TWI421210B - Method to separate the carbon nanotubes by jelly fig pectin - Google Patents

Description

Method for dispersing carbon nanotubes with natural love jade pectin

The invention relates to a method for dispersing a carbon nanotube by natural jade pectin, in particular to using a unique jadely pectin of Taiwan, which has low surface tension and high viscosity. Used in the dispersion of carbon nanotubes.

Because of its unique structure, the carbon nanotubes have excellent mechanical, thermal, physical, chemical and high aspect ratio characteristics, making them extremely versatile. However, because of the weak van der Waals force between the carbon nanotubes, they are easy to gather together and are insoluble in water or organic solvents, which causes the carbon nanotubes to not perform optimally in use, thus dispersing the nanoparticles. Carbon tubes will be a key technology in the application of carbon nanotubes. According to the traditional technology of dispersing carbon nanotubes, chemical surfactants and organic solvents are generally used. However, the chemical materials used in the process are toxic, which not only causes personal injury, but also causes serious damage. Environmental pollution. For example, the prior art patent application technology has the patent application No. 20071194 of the Republic of China, which mainly utilizes a functionalized carbon nanotube having a hydrophilic substance bonded in a covalent manner, and the carbon nanotubes are added to the polar solvent. In the aqueous solution, the carbon nanotubes are dispersed in the aqueous solution, but the polar solvents used in the dispersion process are both toxic and cause environmental pollution. Furthermore, the Patent No. I258789 of the Republic of China patent uses a water-based solvent to add a solute such as a dispersant, a stabilizer, a film former and a tackifier, and a carbon nanotube in which a base solvent and a solute are formed. The low-viscosity aqueous solution, the carbon nanotubes are suspended therein to form a carbon nanotube suspension, and the solvent used in the dispersion process is an organic solvent, which may also cause environmental pollution. In addition, at present, the patents of the Republic of China patents, the publications No. I258789 and No. I284116, and the publications of the patents No. 200700312 and No. 200710029, etc., have no patents for the use of natural jade pectin as a dispersant. And standard methods for dispersing single-walled carbon nanotubes. Obviously, the present invention is the latest dispersing carbon nanotube technology, and does not cause harm to personnel and environmental pollution.

In view of the shortcomings of the existing carbon nanotube dispersion technology, the present inventors have actively invested in research based on rich knowledge and experience, and have developed the present invention which is progressive and industrially usable. The non-toxic natural plant love jade pectin used in the present invention is a unique agricultural product in Taiwan, and the jade jelly is a popular summer drink in Taiwan, and its main component is the peel of the achene achenes. (pericarp) high esterification degree pectin dissolved by pectin ester endogenous pectin esterase (PE) to produce low esterification degree pectin, and then with divalent cations in water such as: calcium The magnesium plasma forms a bridge and is connected into a mesh structure to form a glue. Since the inventors have observed that the jade pectin has low surface tension and high viscosity, after the pectin is dissolved, after ultrasonic vibration, it can help the jade pectin enter the end of the wall of the single-walled carbon nanotube. And the surface, and adsorbed on the surface of the single-walled carbon nanotubes, resulting in a decrease in the van der Waals force between the single-walled carbon nanotubes, effectively dispersing the single-walled carbon nanotubes to avoid the agglomeration phenomenon.

The main object of the present invention is to provide a manufacturing method which is easy to manufacture and non-polluting, and can effectively disperse a carbon nanotube in an aqueous solution to fully exert the performance of the carbon nanotube. Its technical content, especially the use of Taiwan's unique jadely pectin as a material, has low surface tension and high viscosity, can be effectively applied to the dispersion of carbon nanotubes, and is dispersed by ultrasonic vibration. Treatment, further reducing the Van der Waals force between the carbon tubes. The specific technical means includes preparation of raw materials, dispersion treatment, filtration treatment and drying treatment. Preparing the raw materials includes preparing a predetermined amount of single-walled carbon nanotubes and a predetermined amount of purified jade pectin. Preparing a predetermined amount of single-walled carbon nanotubes, including purification and modification: placing the single-walled carbon nanotubes in a sulfuric acid/nitric acid solution for a predetermined period of ultrasonic oscillation; filtering separation: shaking up The solution is separated from the sulfuric acid/nitric acid solution by filtration; neutralization treatment: the sulfuric acid/nitric acid solution remaining on the single-walled carbon nanotube is washed away with deionized water until The pH of the single-walled carbon nanotube is maintained at neutral; and the drying treatment: the neutralized single-walled carbon nanotube is baked at a predetermined temperature and for a predetermined time to remove the steam. Preparing a predetermined amount of purified Aiguo pectin, including dilution treatment: taking a predetermined amount of purified Aiyu pectin diluted with deionized water; and stirring: stirring for a predetermined time to make the love jade fruit The gum is uniformly dissolved in the deionized water to form an aqueous solution of jade pectin. Dispersion treatment: the prepared single-walled carbon nanotubes are added to the prepared aqueous solution of Ai Jade Pectin, and ultrasonic waves are shaken for a predetermined time to uniformly disperse the single-walled carbon nanotubes in the aqueous solution of Aiyu Pectin. . Filtration treatment: the excess jade pectin and deionized water in the aqueous solution of the jade pectin are filtered by a suction filter device. Drying treatment: the remaining single-walled carbon nanotubes are baked at a predetermined temperature for a predetermined time to remove excess moisture, and the single-walled carbon nanotubes after dispersion treatment are obtained.

