Method for hydroconversion of heavy oil fractions

FIELD: chemistry.

SUBSTANCE: invention relates to a method for hydroconversion of heavy oil fractions - feed stock, the method including a zero step and subsequent N steps. The zero step includes feeding, into a reactor, material, a catalyst precursor - aqueous solution of a Mo (VI) salt or salts of Mo and Ni, and hydrogen at pressure of 4-9 MPa under normal conditions; reacting the material and hydrogen at 420-450°C in the presence of a precursor of a suspended nanosize molybdenum or molybdenum-nickel catalyst formed in the reactor; atmospheric or atmospheric-vacuum distillation of the hydrogenation product; removing the low-boiling fraction with a boiling point not higher than 500°C as a product and returning the high-boiling fraction or part thereof into the reactor. The next steps include feeding, into the reactor, material, a catalyst precursor, the returned part of the high-boiling fraction and hydrogen; reaction thereof; said atmospheric distillation of the hydrogenation product; removing the low-boiling fraction as a product; returning part of the high-boiling fraction into the reactor; burning at 1000-1300°C or gasification of the remaining part of the high-boiling fraction, after which trapped ash-slag residues are subjected to further oxidising burning at 800-900°C and the obtained ash product, which is carbon-free, is used to regenerate the catalyst precursor and produce an industrial concentrate of vanadium and nickel. The number of steps N is determined using formulae: b d ( n n + n m + 1 ) = a + i = 1 n m b i + b e n m , N=nn+nm+1, where nn is the number of steps with recirculation, after which equilibrium output of the low-boiling fractions is achieved; nm is the number of steps with recirculation after achieving equilibrium output of the low-boiling fractions, which enables to achieve a given output of low-boiling fractions from the feed stock; bd is the given output of low-boiling fractions, wt %; a is the output of low-boiling fractions at the zero step, wt %; bi is the output of low-boiling fractions at the i-th step before achieving equilibrium, wt %; be is the output of low-boiling fractions after achieving equilibrium, wt %, be>bd.

EFFECT: high output of low-boiling fractions, low molybdenum consumption, high degree of extraction of molybdenum, vanadium and nickel from the solution, enabling calculation of the required reactor volume, obtaining an industrial concentrate of vanadium and nickel, low hydrogen consumption.

3 cl, 1 dwg, 2 tbl, 2 ex

 

The present invention relates to the field of refining heavy oil fractions obtained by atmospheric or vacuum distillation of crude oil or heavy hydrocarbon natural raw materials to produce low-boiling petroleum fractions (with BP. ≤500°C) used for production of motor fuels, and high-boiling fractions (b. p. >500°C) used for combustion with the production of electricity, heat, hydrogen, industrial concentrates vanadium and Nickel.

A method of processing heavy oil-containing raw material containing mainly the fraction with a boiling point above 204°C, the hydro conversion in a distillation column reactor. In the process of hydroconversion simultaneously specified distillation of crude oil and hydrocracking in the presence of a catalyst of hydroconversion. In the process of hydrocracking is cleaned from sulphur and metals. In the hydrocracking process using several types of solid catalysts: for hydrodemetallization, for cracking and for the capture of asphaltenes and solids. The process temperature is 204-649°C (see RF patent №2173696, publ. 23.09.99, CL C10G 47/02).

This method cannot be effectively used for the raw material with a boiling point fractions above 538°C, because the method does not provide high levels of conversion and extraction of low-boiling light �of Ricci and, moreover, requires a high temperature.

The closest analogue (prototype) of the proposed invention is a method of hydroconversion heavy fractions of oil (high-boiling residues of processing oils), as described in the patent 2146274 (from 10.03. 2000, bull. No. 7, Skibicka N. And. etc.). According to this patent the high-boiling residues of oils or other high molecular raw material is subjected to hydrogenation (hydroconversion) with a uniform distribution in the feedstock catalyst with a particle size of 0.02-0.3 μm, obtained directly in the reaction zone of the emulsion formed by mixing the feedstock with an aqueous solution containing a salt of molybdenum acid, such as ammonium paramolybdate, and ammonia, taken in a weight ratio of ammonia: molybdenum, 0.15 to 0.39:1, and drops having a diameter of 0.3-5 μm. The formed organic compounds with a boiling point below 350°C is distilled off. The residue with a boiling point above 350°C is burned completely or partially at 800-1000°C and from ash residues recovered catalyst in the form of ammonium paramolybdate, which are recycled in the process as well as rare and noble metals contained in the feedstock (including vanadium). Part of the high-boiling fraction is recycled in the process and mixed with a new portion of raw materials.

