Method of modifying carbon nanotubes

FIELD: chemistry.

SUBSTANCE: invention can be used to obtain modified carbon nanotubes. The method of modifying carbon nanotubes includes treatment of carbon nanotubes with an aqueous solution of an oxidising agent in the form of a persulphate or hypochlorite solution at pH higher than 10, carried out simultaneously with mechanical treatment.

EFFECT: invention enables to obtain modified carbon nanotubes having good dispersability in water and in polar organic solvents with low consumption of reactants compared to known methods.

3 cl, 2 ex

 

The invention relates to the technology of carbon nanomaterials, particularly to a technology for production of modified carbon nanotubes.

Carbon nanotubes (CNTS) tend to form agglomerates, which complicates their distribution in different environments. Even if nanotubes uniformly distributed in some environments, for example, the intense action of ultrasound, after a short time they spontaneously form agglomerates. To obtain stable dispersions of carbon nanotubes using various methods of modification of carbon nanotubes, which are made by attaching to the surface of the CNTS those or other functional groups, ensuring the compatibility of CNTS with the environment, use of surfactants, shortening too long CNTS by various methods.

In the description of this invention the term "modification" means a change in the nature of the surface of the CNTS and the geometric parameters of individual nanotubes. A special case of the modification is the functionalization of CNTS consisting in grafting to the surface of the CNTS those or other functional groups.

The known method of the modification of CNTS, which involves the oxidation of carbon nanotubes under the influence of various liquid or gaseous oxidizing agents (nitric acid in the form of liquid or steam, hydrogen peroxide, solutions of ammonium persulfate in the ranks pH, ozone, nitrogen dioxide and others). In this way there is a lot of publications. However, since the essence of various methods of oxidation of carbon nanotubes is one and the same, namely the oxidation of the surface of carbon nanotubes with the formation of surface hydroxyl and carboxyl groups, this gives grounds to consider a variety of methods described as variants of the same method. As a typical example, the publication Datsyuk V., M. Kalyva, K. Papagelis, J. Parthenios, D. Tasis, Siokou A., I. Kallitsis, Galiotis C. Chemical oxidation of multiwalled carbon nanotubes //Carbon, 2008, vol.46, p.833-840, which describes several options (using nitric acid, hydrogen peroxide and ammonium persulfate).

Common essential features of the considered method and the claimed invention is the treatment of carbon nanotubes with a solution of an oxidant.

The discussed method is characterized by a lack of efficiency for the breakdown of agglomerates of CNTS and achieve good dispersive ability of the pigment oxidized CNTS in water and polar organic solvents. Typically, the oxidized known methods carbon nanotubes are well dispersed in water and polar organic solvents (under the action of ultrasound) only at very low concentration of nanotubes in a liquid (usually on the order of 0.001-0.05% mass). When exceeding the threshold concentration n is notrouble gather in large agglomerates (flakes) precipitated.

In some works, for example, Wang Y., Deng W., Liu X., Wang X. Electrochemical hydrogen storage properties of ball-milled multi-wall carbon nanotubes //International journal of hydrogen energy, 2009, vol.34, p.1437-1443; J. Lee, Jeong T., Heo J., Park S.-H., Lee, D., Park, J.-B., Han, H., Y. Kwon, I. Kovalev, S.M. Yoon, Choi J.-Y., Jin Y., Kirn J.M., An, K.H., Lee Y.H., Yu S. Short carbon nanotubes produced by cryogenic crushing //Carbon, 2006, vol.44, p.2984-2989; Konya, Z., J. Zhu, K. Niesz, D. Mehn, Kiricsi I. End morphology of ball milled carbon nanotubes //Carbon, 2004, vol.42, p.2001-2008, the described method of the modification of CNTS by shortening, which is achieved by prolonged mechanical processing of carbon nanotubes in liquids or in frozen matrices. Shortened CNTS have better dispersibility in liquids and the best electrochemical properties.

Common essential characteristics considered and the proposed methods is the machining of carbon nanotubes dispersed in any environment.

The disadvantage of the considered method is that it does not provide functionalization of CNTS polar groups, resulting processed in such a way CNTS is still not well dispersed in polar environments.

