Method for cleaning nano-diamonds

FIELD: inorganic chemistry, possible use in bio-medical research and during manufacture of non-magnetic materials, sorbents.

SUBSTANCE: in accordance to the method, industrial mixture of diamond with graphite and metals is processed by mixture of acids and oxidizing compounds. The suspension is additionally processed by cleaned concentrated hydrochloric acid with concentration of nano-diamonds in the hydrochloric acid not exceeding two percents with simultaneous ultrasound processing. Temperature of suspension is measured. Then temperature increases by at least ten degrees, irradiation is stopped. Suspension is settled. Aforementioned operations are repeated at least three times. Then suspension is washed by cleaned concentrated hydrochloric acid until coloration disappears and thiocyanate sample reaction becomes positive. Final washing is performed by deionized water until suspension stops settling.

EFFECT: resulting nano-diamonds do not contain admixtures of iron.

4 ex

 

The invention relates to the field of physico-chemical processing of inorganic materials, specifically to the field of purification of nanodiamonds at the stage of processing, and can be used for the removal of iron oxides ultradispersed diamonds produced by detonation synthesis of explosives.

Ultra-dispersed diamonds (UDD) is the aggregate of crystals of carbon with a diamond lattice with an average crystal size of about 4 nm, i.e. are nanodiamonds. Distinguish them from the technical product obtained from the detonation chamber, called detonation carbon. It contains (30÷70)% UDA, Almazny carbon and inorganic impurities, particularly iron oxides, significantly affecting the magnetic properties of UDD due to ferromagnetism, which does not allow to use the UDA in the industry as magnetochiral material. Thus, the main task is to clean UDA not only from carbon impurities, but also from oxides of iron.

Known purification method UDA (Journal of applied chemistry, t, VIP, 1992, s-2516), including the effects on detonation carbon with an aqueous solution of hydrogen peroxide with the addition of bases, salts, acids at high pressure and temperature. The most effective was found to be nitric acid.

The method gives moznosti substantially clear UDA from non-diamond carbon, however, it is not possible to effectively remove impurities of metals and oxides, such as oxides of iron.

The known method (CN patent No. 1385366) purification of nanodiamonds synthesized by detonation method, by treatment of the resulting product, containing diamonds, concentrated sulfuric acid, in combination with potassium permanganate and subsequent heating of the oxidant and detonation of carbon-containing nanodiamonds. When this occurs the reaction between graphite, other impurities and oxidant and the result is purified water suspension of nanodiamonds.

The method is technologically simple, but the resulting product contains a significant amount of metal oxides and insoluble sulfates.

A known way to clean diamonds, is applicable to purification of nanodiamonds (JP patent No. 63303806)adopted for the prototype, in order to increase the efficiency of cleaning of diamonds at the stage of processing the mixture or aggregates of diamond, graphite and metal catalyst obtained by the process of graphite as the starting material and metal catalyst under high pressure at high temperature by the usual process (called NMT), is treated with a mixture of acids and oxidizing agents (for example, a mixture of sulfuric acid and chromic anhydride), and in combination with this use of ultrasonic waves. When synthesized static what Ecodom crystals in the first stage are subjected to oxidation treatment as a method of removal of unreacted graphite, along with this use and sonication, for example 20000 kHz resonant frequency and 200 watts of power (normally applied to the generator of ultrasonic vibrations). The metal catalyst is treated with acid in combination with ultrasonic irradiation. Through these above two treatments graphite adhering to the surface of the diamond, and recrystallized graphite metal-catalyst sprayed and removed in a short time using the method of separation in heavy liquids, using the difference in densities, followed by rinsing with clean water and protecting.

The disadvantage of this method is that if it is used for processing raw detonation of carbon, oxides of iron, present as impurities, only partially dissolved, the iron content is reduced, but not enough for the product was magneticity.

The present invention solves the problem of increasing the efficiency of purification of nanodiamonds from oxides of iron.

The problem is solved by the method of purification of nanodiamonds, including the processing of industrial mixtures of diamond from graphite and metals with a mixture of acids and oxidants, ultrasonic impact on the resulting suspension of nanodiamonds, rinse it with water and decanting, when ultrasonic treatment is carried out after the aforementioned processing the mixture of acids and oxidizing agents and washing obtained by oxidation of a suspension of nanodiamonds, at the same time further treated suspension treated with concentrated hydrochloric acid at a concentration of nanodiamonds in hydrochloric acid not more than two percent, while measuring the temperature of the suspension and stopping the irradiation with increasing temperature at least ten degrees, defend suspension, repeat the above operations at least three times, after which the suspension was washed with purified concentrated hydrochloric acid until the colour disappears and the positive response to the test with thiocyanate, and then conduct a final rinse using deionized water until the termination of sedimentation of suspensions.