The disadvantages of the prototype zaklyuchayut� the following:

- not enough high yield of low-boiling fractions with BP. ≤350°C and 58.2-70,8% wt. - due to the lack of calculating the number of stages of recycling the high-boiling fractions necessary for the achievement of the desired outputs (≥90%) boiling fractions;

the inability to calculate the volume of the reactor required for the conduct of the process;

- insufficient reducing the consumption of molybdenum by recycling the high-boiling fraction and the regeneration of the precursor from ash particles formed during combustion of high-boiling fractions;

- low yield of the precursor of the catalyst from ash particles (8,45 g Mo on 147,3 g ash residue).

Object of the invention is to increase the yield of low-boiling fractions, to reduce the consumption of molybdenum, to increase the output of the precursor of the high-boiling fractions, to provide the industrial concentrate vanadium and Nickel and the ability to calculate the volume of the reactor required for the conduct of the process.

The solution of this problem is achieved by a method of hydroconversion heavy fractions of crude oil feedstock, comprising feeding to the reactor feedstock, the catalyst precursor-containing aqueous salt solution of Mo (VI) and hydrogen, the reaction of the raw material and hydrogen in the presence of formed in the reactor from the precursor suspended nanosized molybdenum or molybdate-rolled Nickel�lit, distillation of the hydrogenation, the output of the low-boiling fraction as a product, the return of some of the high-boiling fraction CCF to the stage of flow in the reactor, raw materials, precursor of the catalyst is fresh and regenerated and hydrogen, the heat treatment of the rest of the CCF with getting ash residues, which are used for regeneration of the catalyst precursor and the extraction of metals, which consists of zero stage comprising feeding to the reactor feedstock, the catalyst precursor is an aqueous salt solution of Mo (VI) or salts of Mo and Ni, and hydrogen at a pressure of 4 to 9 MPa under normal conditions, the reaction of the feedstock and hydrogen at 420-450°C in the presence formed in the reactor from the precursor suspended nanosized molybdenum molybdate or Nickel catalyst, then atmospheric or atmospheric and vacuum distillation of the hydrogenation, the output of the low-boiling fraction with a boiling point of not higher than 500°C both the product and the return of the CCF or its part on the stage of flow in the reactor, raw materials, precursor of the catalyst is fresh and regenerated and hydrogen, the next N stages comprising feeding to the reactor feedstock, catalyst precursor, returned part of the CCF with the previous stage and hydrogen, the reaction in these conditions, atmospheric or atmospheric and vacuum distillation of the hydrogenation, the output of the low-boiling fraction with temperature�Roy boiling point not higher than 500°C of the product the return part of the CCF to the stage of flow in the reactor, raw materials, precursor of the catalyst is fresh and regenerated and hydrogen, burning at a temperature of 1000-1300°C or gasification of the rest of the CCF, and then caught ash residues subjected to further oxidative firing at 800-900°C and the obtained ash product not containing carbon is used for the regeneration of the catalyst precursor and production of concentrate vanadium and Nickel, and the number of stages N is determined by the formulas:

where nn- the number of stages with recirculation, after which equilibrium is reached the output NKF; nm- the number of stages with recirculation after reaching equilibrium output NKF, ensuring the achievement of specified output of the low-boiling fractions from a feedstock; bd- preset output low-boiling fractions from a feedstock, wt%; and the yield of low-boiling fractions at the zero stage, % wt.; b - the output of the low-boiling fractions at the first stage before reaching equilibrium, wt.%, be- the output of the low-boiling fractions after reaching equilibrium, wt.%, be>bd.

As a heavy petroleum fractions use the balance of atmospheric or atmospheric and vacuum distillation of crude oil.

Additional roasting these ash residues�s is carried out when the percentage of excess air α=1,4-1,5, the resulting gaseous products together with ash and slag residues cooled to a temperature of 200°C or below and catch it in the filter from aplodan, ash obtained product is treated for 1-1. 5 hours water-ammonia solution containing 10-15 wt%. NH3and 4-6 wt%. (NH4)2CO3at a temperature of 50-60°C, filtering the resulting suspension to obtain a solution - regenerated catalyst precursor and the solid residue - industrial concentrate vanadium and Nickel.