Closest to the claimed invention is a method described in Chiang Y.-C., Lin, W.-H., Chang Y.-C. The influence of treatment duration on multi-walled carbon nanotubes functionalized by H2SO4/HNO3 oxidation //Applied Surface Science, 2011, vol.257, p.2401-2410 (prototype). According to this method, the modification of CNTS is achieved by deep oxidation when cont is liteline boiling in aqueous solution, containing sulfuric and nitric acid. When this first happens grafting to the surface of the CNTS polar functional groups (in particular, carboxyl), and when a sufficiently long processing time is achieved by shortening of the nanotubes. At the same time there was also a decrease in the thickness of the nanotubes due to complete oxidation of surface carbon layer to carbon dioxide. Variants of this method are described in other sources, for example in the above-mentioned article V. Datsyuk, M. Kalyva, etc, and K.J. Ziegler, Z. Gu, H. Peng, Flor E.L., R.H. Hauge, R.E. Smalley Controlled oxidative cutting of single-walled carbon nanotubes //Journal of American Chemical Society, 2005, vol.127, issue 5, p.1541-1547. In the published sources noted that the shortened oxidized carbon nanotubes have improved dispersibility in water and in polar organic solvents.

General the essential feature of the proposed method and the prototype method is the handling of CNTS in an aqueous solution of oxidizer. The inventive method and prototype method are the same as on the achieved result, and it is achieved by grafting to the surface of the CNTS polar functional groups simultaneously with the truncation of long CNTS.

The disadvantages of the prototype method are the necessity of using a large excess of acid, which increases the process and creates environmental problems with disposal ododo is, as well as the oxidation of part of the carbon nanotubes to carbon dioxide, which reduces the yield of the final product (modified carbon nanotubes) and expensive. In addition, this method is difficult to scale. In laboratory conditions it is possible to use glass devices, however, for the pilot production of preferably stainless steel equipment. Boiling nanotubes in acid solution creates a problem of corrosion resistance equipment.

The basis of the claimed invention is the task by selecting oxidizing reagent and oxidizing conditions to eliminate the disadvantages of this method.

The problem is solved because, according to the method of modifying carbon nanotubes, including processing of carbon nanotubes with an aqueous solution of oxidizing agent, processing carbon nanotubes with an aqueous solution of oxidizing agent is conducted simultaneously with machining and as an oxidant solution using persulfate or sodium hypochlorite at pH greater than 10.

Machining is performed using a bead mill.

The oxidizer charge in an amount equivalent to from 0.1 to 1 g-atom of active oxygen per 1 g-atom of carbon nanotubes.

An excess of hypochlorite in the reaction mixture at a pH of more than 10 are removed by the addition of hydrogen peroxide.

Conducting education is otci carbon nanotubes with an aqueous solution of oxidizing agent simultaneously with machining and use as oxidant solution of persulfate or sodium hypochlorite at pH more than 10 provide the necessary exception use a large excess of acid, more expensive process and creating environmental problems with disposal of waste and loss of the finished product due to oxidation of a part of carbon nanotubes to carbon dioxide.

For machining can be used known in the art device, such as a bead mill, a vibration mill, ball mill, or other similar device. Practically bead mill is one of the most convenient devices to accomplish the task.

As oxidizers can be used ammonium persulfate, sodium persulfate, potassium persulfate, sodium hypochlorite, potassium hypochlorite. Most effectively the inventive method is carried out when processing carbon nanotubes with a solution of an oxidant at pH greater than 10. At lower pH the possible corrosion of equipment and improper decomposition of the oxidant with the release of chlorine (hypochlorite) or oxygen (persulfate). To establish the desired pH value by adding to the solution of a known substance having an alkaline reaction, such as ammonia, sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide and other alkaline substances which do not react under the conditions of the treatment with the oxidizing agent. This should take into account the known data that the hypochlorite react with ammonia. Thus, the system is IU with hypochlorite to apply ammonia cannot. When using persulfate to establish an alkaline pH you can use all of the listed substances.

For the implementation of the proposed method is optimal quantity of oxidant equivalent to from 0.1 to 1 g-atom of active oxygen per 1 g-atom of carbon nanotubes. When the amount of the oxidant is less than the specified lower limit, the resulting modified carbon nanotubes worse dispersed in water and polar organic solvents. The excess of the same amount of oxidant in excess of the upper limit is impractical because, although speeds up the process of oxidation of nanotubes does not improve the effect.

The following are data proving the possibility of implementing the claimed invention and its effectiveness.

