Method of processing detonation carbon (versions)

FIELD: chemistry.

SUBSTANCE: invention relates to modification of properties of superhard materials and can be used in synthesis highly pure ultradisperse diamonds. Detonation carbon is processed in supercritical water or in supercritical water with addition of hydrogen peroxide.

EFFECT: modification of surface of nanoparticles of condensed carbon phase containing ultradisperse diamonds, removal and decomposition of non-diamond carbon structures, environmentally safe non-waste technology.

2 cl, 2 dwg, 2 ex


The invention relates to the field of modification of properties of superhard materials, namely spraying detonation of carbon (charge detonation of carbon-containing ultrafine nanodiamonds)obtained by the method of detonation synthesis in the explosion of the solid carbon-containing explosives with negative oxygen balance, and may find application in the preparation of ultra-dispersed diamond of high purity.

Studies of carbon nanostructures in the development of new nanotechnologies recently given much attention. Among the various synthesized carbon structures should be allocated so-called ultra dispersed nanodiamonds (UDA)obtained by the method of detonation synthesis with the detonation of the solid carbon-containing explosives [Aiyin, Ehapter, A.P. Ershov, Gavranovic, Ametuer, V.m.titov. Dokl. Academy of Sciences, 1988. 302, 611]. Despite the high performance of this method we obtain the product of detonation soot or carbon contains various patterns and forms of carbon, including the content of the diamond phase is only 35-45 wt.%. Moreover, depending on the production technology [O.A.Shenderova V.V.Zhirnov D.W.Brenner. Carbon nanostructures. In Critical Reviews in Solid State and Materials Sciences. 2002. 27. 3/4 / P.227-356; Woodyates. Ultradisperse diamonds of detonation synthesis: properties and application. The success khimii, 70, 7. 687-708]in detonation soot may contain adsorbed impurities in the form of metals, oxides and carbides.

To highlight the diamond phase or UDA initial charge, usually liquid or gaseous oxidants. As a liquid oxidant is a mixture of sulfuric and nitric acids, sulfuric and chromic anhydride [Woodlots. Ultradisperse diamonds of detonation synthesis: properties and application. The USP. 2001, 70, 7. 687-708]. Oxygen and ozone are also used as gaseous thermocycles. In practice, the most used method of treatment of the mixture with concentrated nitric acid under temperature and pressure conditions in the autoclave at high pressure and temperature. This method allows to oxidize Almazny carbon and remove metals, their oxides and some other impurities. Purified by this method, the powder may contain up to 90-97 wt.% various forms of nanodiamonds and 3-10 wt.% non-diamond carbon and other impurities.

The main disadvantages of the known methods of chemical and mechanical cleaning using strong acids and oxidizers should include the allocation of a large number of aggressive waste, as well as oxidation of the diamond phase.

There is a method of removal of non-diamond carbon [of the Russian Federation No. 2132816, C01B 31/06, B01J 3/04, 10.07.99], in which the cleaning almasoud Rasa mixture is held when it is heated to a temperature of 320-400°C with potassium nitrate for 30 minutes The disadvantage of this approach is the presence in the treated sample of potassium oxide (melting point of which 740°C), which is the product of the decomposition of potassium nitrate.

There is a method of allocation of ultradispersed diamonds, we adopted for the prototype [of the Russian Federation No. 2109683, C01B 31/06, 27.04.1998], in which cleaning of the diamond-containing mixture from various impurities and the allocation of ultradispersed diamonds is carried out in the two-stage treatment with an aqueous solution of nitric acid at high temperatures and pressures.

To the main disadvantage of the prototype should include the use of strong acids and, as a consequence, the presence of hazardous waste in the form of acids.

The present invention solves the problem of efficient removal of non-diamond phase of carbon and process of detonation of carbon without the use and formation of harmful, toxic compounds and substances.

The technical result - surface modification of the nanoparticles condensed carbon phase containing ultrafine diamonds, removal and decomposition of non-diamond carbon structures, creating an environmentally friendly waste-free technology.

The problem is solved in two variants of the method of processing the detonation of carbon.

In the first embodiment processing detonation of carbon is carried out in supercritical water (SLE).

The second option clicks the processing detonation of carbon is carried out in supercritical water (SLE) with the addition of hydrogen peroxide.