Fig.1 shows a block diagram of the process according to the invention. Under this scheme carry out dispersion in the raw precursor of the catalyst (an aqueous solution of ammonium paramolybdate, molybdenum content of 20-25 g/l) or a mixture of this solution with an aqueous solution of Nickel salt at a ratio of Mo/Ni is at least 4:1 with a ratio of raw material/precursor (95-98)/(5-2); hydroforming (reaction hydroconversion) mixture at 420-450°C and in an atmosphere of hydrogen (4 to 9 MPa under normal conditions) in the presence of a catalyst MoS2formed in the reaction zone from the precursor, subsequent atmospheric or atmospheric and vacuum distillation of the hydrogenation of obtaining low-boiling (BP. not higher than 500°C) and high-boiling (BP. above 500°C) fractions of hydrocarbons and a part of the high-boiling fractions of the hydro conversion with a new one then�Oia as a raw material recycle. The remainder of the high-boiling fractions is subjected to combustion in industrial conditions, for the removal of solid particles from gaseous products of combustion after they have additional oxidizing roasting and cooling. Captured solids are subjected to hydrometallurgical processing of obtaining industrial concentrate vanadium, Nickel and molybdenum precursor molybdate or Nickel catalyst.

The technical result of the invention is increasing the yield of low-boiling fractions; reducing the consumption of molybdenum by conducting the process in the form of cycles, each of which includes several stages of recirculation of part of the high-boiling fractions; increasing the degree of extraction of molybdenum, vanadium and Nickel from the solution due to the additional oxidizing roasting of collected particulate matter (ASW) after combustion of the high-boiling fractions; the ability to predict the number of stages to reach equilibrium mode providing an output to the desired level of conversion, which also allows you to calculate the volume of the reactor required for the conduct of the process; the possibility of obtaining industrial concentrate vanadium and Nickel; the ability to reduce hydrogen consumption.

Example 1.

To 1 kg of sludge (residue atmospheric and vacuum distillation of crude oil) was added to 500 mg of Mo in the form of a 20 ml aqueous solution� - (NH4)2MoO4with a molybdenum content of 25 g/l. Conduct the hydro conversion of the 0 - phase at an initial partial pressure of H2- 7 MPa and t=445°C, the duration of the hydrogenation reaction at each stage - 30 minutes Simultaneously in the reaction mixture is formed nanosized catalyst - MoS2with particle sizes between 50 and 800 nm. Products hydroconversion subjected to atmospheric and then vacuum distillation (atmospheric and vacuum distillation) of the standard installations. Get 500 g of low-boiling fraction with a boiling point of ≤500°C and 500 g of high-boiling fraction with a boiling point of >500°C. the Amount of molybdenum in high-boiling fraction is ~499 mg. the Amount of vanadium and Nickel is about 235 and 40 mg, respectively. In the low-boiling fractions: Mo<0.2 mg or <0,04% wt.; V<0.1 mg or<0,04% wt.; Ni<0.1 mg or <a 0.25% wt.

From the high-boiling fraction is taken 20 grams, which is sent for incineration, and 480 g mixed with 1 kg of sludge and 240 mg Mo in the form of 9.6 ml of an aqueous solution of (NH4)2MoO4with a molybdenum content of 25 g/L. the Mixture was subjected to hydroconversion under the conditions described above. After hydroconversion conduct atmospheric and then vacuum distillation, receive 740 g of fraction with boiling point ≤500°C and 740 g of fraction with a boiling point of >500°C. Specified average degree of hydroconversion (preset output low boiling fracc�th of feedstock) for the entire cycle is 90% output of the low-boiling fraction. On the table.1 shows that the equilibrium of the process is achieved at the 7th stage, including zero, on which the conversion rate is 96%. By the relations (1) and (2) the number of stages in the cycle to achieve an average degree of conversion of 90% must be equal to 14, including 0 - stage. After the completion of the cycle, the amount of high-boiling fraction formed after stage 14, is sent for incineration. The outputs of the NKF to achieve equilibrium and the distribution of Mo, V and Ni, including the number that is returned in hydroconversion shown in table.1. The amount of Mo in the reactor necessary for the implementation process to achieve the degree of conversion of 90% for the entire cycle (14 stages, including 0-th stage), is 1.435 G. If not implemented recirculation, flow Mo would have amounted to 7 g (0,05%* 14 kg). Therefore, the implementation of the recirculated air is reduced Mo about the 5.56 g in the processing of 14 kg of sludge. Just after burning CCF in ASW at a temperature of 1200°C are formed 1.43 g Mo, and 3,36 g V, and 0.56 g of Ni. The number of ASW is 12.7 g taking into account the losses. For regeneration of the solution of the precursor and producing a concentrate vanadium and Nickel 12,7 g ASW process 63,5 ml of an aqueous solution (10% NH3and 5% (NN4)2CO3) at 60°C for 1 h. the Solution is filtered, the filter cake washed with water. Passes into solution of 1.21 g of Mo, i.e. the content �th in solution, representing the amount of filtrate and wash water is 19.2 g/l Mo. The resulting solution is mixed with a fresh solution of ammonium paramolybdate. The flow rate of fresh solution of ammonium paramolybdate (molybdenum), necessary for hydroconversion 14 kg of sludge, is 0.22 g Mo 14 kg of sludge or 15.7 g per 1 ton of sludge. The dry mass of the residue on the filter is 9, the Number of molybdenum, vanadium and Nickel, calculated as oxides, are 0,319; 4,2 and 0.64 g or 3,54; 46,7 and 7.1 wt%. respectively. The residue after leaching of ash and slag is an industrial concentrate vanadium and Nickel with a mixture of molybdenum.