For the implementation of the proposed method was applied the following source materials and equipment:

- Carbon nanotubes brands "Taunit" and Taunit-M production LLC Nanocenter", Tambov.

The ammonium persulfate grade analytical grade.

- Sodium hypochlorite according to GOST 11086-76 in the form of an aqueous solution containing 190 g/l of active chlorine and 12 g/l free sodium hydroxide.

- Ammonia 25%aqueous brands of analytical grade.

- Sodium carbonate anhydrous grade analytical grade.

- Distilled water.

- Dimethylacetamide grade analytical grade.

- Ethyl alcohol 96%.

The horizontal mill is the material of bead MSPM-1/0,05-BK-04 NPO "DESPOT". As the grinding media used balls made of Zirconia with a diameter of 1.6 mm

Ultrasonic installation of IL-10.

Example 1

4-liter capacity stainless steel poured 1460 ml of distilled water and dissolved 228,4 g of ammonium persulfate, and then added 460 ml of 25%aqueous ammonia. This solution has made a 1099 g water paste with carbon nanotubes Taunit-M (purified from mineral impurities by treatment with hydrochloric acid)containing 5.46 percent dry matter, and thoroughly mixed until a homogeneous suspension. The resulting suspension was loaded into a ball mill with balls with a diameter of 1.6 mm Zirconia and were processed within 7 hours. Then the treated suspension was unloaded, was filtered from the balls, was acidified with hydrochloric acid to acid reaction, was filtered through a filter of non-woven polypropylene material and washed with water until neutral wash water. The washed precipitate was sucked out into the vacuum and Packed up in a sealed plastic containers. Mass dry matter content (nanotubes) in the obtained paste was charged 8.52% (the rest is water). The resulting product was dried in a drying Cabinet at 80°C to constant weight.

Further modified carbon nanotubes obtained according to example 1 will be shown as UTM-1.

To test the solubility (dispersi is hemosta) a portion UTM-1 was dispersible in water or in organic solvents by ultrasonic treatment. Experiments have shown that UTM-1 well dissolved in water, preferably in the basic pH (generated by the addition of ammonia or organic bases). Additive Foundation promotes the formation of a stable solution (dispersion) of nanotubes, because it leads to ionization of surface carboxyl groups and the emergence of a negative charge on the nanotube.

Thus, there was obtained a stable aqueous solution (which can be seen in the transparency of the solution and no flakes), containing 0.5% UTM-1 in the presence of 0.5% triethanolamine as a pH regulator. The solubility of UTM-1 in this system is approximately 1%, above this concentration appear inclusion gel.

In dimethylacetamide (without other additives) sonification were obtained stable transparent solution UTM-1 with a mass concentration of 1 and 2%. In this case, dimethylacetamide, which in itself is a weak base, effectively dissolves UTM-1 without the addition of extraneous pH regulators. 1%solution was indefinitely stable when stored, 2%same after a few days began to show signs of thixotropy, but without the formation of agglomerates.

Example 2

4-liter capacity stainless steel poured 2,7 liters of distilled water, poured 397,5 g of anhydrous sodium carbonate and displaced ivali until dissolved. After dissolution of the sodium carbonate was poured a solution of sodium hypochlorite (0,280 l) and the mixture was thoroughly mixed. Then gradually with stirring gave 60 g of the crude Taunit-M (containing about 3% of the mass. the admixture of catalyst, preferably magnesium oxide) and stirred until a homogeneous suspension. This suspension was loaded into a ball mill with balls with a diameter of 1.6 mm Zirconia and were processed within 7 hours. Then the treated suspension was unloaded, was filtered from the balls, was acidified with hydrochloric acid to acid reaction and survived 3 days at room temperature for complete dissolution of the catalyst residues and possible impurities of iron compounds (from the chassis and fingers bead mill). Thus, at the same time spent acid cleaning nanotube impurities from the catalyst. Received an acidic suspension was filtered through a filter of non-woven polypropylene material and washed with water until neutral wash water. The washed precipitate was sucked out into the vacuum and Packed up in a sealed plastic containers. Mass dry matter content (nanotubes) in the obtained paste was 7,33% (the rest is water). The resulting product was dried in a drying Cabinet at 80°C to constant weight.