one. Basic technical features of the present invention

As shown in FIG. 1 , the method for dispersing a carbon nanotube in natural jade pectin of the present invention comprises:

(a) Preparing raw materials, including:

(a1) preparing a predetermined amount of single-walled carbon nanotubes; and

(a2) Preparing a predetermined amount of purified Ai Pectin comprising:

(b) Dispersing treatment: then adding an appropriate amount of purified and modified single-walled carbon nanotubes to the aqueous solution of Ai Jade Pectin, so that the single-walled carbon nanotubes are uniformly dispersed in the aqueous solution of Aiyu Pectin;

(c) Filtration treatment: filtering out excess jade pectin by using a suction filter device;

(d) Drying treatment: Finally, the remaining single-walled carbon nanotubes are baked in a vacuum oven to obtain a single-walled carbon nanotube after dispersion treatment.

two. Experimental example of the present invention

As shown in FIG. 1 , the method for dispersing a carbon nanotube in natural jade pectin of the present invention comprises:

(a) Preparing raw materials, including:

(a1) Preparing a predetermined amount of single-walled carbon nanotubes, including:

(a11) Purification and modification: Since the single-walled carbon nanotubes themselves have impurities, the single-walled carbon nanotubes must be purified and modified, that is, the single-walled carbon nanotubes are first placed in a volume ratio of 3:1. Ultrasonic vibration in a sulfuric acid/nitric acid solution (98% sulfuric acid, 70% nitric acid) (please refer to Appendix 1), the oscillation time is 1 hour;

(a12) Filtration separation: separating the shock-washed solution into a single-walled carbon nanotube and a sulfuric acid/nitric acid solution by filtration;

(a13) Neutralization treatment: then the sulfuric acid/nitric acid solution remaining on the single-walled carbon nanotubes is washed away with deionized water until the pH of the single-walled carbon nanotubes is maintained at neutral (pH is about 7);

(a14) drying treatment: the neutralized single-walled carbon nanotubes are then baked in a vacuum oven at about 100 ° C for about 24 hours to remove moisture from them;

(a2) Preparing a predetermined amount of purified Ai Pectin comprising:

(a21) Dilution treatment: weighing a predetermined amount of purified Aiyu pectin diluted with deionized water;

(a22) stirring: stirring with a magnet mixer for about 1 hour, so that the jade pectin can be uniformly dissolved in deionized water;

(b) Decentralized treatment: Then, an appropriate amount of purified and modified single-walled carbon nanotubes were added to the aqueous solution of Aiyu Pectin, and the single-walled carbon nanotubes were uniformly dispersed in Aiyuguo by ultrasonic vibration for about 1 hour. In the aqueous solution of glue;

(c) Filtration treatment: filtering excess jade pectin and deionized water by means of a suction filtering device;

(d) Drying treatment: Finally, the remaining single-walled carbon nanotubes were baked in a vacuum oven at about 100 ° C for about 24 hours to remove excess moisture, thereby obtaining a dispersed single-walled carbon nanotube.

Participation. Experimental analysis of the present invention

The present invention utilizes a transmission electron microscope analysis which can be used as a tool for judging the distribution of single-walled carbon nanotubes. Figure 1 (a) of Annex II shows the structure of single-walled carbon nanotubes before they are treated with Aiyu Pectin. The overall diameter range is widely distributed. It can be seen that the single-walled carbon nanotubes have poor dispersion. It has the phenomenon of entanglement and agglomeration, which causes the carbon nanotubes to not play the best role in use. Figure 1 (b) of Annex II shows the TEM photograph of the evidence for the existence of agglomerated single-walled carbon nanotubes in a separate form by ultrasonic vibration dispersion and a mixture of jade pectin.

In the experimental example of the present invention, it is proved that the single-walled carbon nanotubes can effectively reduce the van der Waals force between the carbon nanotubes and improve the agglomeration phenomenon through the ultrasonic vibration and the double dispersion of the jade pectin. Figure 3 (a) of Annex III shows the case where the single-walled carbon nanotubes are only oscillated by ultrasonic waves for 1 hour in an aqueous solution and left at room temperature for 2 hours. It is apparent from the photograph that the underlying single-walled carbon nanotubes are entangled and entangled with each other, causing agglomeration and precipitation to cause delamination. The purified single-walled carbon nanotubes were added to the aqueous solution of the jade pectin dispersion under the same conditions and subjected to ultrasonic vibration for 1 hour, and left at room temperature for more than 6 months, as shown in Figure 3 (b) of Annex III. A black suspension that remains stable and evenly dispersed remains.