Consequently, the average consumption of molybdenum is 15.7 g/t of sludge.

Table 1
An example of processing of the sludge in the recirculation mode rest of hydroconversion (partial pressure of H2- 7 MPa; t=445°C and the duration of the hydrogenation reaction at each stage - 30 min)
IndicatorsThe number of the stage recycling
012345 678
The number of recycled mixture of raw materials, kg11.481.711.8551.891.9071.9161.921.922
The number of NKF, kg0.50.740.8550.9280.9450.9540.9580.960.96
The degree of conversion of feedstock (output NKF), % wt.507485.592.894.595.495.89696
The number of generated CCF, kg0.50.740.8550.9280.9450.954 0.9580.960.96
The number of return of recycle to the next stage, kg0.480.710.820.890.9070.9160.920.9220.922
The amount of Mo in the reactor, mg500740855928945954958960960
The number of Mo returned with a fresh solution of the precursor mg5002601451075447424040
The number of Mo returned with resicom mg480710821891 907916920922922

Example 2.

To 1 kg of fuel oil (residue from atmospheric distillation of crude oil) was added to 500 mg of Mo in the form of a 20 ml aqueous solution of (NH4)2MoO4with a molybdenum content of 25 g/l. Conduct the hydro conversion of the 0 - phase partial pressure of H2- 7 MPa; t - 445°C, the duration of the hydrogenation reaction at each stage - 30 minutes Simultaneously in the reaction mixture formed from the precursor nanoscale catalyst - MoS2with particle sizes between 50 and 800 nm. Products hydroconversion subjected to atmospheric and vacuum distillation in a laboratory setting. Get 600 g of fraction with boiling point ≤500°C and 400 g of high-boiling fraction with a boiling point of >500°C. the Amount of molybdenum in high-boiling fraction is ~498 mg. the Amount of vanadium and Nickel in high-boiling fractions, respectively - about 279 and 47 mg low boiling fractions: Mo<0.2 mg or <0,04% wt.; V<0.1 mg or <0,04% wt.; Ni<0.1 mg or <0.2% wt.

From the high-boiling fraction is taken 30 g, which is sent for incineration, and 370 g mixed with 1 kg of fuel oil and 223 mg Mo in the form of 8.9 ml of aqueous solution of (NH4)2MoO4with a molybdenum content of 25 g/L. the Mixture was subjected to hydroconversion under the conditions described above. After hydroconversion about�odat atmospheric distillation, get 822 g of fraction with boiling point ≤500°C and 548 g of fraction with a boiling point of >500°C. Given the average degree of conversion of feedstock for the entire cycle is 90%. On the table.2 shows that the equilibrium process is achieved at the 6th stage, including zero, at which the degree of conversion of feedstock is 96%. By the relations (1) and (2) the number of stages in the cycle to achieve an average degree of conversion of raw materials 90% must be equal to 11, including 0 - stage. After the completion of the cycle, the amount of high-boiling fraction formed after stage 11, sent for incineration. The outputs of the NKF to achieve equilibrium and the distribution of Mo, V and Ni, including the number that is returned in hydroconversion shown in table.2. The amount of Mo in the reactor necessary for the implementation process to achieve the degree of conversion of the feedstock is 90% for the entire cycle (11 stages, including the 0-th stage), is 1.35 g. If did not carry out recycling, the consumption of Mo would have amounted to 5.5 g (0,05%*11 kg). Consequently, the implementation of recirculated air mode allows you to cut about 4,15 g Mo in the processing of 11 kg of fuel oil. Just after burning CCF in ASW at a temperature of 1200°C are formed 1.35 g Mo, and is 3.08 g V and 0.52 g of Ni. The number of ASW is 11 g taking into account losses. For regeneration of the solution of the precursor and producing a concentrate vanadium and Nickel 11 g ASW obrabatyvat ml of an aqueous solution (10% NH 3and 5% (NH4)2CO3) at 60°C for 1 h. the Solution is filtered, the filter cake washed with water. Passes into solution of 1.15 g of Mo, i.e. its content in the solution, representing the amount of filtrate and wash water will amount to 21.3 g/l Mo. The resulting solution is mixed with a fresh solution of ammonium paramolybdate. The flow rate of fresh solution of ammonium paramolybdate (molybdenum), necessary for hydroconversion 11 kg of fuel oil, is 0.2 g Mo 11 kg of fuel oil or 18.2 g per 1 ton of fuel oil. The dry mass of the residue on the filter is 7.5, the Content of molybdenum, vanadium and Nickel, calculated as oxides, is 0.2; and 3,85 0.59 g or 2.7; 51,3 and 7.9 wt%. respectively. The residue after leaching of ash and slag is an industrial concentrate vanadium and Nickel with a mixture of molybdenum.

