliliters of distilled water, and then rinsed with 50 milliliters of acetone, The obtained solid matter was vacuum-dried at 50° C. for 10 hours to obtain the product (about 1.49 g).

Example 3

3 grams of glucose, 3 grams of melamine, 3 grams of cobalt chloride and 5 milliliters of distilled water were mixed and ground into a uniform mixture, and the above mixture was dried at 80 degrees Celsius for 12 hours to obtain a pink solid; after the above pink solid was ground into a powder Transfer to the high-temperature tube furnace, heat up to 800 degrees Celsius in flowing nitrogen, and maintain 800 degrees Celsius for 4 hours to obtain a black solid; the above-mentioned black solid substance is cooled to room temperature, transferred to a glass beaker, and 50 milliliters of HCl is added with a content of 10 % (mass percent) hydrochloric acid solution, stirred and dissolved for 6 hours; after the above-mentioned solid matter washed with hydrochloric acid was suction-filtered with a microporous membrane, washed to neutrality with 2000 milliliters of distilled water, and then rinsed with 50 milliliters of acetone, The obtained solid matter was vacuum-dried at 50° C. for 10 hours to obtain the product (about 1.23 g).

The above examples are only preferred implementations of the present invention, and the present invention is not limited to the above examples. Those skilled in the art can directly derive or associate other improvements and changes without departing from the spirit and concept of the present invention. It should be considered to be included in the protection scope of the present invention.

Claims (3)

1. a cobalt chloride catalyst prepares the preparation method of carbon nanotube, it is characterized in that, adopted main raw material is glucose, melamine and cobalt chloride, and concrete preparation steps are as follows: 1), glucose, melamine, cobalt chloride and distilled water are mixed and ground into a uniform mixture, the mass ratio of glucose, melamine and cobalt chloride is controlled to be 1:1:1, and the quality of distilled water is 1-2 times that of glucose, The above mixture was dried at 80°C for 12 hours to obtain a pink solid; 2), the above-mentioned pink solid is ground into powder and then transferred to a high-temperature tube furnace, heated to 700-800 degrees Celsius in flowing nitrogen, and maintained at 700-800 degrees Celsius for 4 hours to obtain a black solid; 3), the above-mentioned black solid substance is cooled to room temperature, transferred to a glass beaker, washed with HCl solution of 10% hydrochloric acid for 6 hours, controlling the quality of the hydrochloric acid solution to be 10-20 times that of the black solid; 4) After the above-mentioned solid matter washed with hydrochloric acid is suction-filtered with a microporous membrane, it is washed with distilled water until it is neutral, and the obtained solid matter is vacuum-dried at 50 degrees Celsius for 10 hours to obtain nitrogen-containing carbon nanotubes catalyst. 2. cobalt chloride catalyst according to claim 1 prepares the preparation method of carbon nanotube, is characterized in that, described obtained cobalt chloride catalyst prepares carbon nanotube length at 5-30 micron, pipe diameter at 200- 300 nm. 3. according to claim 1 and 2 described cobalt chloride catalysts prepare the preparation method of carbon nanotube, it is characterized in that, described glucose is 3 grams, melamine is 3 grams, and cobalt chloride is 3 grams; Distilled water is 5 grams. ml.