The above is only one of the possible embodiments of the present invention, and is not intended to limit the scope of the patents of the present invention, and the equivalent implementations of other changes according to the contents, features and spirits of the following claims are It should be included in the scope of this creation patent. In addition to the above advantages, this creation has deep industrial applicability, can effectively improve the lack of use, and is specifically defined in the characteristics of the request item, not found in similar items, so it is practical and progressive, and has been in line with the new type. For patents, the application shall be filed in accordance with the law. The Bureau shall be required to approve the patent in accordance with the law to protect the lawful rights and interests of the applicant.

(a). . . Preparing raw materials

(a1). . . Prepare a predetermined amount of single-walled carbon nanotubes

(a11). . . Purification and upgrading

(a12). . . Filter separation

(a13). . . Neutralization

(a14). . . Drying treatment

(a2). . . Prepare a predetermined amount of purified Ai Pectin

(a21). . . Dilution treatment

(a22). . . Stir

(b). . . Decentralized treatment

(c). . . Filter processing

(d). . . Drying treatment

Figure 1 is a schematic flow chart of the present invention.

Annex I: Figure of the experimental device of the present invention.

Annex II:

Figure 1 (a) is a single-walled carbon nanotube treated without jade pectin; and

Fig. 1(b) shows a single-walled carbon nanotube under the ultrasonic vibration dispersion and the jade pectin coating.

Annex III:

1(a) is a single-walled carbon nanotube aqueous solution purified by ultrasonic vibration treatment for 1 hour, and is placed at room temperature for more than 6 months; and

Fig. 1(b) shows the addition of jade pectin in the present invention, which is subjected to ultrasonic vibration for 1 hour and left at room temperature for more than 6 months.

(a). . . Preparing raw materials

(a1). . . Prepare a predetermined amount of single-walled carbon nanotubes

(a11). . . Purification and upgrading

(a12). . . Filter separation

(a13). . . Neutralization

(a14). . . Drying treatment

(a2). . . Prepare a predetermined amount of purified Ai Pectin

(a21). . . Dilution treatment

(a22). . . Stir

(b). . . Decentralized processing

(c). . . Filter processing

(d). . . Drying treatment

Claims (6)

A method for dispersing a carbon nanotube in natural jade pectin comprises: (a) preparing a raw material comprising: (a1) preparing a predetermined amount of single-walled carbon nanotubes, further comprising the steps of: purifying Modification: the single-walled carbon nanotube is placed in a sulfuric acid/nitric acid solution for ultrasonic vibration for a predetermined period of time; filtration separation: the shock-washed solution is filtered to the single-walled carbon nanotube with the sulfuric acid /Nitric acid solution separation; neutralization treatment: the sulfuric acid/nitric acid solution remaining on the single-walled carbon nanotubes is washed away with deionized water until the pH of the single-walled carbon nanotubes is maintained at neutral; a first drying process: the neutralized single-walled carbon nanotubes are baked at a predetermined temperature and for a predetermined time to remove moisture from the water; and (a2) a predetermined amount is prepared Purified jade pectin, which further comprises the following steps: dilution treatment: diluting the purified jade pectin with deionized water; and stirring, stirring for a predetermined time to uniformly dissolve the jade pectin in the deionized In water, to form an aqueous solution of jade pectin; (b) dispersing treatment: the single-walled naphthalene will be prepared The carbon nanotubes are added to the prepared aqueous solution of the jade pectin, and the single-walled carbon nanotubes are uniformly dispersed in the aqueous solution of the jade pectin, and the single-walled carbon nanotubes are added to the aqueous solution of the jade pectin. The ultrasonic wave is oscillated for a predetermined time, so that the single-walled carbon nanotubes are uniformly dispersed in the aqueous solution of the jade pectin; (c) the filtration treatment: the excess jade pectin in the aqueous solution of the jade pectin is filtered by using a suction filtering device; And (d) second drying treatment: drying the remaining single-walled carbon nanotubes at a predetermined temperature Bake for a predetermined time to remove excess moisture to obtain the single-walled carbon nanotubes after dispersion treatment. The method of claim 1, wherein the volume ratio of sulfuric acid to nitric acid in the sulfuric acid/nitric acid solution is 3:1, the predetermined The time is 1 hour. The method of claim 1, wherein the first drying treatment step is to place the single-walled carbon nanotube in a vacuum oven for baking. The predetermined temperature was 100 ° C, and the predetermined time was 24 hours. A method of dispersing a carbon nanotube by natural jade pectin according to claim 1, wherein the stirring step is performed by a magnet mixer for a predetermined time of 1 hour. The method of claim 1, wherein the predetermined time in the dispersing treatment step is 1 hour. The method for dispersing a carbon nanotube by natural jade pectin according to claim 1, wherein in the second drying step, the single-walled carbon nanotube is baked in a vacuum oven. The predetermined temperature is 100 ° C, and the predetermined time is 24 hours.