Consequently, the average consumption of molybdenum at 18.2 g/t of fuel oil.

Table 2
An example of processing of heavy fuel oil high-viscosity oil in recirculation mode (at a pressure of N2- 7 MPa; t=445°C and the duration of the hydrogenation reaction at each stage - 30 min)
IndicatorsThe number of the stage recycling
01234567
The number of recycled mixture of raw materials, kg11.371.5071.5581.5761.5831.5861.586
The number of NKF, kg0.60.8220.9040.9350.9460.950.9520.952
The degree of conversion of feedstock (output NKF), % wt.6082.290.493.594.69595.295.2
The number of generated CCF, kg0.40.5480.6030.623 0.630.6330.6340.634
The number of return of recycle to the next stage, kg0.370.5070.5580.5760.5830.5860.5860.586
The amount of Mo in the reactor, mg500685754779788792793793
The number of Mo returned with a fresh solution of the precursor mg500223120826862.56060
The number of Mo returned with resicom mg462634697720729733 734734

The implementation of the process heat from the combustion of the high-boiling fraction can be disposed of. If high-boiling fraction is subjected to gasification, the main indicators of the process will not change, but additionally will produce hydrogen, which can be used in the process of hydroconversion. This will reduce the flow rate used in the process of hydrogen.

When using as a precursor an aqueous solution of salts of Mo and Ni, in particular, ammonium paramolybdate and emmakate Nickel at a weight ratio of molybdenum to Nickel of not less than 3, the resulting catalyst consists of sulfides of molybdenum and Nickel. The application of this molybdate-Nickel catalyst get results similar to the results obtained when applying the molybdenum catalyst.

1. Method of hydroconversion heavy fractions of crude oil feedstock, comprising feeding to the reactor feedstock, the catalyst precursor-containing aqueous salt solution of Mo (VI) and hydrogen, the reaction of the raw material and hydrogen in the presence of formed in the reactor from the precursor suspended nanosized molybdenum molybdate or Nickel catalyst, distillation of the hydrogenation, the output of the low-boiling fraction as a product, the return of some of the high-boiling fraction CCF on the stage of the innings� in the reactor, raw materials, the precursor of the catalyst is fresh and regenerated and hydrogen, the heat treatment of the rest of the CCF with getting ash residues, which are used for regeneration of the catalyst precursor and the extraction of metals, characterized in that the method consists of zero stage comprising feeding to the reactor feedstock, the catalyst precursor is an aqueous salt solution of Mo (VI) or salts of Mo and Ni, and hydrogen at a pressure of 4 to 9 MPa under normal conditions, the reaction of the feedstock and hydrogen at 420-450°C in the presence formed in the reactor from the precursor suspended nanosized molybdenum molybdate or Nickel catalyst, then atmospheric or atmospheric and vacuum distillation of the hydrogenation, the output of the low-boiling fraction with a boiling point of not higher than 500°C both the product and the return of the CCF or its part on the stage of flow in the reactor, raw materials, precursor of the catalyst is fresh and regenerated and hydrogen, the next N stages comprising feeding to the reactor feedstock, catalyst precursor, returned part of the CCF with the previous stage and hydrogen, the reaction under these conditions, atmospheric or atmospheric and vacuum distillation of the hydrogenation, the output of the low-boiling fraction with a boiling point of not higher than 500°C of the product the return part of the CCF to the stage of flow in the reactor, raw materials, precursor of the catalyst - CBE�it and regenerated - and hydrogen, burning at a temperature of 1000-1300°C or gasification of the rest of the CCF, and then caught ash residues subjected to further oxidative firing at 800-900°C and the obtained ash product not containing carbon is used for the regeneration of the catalyst precursor and production of concentrate vanadium and Nickel, and the number of stages N is determined by the formula:
bd(nn+nm+1)=a+i=1nmbi+benm
N=nn+nm+1,
where nn- the number of stages with recirculation, after which equilibrium is reached the output NKF; nm- the number of stages with recirculation after reaching equilibrium output NKF, ensuring the achievement of specified output of the low-boiling fractions from a feedstock; bd- preset output low-boiling fractions, wt.%; and - the output of the low-boiling fractions at the zero stage, % wt.; bi- the output of the low-boiling fractions at the first stage to achieve balance, % wt.; be- the output of the low-boiling CHF�of CCI after reaching equilibrium, wt.%, be>bd.