The authors found that the oxides of iron, which is an admixture formed under the influence of a shock wave in the process of detonation synthesis ULTRADISPERSED diamonds, pass in a dense form, dissolution and peptidase which is unacceptably slow for industrial cycle and incomplete, and found that for the complete dissolution of dense oxides requires the combined use of hydrochloric acid for peptization and chemical dissolution of oxides and ultrasonic irradiation for cavitation crushing particles of oxides, without which peptidase does not leak. The set of operations, materials and modes necessary for complete removal of dense iron oxides from industrial UDA, provide the future can create magnetotactic materials, expressed in the essential characteristics of the method meet the criteria of the invention.

Purified concentrated hydrochloric acid is used because of its ability to particiapate iron oxides, including in dense forms, whereas other acids dissolve their only chemically. It is required that the concentration of the UDA (nanodiamonds) in hydrochloric acid was not more than 2%, as the authors experimentally found that in this case there is sufficient mixing of suspensions by ultrasound, and if the concentration is larger, then the suspension will be too viscous for good mixing. Ultrasonic irradiation provides cavitation crushing impurities, which dramatically accelerates the process of dissolution-peptization. Temperature increases in proportion to the absorbed dose. When this temperature difference (increase of not less than 10 degrees), as determined by the authors, provided the necessary cleaning UDA dose. The upper limit of temperature rise, in principle, is not significant, however, when a large increase its suspension can boil and spray. It is experimentally shown that the repetition of the operations not less than three times is necessary and sufficient to achieve a high degree of purification from iron oxides. The suspension is washed with purified concentrated Sol is Noah acid until the colour disappears and the positive response to the test with thiocyanate, as this is a sign of reaching a high degree of purification from iron oxides. The use of deionized water when washing is required in order to avoid the adsorption of iron impurities which are always present in industrial water.

The method is as follows. As the source material used for the detonation of the carbon is treated with an oxidising agent in acidic medium and washed with water. The resulting aqueous suspension of nanodiamonds (UDD), also containing impurities of iron compounds (typically 0.1÷10%), mixed with a concentrated aqueous solution of HCl (e.g., 40%) with an iron content of <1·10-6so the resulting suspension UDA in hydrochloric acid has a concentration of not more than 2%. The mixture is subjected to ultrasonic irradiation (frequency of 20-25 kHz is the usual frequency of sources of ultrasound). Exposure occurs when a continuous measurement of the temperature of the mixture, and when the temperature of the mixture will increase by at least 10 degrees, the irradiation is stopped. The mixture defend (usually within 12-24 hours) to lighten the liquid and then clarified the upper part of the merge. Operation, since the effect of the hydrochloric acid with the simultaneous effect of ultrasound, repeat at least 3 times. After that, the UDD suspension was washed with hydrochloric acid (preferably in the same ratios). Washing is the lead until while the clarified liquid is not specific yellow-brown colour of iron salts, and the clarified acid will not give a negative reaction on rhodanate sample (test for such a reaction is known from the technical literature). After washing the suspension with hydrochloric acid to produce the rinsing deionized water. After cessation of sedimentation of suspensions leaching ceased.

Example 1.

Sample UDA (detonation nanodiamond) was obtained from detonation of carbon content UDA 60% and iron oxide 4% and were purified from non-diamond carbon with nitric acid under pressure. After primary treatment, the content of iron oxides was 1.0%. Then 500 ml of water suspension SHOCK with a concentration of dry UDA 5,0% was mixed with 2000 ml of concentrated hydrochloric acid brand OFS in a glass beaker (the concentration of the UDA was 1%). The glass top was lowered irradiator magnetostrictive type, to which was connected to an ultrasonic generator with electric output power of 300 W and a frequency of about 22 kHz. The exposure time was 30 min, the temperature rose 10 degrees (which corresponds to the absorbed acoustic dose of 40 j/ml). After the termination of the acoustic impact of the suspension was defended within 12 hours. The volume of the upper clarified layer was 80% of the total. This with the Oh was painted in the characteristic solutions of iron salts in hydrochloric acid a yellow-brown color. The clarified layer was decanted. The process of ultrasonic treatment with concentrated hydrochloric acid was repeated three times, after which the irradiated suspension was washed with concentrated hydrochloric acid OFS brands in the same ratio of 6 times. Washing was discontinued after the disappearance of the color of the upper defend layer and the disappearance of the positive qualitative tests for ammonium thiocyanate. Rinse the cleaned suspension SHOCK from the remnants of hydrochloric acid was carried out by mixing - by decantation with deionized water at a ratio of 1:10. The washing process was repeated until the termination of sedimentation of suspensions (4 times). Formed a stable suspension with a pH of 3.0 and a concentration of 0.5 wt.%. The completeness of the removal of iron was produced by the method of electron paramagnetic resonance (EPR) isolated from a suspension of solid UDA. The absence of iron impurities was confirmed by measurements of the EPR spectrum and gravimetric determination of residue after burning (received less than the threshold sensitivity of this method).