If the amount of hypochlorite in the reaction mixture with nanotubes excessive, it speeds up the t oxidation of the surface of the nanotubes, but creates an environmental problem, because the acidification of the mixture of unreacted hypochlorite allocates chlorine according to the reaction equation:

2NaOCl+2hcl→2NaCl+H2O+CL2

In order to neutralize the excess hypochlorite, to the reaction mixture at a pH of more than 10 add the hydrogen peroxide. As established by us, when this reaction occurs:

NaOCl+H2O2→NaCl+H2O+O2

The result is the formation of harmless products.

Further modified carbon nanotubes obtained according to example 2 will be denoted as OTM-2.

To test the solubility (dispersive ability of the pigment) hitch UTM-1 was dispersible in water or in organic solvents by ultrasonic treatment. Experiments have shown that UTM-1 well dissolved in water, preferably in the basic pH (generated by the addition of ammonia or triethanolamine). Additive Foundation promotes the formation of a stable solution (dispersion) of nanotubes, because it leads to ionization of surface carboxyl groups and the emergence of a negative charge on the nanotube.

Thus was obtained a stable aqueous solution (which can be seen in the transparency of the solution and no flakes), containing 0.5% UTM-1 in the presence of 0.5% triethanolamine as a pH regulator. The solubility of UTM-1 in this system, the e is approximately 1%, when exceeding this concentration appear to activate the gel.

In dimethylacetamide (without other additives) sonification were obtained stable transparent solution UTM-1 with a mass concentration of 1 and 2%. In this case, dimethylacetamide, which itself is the basis, effectively dissolves UTM-1 without the addition of extraneous controls pH, 1%solution was indefinitely stable when stored, 2%same after a few days began to show signs of thixotropy, but without the formation of agglomerates.

For comparison we have studied the solubility (under the action of ultrasound in the same conditions) in the same solvent of carbon nanotubes Taunit-M, oxidized according to the method specified in the method-prototype, a mixture of nitric and sulphuric acids without mechanical processing. Experiments have shown that carbon nanotubes oxidized by an excess of nitric acid without mechanical processing, have the same solubility as obtained according to the claimed invention. However, the inventive method can easily be scaled, no problems with corrosion resistance equipment and environmental problems with waste neutralization. The process of mechanochemical processing according to the present method proceeds at room temperature. The way the prototype requires such great is th excess nitric and sulfuric acids, what scaling it and ensuring environmental security is very problematic.

These data confirm the effectiveness of the proposed method for production of modified CNTS. It does not apply aggressive acid solutions, as in the method prototype, and the loss of carbon nanotubes by oxidation to carbon dioxide (carbonate in alkaline solution) is virtually absent.

Thus, the inventive method allows to obtain a modified carbon nanotubes having a good dispersibility in water and polar organic solvents, can be easily scaled, provides ecological safety.

1. Method of modifying carbon nanotubes, including processing of carbon nanotubes with an aqueous solution of oxidizing agent, characterized in that the processing carbon nanotubes with an aqueous solution of oxidizing agent is conducted simultaneously with machining, and as oxidant solution using persulfate or sodium hypochlorite at a pH of more than 10, and the oxidizer charge in an amount equivalent to from 0.1 to 1 g-atom of active oxygen per 1 g-atom of carbon nanotubes.

2. The method according to claim 1, characterized in that the machining is performed using a bead mill.

3. The method according to claim 1, characterized in that an excess of hypochlorite in the enjoyment of the operating mixture at a pH of more than 10 are removed by the addition of hydrogen peroxide.



 

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1 dwg

FIELD: carbon materials.

SUBSTANCE: weighed quantity of diamonds with average particle size 4 nm are placed into press mold and compacted into tablet. Tablet is then placed into vacuum chamber as target. The latter is evacuated and after introduction of cushion gas, target is cooled to -100оС and kept until its mass increases by a factor of 2-4. Direct voltage is then applied to electrodes of vacuum chamber and target is exposed to pulse laser emission with power providing heating of particles not higher than 900оС. Atomized target material form microfibers between electrodes. In order to reduce fragility of microfibers, vapors of nonionic-type polymer, e.g. polyvinyl alcohol, polyvinylbutyral or polyacrylamide, are added into chamber to pressure 10-2 to 10-4 gauge atm immediately after laser irradiation. Resulting microfibers have diamond structure and content of non-diamond phase therein does not exceed 6.22%.

EFFECT: increased proportion of diamond structure in product and increased its storage stability.

2 cl

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