2. A method according to claim 1, characterized in that the heavy fractions of oil use the balance of atmospheric or atmospheric and vacuum distillation of crude oil.

3. A method according to claim 1 or 2, characterized in that the additional firing of these ash residues is carried out at the rate of excess air α=1,4-1,5 formed gaseous products together with ash and slag residues cooled to a temperature of 200°C or below and catch it in the filter from aplodan, ash obtained product is treated for 1-1. 5 hours water-ammonia solution containing 10-15 wt%. NH3and 4-6 wt%. (NH4)2CO3at a temperature of 50-60°C, filtering the resulting suspension to obtain a solution - regenerated catalyst precursor and the solid residue - industrial concentrate vanadium and Nickel.



 

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3 cl, 22 tbl, 16 ex

FIELD: oil and gas industry.

SUBSTANCE: invention refers to oil-processing and petrochemical industries and can be used to increase the processing depth of hydrocarbon-containing raw material. The invention refers to the processing method of hydrocarbon-containing raw material using metal nanoparticles and includes its separation into fractions so that light hydrocarbon fractions and residual fraction is obtained; at that, before the stage of separation into fractions, either metal organic salt having formula M(OOC-R)n, or M(SOC-R)n or M(SSC-R)n is introduced, where R means alkyl, aryl, isoalkyl, tert-alkyl, alkylaryl, which possibly includes hydroxylic, keto-, amino-, carboxyl, thiocarbamic group, N - 1-3, and M means transition metal from elements of the Periodic table, at the decomposition of which there obtained are metal nanoparticles, or nanoparticles of those metals based on 0.001-0.1 wt % of metal per mass of raw material; at that, at least some portion of residual fraction is supplied by recycling to the stage of separation into fractions after being mixed with raw material. The invention also refers to versions of the method.

EFFECT: higher quality and extraction degree of light hydrocarbons of up to 95%.

16 cl, 5 dwg, 9 tbl, 10 ex

FIELD: metallurgy.

SUBSTANCE: method involves the following steps at which: initial material is processed into the ash containing the metals subject to regeneration, which have been chosen from the metals including vanadium, metals of group 8-10 and metals of group 6; the above ash is leached by leaching solution so that the first solid substance is obtained, which contains metals of group 8-10, solid carbonaceous material and supernatant fluid containing vanadium and metal of group 6; supernatant fluid is mixed with solution of ammonia sulphate and the deposit containing vanadium and additional fluid containing metal of group 6 is obtained; additional supernatant fluid is mixed with leaching solution, solution of ammonia sulphate and solution of sulphuric acid and the deposit containing metal of group 6 is obtained.

EFFECT: methods are effective for regeneration of metals without formation of other undesirable by-products.

10 cl, 9 dwg, 12 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention can be used in obtaining coatings, reducing coefficient of secondary electronic emission, growing diamond films and glasses, elements, absorbing solar radiation. Colloidal solution of nano-sized carbon is obtained by supply of organic liquid - ethanol, into chamber with electrodes, injection of inert gas into inter-electrode space, formation of high-temperature plasma channel in gas bubbles, containing vapours of organic liquid. High-temperature plasma channel has the following parameters: temperature of heavy particles 4000-5000K, temperature of electrons 1.0-1.5 eV, concentration of charged particles (2-3)·1017 cm3, diameter of plasma channel hundreds of microns. After that, fast cooling within several microseconds is performed.

EFFECT: simplicity, possibility to obtain nanoparticles of different types.