Many of the substances in supercritical conditions are effective reaction medium for various chemical transformations and show unusual properties, which allows for variations of temperature, pressure and residence time at high speed to carry out chemical reactions. Among supercritical solvents most attention of researchers is water (RRC=22 MPa, Tcrit≈374°C) due to the fact that supercritical water - SLE is a multi-component medium consisting of a weakly interacting polar molecules H2O and nanoparticles condensed phase neutral and charged clusters (H2O)nH+(H2O)i, OH-(H2O)j. Properties of a supercritical fluid water depend on density, temperature, composition and concentration of impurities, and can change when an external impact, for example, force fields, hydrodynamic perturbations. The dissociation constant of water near the critical point in three times more constants for water in its normal state and, thus, near the critical point has a large concentration of ions H3O+and OH-than water in its normal or subcritical conditions. Therefore, the water in this state can show properties of acid and basic catalysis. But, should it is to emphasize, such properties are preserved only near the critical point. Among the chemical reactions carried out in GFR, the most practical use today are oxidation reactions carried out in supercritical water.

The invention is illustrated by the following examples.

Example 1. Processing of samples detonation of carbon in supercritical water.

In the reactor-autoclave with a volume of 45 cm3with electric heating and stirring was placed a sample of the mixture with water and heated with stirring until the temperature of the experiment 390°C (+/-5), pressure - 285(+/-5) ATM. After setting the temperature and pressure corresponding to the water transfer in the supercritical state, the process continues from 4 to 6 hours, After cooling the reactor to measure the pressure and gas volume of the reaction products, the latter increases as compared with the initial 1.5-2 times, indicating that the oxidation of carbon-containing phase. About

80% vol. the resulting gas is CO2in addition, in the reaction products observed some amount of CO, CH4H2. There is loss of mass of the initial charge, which indicates substantial oxidation of the carbon content of the mixture during the process in SLE.

Studies of the solid phase before and after treatment in SLE carried out by electron (HRTEM), (SEM) mi is rescobie, method of x-ray phase analysis (XRD). Using chromatography to analyze the composition of the resulting gaseous reaction products, measure their volume.

The results of x-ray phase analysis

The analysis of diffraction spectra processed in SLE samples shows that the ratio of the integral intensities of the peaks (ID/IGfor this type of processing depends on the process time and increases from the initial value to a value of 0.8 1.1-1.3.

The results of HRTEM analysis.

Figure 1 shows the HRTEM images of detonation of carbon after treatment in SLE. Comparison shots of the charge of the original sample detonation of carbon with the images obtained after processing in supercritical water (Figure 1), showing a significant difference of the latter. First, it significantly decreased the amount of amorphous phase of carbon, secondly, the increased concentration of carbon cubic modification.

Example 2. Processing of samples detonation of carbon in supercritical water in the presence of hydrogen peroxide.

In the reactor-autoclave with a volume of 45 cm3place the sample mixture with water and heated with stirring to a temperature of 300°C, then using a syringe pump is introduced into the reactor under a pressure of 30% aqueous hydrogen peroxide solution in an amount to provide the stoichiometric autochangecolor, formed in the decomposition of hydrogen peroxide (one mol H2O2- 0.5 mole of O2), with non-diamond carbon contained in the original sample mixture.

After the establishment of the stationary temperature 390°C (+/-5) and pressure -285(+/-5) ATM the process continues from 4 to 6 o'clock Processed in SLE in the presence of oxygen formed by the decomposition of hydrogen peroxide, the sample detonation of carbon changes the color from black to grey. Volume of gas evolved taking into account unreacted oxygen exceeds more than 8 times the initial free volume of the reactor.

The results of x-ray phase analysis.

The relationship of the integral intensities processed in SLE in the presence of oxygen samples detonation of carbon vary considerably in the direction of increasing the share of diamond and equal for samples ID/IG=1.35-1.86, which corresponds to 65-75 wt.% diamond phase.

The results of HRTEM analysis.

Figure 2 presents HRTEM images detonation of carbon after treatment in SLE in the presence of the decomposition products of hydrogen peroxide. Analysis of HRTEM images of samples detonation of carbon after it is processed in supercritical water with the participation of the decomposition products of hydrogen peroxide showed, first, a high degree of purification. 2, secondly, the practical absence of amorphous phase angle is ode and of a carbon onion structure and thirdly, the size of the diamond core is not changed, i.e. the diamond phase is not oxidized.

The examples demonstrate that the most significant transformation of the non-diamond phase of carbon is observed when processing the mixture in SLE containing the decomposition products of hydrogen peroxide. Found that when processing the detonation of carbon in supercritical aqueous solvents, oxidation of the diamond core.

As can be seen from the text and examples, the invention solves the problem of surface modification of nanoparticles condensed carbon phase containing ultrafine diamonds, removal and decomposition of non-diamond structures, creation of environmentally friendly waste-free technology.

1. The processing method of detonation of carbon, characterized in that the processing is carried out in supercritical water.

2. The processing method of detonation of carbon, characterized in that the processing is carried out in supercritical water with the addition of hydrogen peroxide.


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25 cl, 6 ex, 2 dwg