Example 2.

The cleaning process was carried out analogously to example 1, however, for washing was taken in 1000 ml of concentrated hydrochloric acid, the concentration of the UDA was 2.5%. In this case, when the irradiation there was no complete mixing of the suspension UDA. By the EPR method in the final product was found approx the camping iron.

Example 3.

The cleaning process was carried out analogously to example 1, however, the irradiation of the suspension was continued for 15 minutes, raise the temperature was 5 degrees, which corresponds to the absorbed acoustic radiation dose of about 20 j/ml by the EPR Method in the final product was detected admixture of iron.

Example 4.

The cleaning process was carried out analogously to example 1, however, the irradiation of the suspension was continued for 3 hours, the temperature increase was 45 degrees, there was a boiling suspension with the release of part of the suspension from a glass. Received UDA was of high quality, but its output has decreased due to the loss of part of the suspension.

Thus, the proposed method allows to obtain magneticity nanodiamonds, which can be used, for example, in scientific research, the production of non-magnetic materials, sorbents, in biomedical applications.

The purification method of nanodiamonds, including the processing of industrial mixtures of diamond from graphite and metals with a mixture of acids and oxidants, ultrasonic impact on the resulting suspension of nanodiamonds, rinse it with water and sedimentation, characterized in that the ultrasonic treatment is carried out after the above-mentioned processing the mixture of acids and oxidizing agents and washing obtained by oxidation of a suspension of nanodiamonds, simultaneity is b further treated suspension treated with concentrated hydrochloric acid at a concentration of nanodiamonds in hydrochloric acid not more than two percent, measuring the temperature of the suspension and stopping the exposure when the temperature is not less than 10°, defend suspension, repeat the above operations at least three times, after which the suspension was washed with purified concentrated hydrochloric acid until the colour disappears and the positive response to the test with thiocyanate, and then conduct a final rinse using deionized water until the termination of sedimentation of suspensions.



 

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1 tbl, 2 ex

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1 ex

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7 cl, 1 tbl, 4 ex

Cavitation reactor // 2290990

FIELD: chemical engineering.

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5 dwg

Cavitation reactor // 2286205

FIELD: chemical industry; food processing industry; pharmaceutical industry; perfumery industry; power industry; medical equipment industry; devices for action on the liquids by the energy of the acoustic field of cavitation.

SUBSTANCE: the invention is pertaining to the apparatuses for action on the liquid by the energy of the acoustic field of cavitation formed by the elastic harmonic oscillations of the liquid of the ultrasonic frequency with the purpose of creation in them of the thermodynamically non-equilibrium states. The invention can be used in the chemical, alimentary, pharmaceutical and perfumery industry, and also in medicine and energetics. The reactor contains the sources of the harmonic oscillations made in the form of the resonators of the similar frequency, inside which the liquid oscillations form the elastic standing waves. The phases of the resonators are shifted for the advance as their distance from the center of the reactor is varying. Realization of the invention allows to increase the maximum value of the density of the potential energy of the cavitation without changing neither the volume of the reactor, nor the hydrostatic pressure inside it and without changes of the volumetric density of the sound power of the harmonic frequencies.

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2 cl, 6 dwg

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3 cl, 1 dwg

FIELD: chemical industry; mining; food industry; pharmaceutical and perfumery industry.

SUBSTANCE: the invention is dealt with the field of the hypersonic cavitational desintegration of liquid mediums and may be used in food, chemical, ore mining, pharmaceutical and perfumery industries. The method provides, that a liquid flow is passing through a resonant cell of the cavitational reactor, where in the liquid is formed a stagnant acoustic wave with the given average value of a volumetric density of the power causing generation of a cavitation in it in the form of one or several stationary cavitational zones. Density of the potential energy evolving for a period of the acoustic wave, in any point of perimeter of any cross-section of the liquid flow inside the reactor is set not exceeding its peak value on the walls of the resonant cell. The reactor contains a resonant cell, a body, a diaphragm with an aperture placed in a plane parallel to the oscillation shifts of the resonant cell walls. Coordinates of points of the perimeter of the minimum area of the cross-section of the reactor in the plane parallel to oscillating shifts of the walls of the resonant cell, are determined by an equation. The technical result is an increase of dispersion, homogeneity, intensifications of reactions, synthesis of new compounds and increase of their activity.

EFFECT: the invention ensures increased dispersion, homogeneity, intensifications of reactions, synthesis of new compounds and an increase of their activity.

2 cl, 7 dwg

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