3 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to field of nanotechnologies and can be used for obtaining composite materials with high electric and heat conductivity, additives to concretes and ceramics, sorbents, catalysts. Carbon-containing material is evaporated in volume thermal plasma and condensed on target surface 9 and internal surface of collector 7. Plasma generator 3, which includes coaxially located electrodes: rod cathode 4 and nozzle-shaped output anode 5, are used. Gaseous carbon-containing material 6 is supplied with plasma-forming gas through vortex chamber with channels 2 and selected from the group, consisting of methane, propane, and butane. Bottom of collector is made with hole 8 for gas flow to pass.

EFFECT: invention makes it possible to reduce energy consumption of the process, extend types of applied hydrocarbon raw material, simplify device construction and provide continuity of the process and its high productivity.

2 dwg, 3 ex

FIELD: chemistry.

SUBSTANCE: method of obtaining a composite material includes the influence on a mixture of a carbon-containing material, filler and sulphur-containing compound by a pressure of 0.1-20 GPa and a temperature of 600-2000°C. As the sulphur-containing compound applied is carbon bisulphide, a compound from the mercaptan group or a product of its interaction with elementary sulphur. As the carbon-containing material applied is molecular fullerene C60 or fullerene-containing soot. As the filler applied are carbon fibres, or diamond, or nitrides, or carbides, or borides, or oxides in the quantity from 1 to 99 wt % of the weight of the carbon-containing material.

EFFECT: obtained composite material can be applied for manufacturing products with the characteristic size of 1-100 cm and is characterised by high strength, low density, solidity not less than 10 GPa and high heat resistance in the air.

11 cl, 3 dwg, 11 ex

FIELD: chemistry.

SUBSTANCE: invention relates to inorganic chemistry, namely to obtaining silicon-carbide materials and products, and can be applied as thermal-protective, chemically and erosion resistant materials, used in creation of aviation and rocket technology, carriers with developed surface of heterogeneous catalysis catalysts, materials of chemical sensorics, filters for filtering flows of incandescent gases and melts, as well as in nuclear power industry technologies. To obtain nanostructures SiC ceramics solution of phenolformaldehyde resin with weight content of carbon from 5 to 40% with tetraethoxysilane with concentration from 1·10-3 to 2 mol/l and acidic catalyst of tetraethoxysilane hydrolysis id prepared in organic solvent; hydrolysis of tetraethoxysilane is carried out at temperature 0÷95°C with hydrolysing solutions, containing water and/or organic solvent, with formation of gel. Obtained gel is dried at temperature 0÷250°C and pressure 1·10-4÷1 atm until mass change stops, after which carbonisation is realised at temperature from 400 to 1000°C for 0.5÷12 hours in inert atmosphere or under reduced pressure with formation of highly-disperse initial mixture SiO2-C, from which ceramics is moulded by spark plasma sintering at temperature from 1300 to 2200°C and pressure 3.5÷6 kN for from 3 to 120 min under conditions of dynamic vacuum or in inert medium. Excessive carbon is burned in air at temperature 350÷800°C.

EFFECT: obtaining nanostructured silicon-carbide porous ceramics without accessory phases.

4 cl, 4 dwg, 3 ex

FIELD: medicine.

SUBSTANCE: what is presented is a method for preparing submicron biphasic tricalcium phosphate and hydroxyapatite ceramics involving synthesis of single-phase powder of calcium salts and ammonium hydrophosphate, disaggregation, moulding and annealing. According to the invention, the calcium salt is presented by calcium acetate in the form of an aqueous solution of the concentration of 1M - 2M in Ca/P ratio applicable for initial salts and falling within the range of 1.5-1.6. The synthesis procedure involves single-step pouring of an aqueous solution of ammonium hydrophosphate to the aqueous solution of calcium acetate and mixing of the above solutions for 10-20 minutes, and separating the precipitate. The products are annealed at a temperature falling within the range of 1,050-1,150°C and kept at the above temperature for 0.5-1.5 hours. The produced ceramics contains β-tricalcium phosphate and hydroxyapatite with a grain size of 400-600 nm.

EFFECT: preparing the submicron biphasic ceramics having a uniform microsctructure.

2 dwg, 1 tbl, 1 ex

FIELD: physics, optics.

SUBSTANCE: invention relates to forming a digital imaginary image of the surface of a nano-object in a scanning tunnelling microscope. An imaginary image of a nano-object is its topography, which is different from the true topography, but retains distinctive features. A method of forming an imaginary image of the surface of a nano-object in a scanning tunnelling microscope includes scanning the surface of the analysed substance with a metal needle in direct current mode, for which, at each scanning point, the needle is moved vertically relative to the analysed surface such that tunnelling current at each scanning point is equal to the tunnelling current at the first scanning point. Data on the microstructure of the surface of the analysed substance are obtained by recording movement of the needle. A plane, which is parallel to the surface of the substrate, which is higher than the initial roughness of the substrate but lower than the transverse radius of the nano-object, is subtracted from the experimental topography of the surface with nano-objects on the substrate. The obtained image of the nano-object is scaled by multiplying with a coefficient greater than one.

EFFECT: high selective resolution and efficiency of scanning tunnelling microscopy of nano-objects, for example, polymer molecules, enabling use of the method to determine the fragmentary sequence thereof.

3 cl, 2 dwg

FIELD: measurement equipment.

SUBSTANCE: device is used to determine spectrum of size of suspended particles in gases, comprising the following components installed along the analysed gas flow: an inlet nozzle with supply channels; diffusion batteries of meshed type for passage of aerosol particles of certain size; an aggregating device of condenser growth; a counting volume; a vacuum pump; temperature sensors, a heater, a cooler and a microcontroller for control of heating and cooling processes in the aggregating device of condenser growth; an optical system comprising a pulse source of radiation, a lighter and lenses for focusing of optical radiation in the field of counting volume of particle flow and generation of images on a CCD array; an analogue-digital converter and a PC for control of the microcontroller of thermostatting, the vacuum pump and processing of six images of aggregated particles for analysis of the spectrum of their size. The device makes it possible to process simultaneously six images of aggregated particles on a PC, which characterise various size ranges of nanoparticles.

EFFECT: invention makes it possible to reduce time of measurements and to increase their accuracy.

3 dwg

FIELD: medicine.

SUBSTANCE: invention refers to medicine, namely to pharmaceutical engineering, and concerns a method for the quantitative estimation of chemically combined organic substances, first of all, biologically active and medical substances with a nanodiamond surface in its conjugate. The method is based on using the method for the qualitative IR-spectroscopy of the conjugate and model mixtures of the organic substance with the nanodiamond to be detected. IR-spectrum signal intensity/amount of the model mixture organic substance calibration curves are constructed to determine its content in the conjugate.

EFFECT: improving the method.

3 tbl, 5 dwg, 1 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to pharmaceutics and represents a suspension for treating psoriasis, containing calcipotriol monohydrate in the form of nanocrystals having the particle size distribution within the range of 200-600 nm; the particles are dispersed in an aqueous phase containing a non-ionic polymer surfactant specified in a group consisting of a surfactant in the form of poloxamers or polysorbates, in the amount of 0.01-5 wt % calculated using a suspension for preventing development of aggregation and/or calcipotriol monohydrate nanocrystal growth; the calcipotriol monohydrate nanocrystals are produced in the suspension by processing the suspension by a method involving the stages of reduction in crystalline calcipotriol monohydrate particle size in an aqueous phase to form microparticles having the particle size distribution within the approximate range of 5-20 mcm and the average approximate particle size of 10 mcm; the suspension is exposed to three high-pressure homogenisation cycles for 7-15 minutes each; in the first, second and third cycles, the pressure makes 300-800 bars, 800-1,200 bars and 1,200-1,700 bars respectively.

EFFECT: invention provides creating the local composition containing calcipotriol as an active agent, however being free from propylene glycol as a solvent.

34 cl, 8 ex, 5 tbl, 9 dwg

FIELD: electricity.

SUBSTANCE: invention is related to electrochemical installation intended to shape nanosized coating and may be used in semiconductor and electronics industry. The installation contains a computer, a controller and manipulator 1 mounted at the rack 2 rotatable around vertical axis and equipped with holder 3 for a processed sample 4. Around the manipulator 1 rack there are electrochemical cells 5 with electrodes connected to one pole of current source. The sample 4 submerged to electrochemical cells is connected to the other pole of current source. Holder 3 is installed so that it can be moved in regard to manipulator 1, and at that sample 4 in downwardmost position of holder 3 is placed in one of electrochemical cells. One of electrochemical cells is made as measuring cell 7 to control parameters of the processed sample 4. The installation is equipped with tube-type furnace 8 intended for thermal processing of the sample.

EFFECT: potential determining and setting of the required parameters for obtained nanomaterial against absolute value and conditions of their change.

4 dwg

FIELD: medicine.

SUBSTANCE: invention relates to medicine and deals with nanoliposome which includes liposomal membrane, contains ethgerificated lecitin and one or more physiologically active ingredients, incorporated in the internal space of liposomal membrane, method of obtaining such, as well as composition for prevention or treatment of skin diseases, containing nanoliposome.

EFFECT: invention ensures long-term stability and homogenecity of nanoliposomes.

15 cl, 22 ex, 4 dwg, 2 tbl

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