Method of producing carbon nanofibres

FIELD: chemistry.

SUBSTANCE: invention relates to heterogeneous catalysis and can be used to recycle hydrocarbons and halogen-substituted hydrocarbons when producing composite materials, catalysts, sorbents and filters. Catalytic pyrolysis of hydrocarbons is carried out at 500-700°C on a catalyst obtained by dispersing articles of solid nickel and alloys thereof with other metals, e.g., iron, chromium, as a result of reaction with 1,2-dichloroethane vapour. The catalyst contains dispersed active nickel particles attached to carbon nanofibres with diameter 0.1-0.4 mcm. The starting material used is bromine- or chlorine-containing hydrocarbons, alkanes, olefins, alkynes or aromatic hydrocarbons, e.g., ethane, propane, acetylene, benzene. Output of carbon nanofibres is equal to or more than 600 g per 1 g metal.

EFFECT: high efficiency of the method.

5 cl, 2 dwg, 9 ex

 

The invention relates to the field of heterogeneous catalysis, in particular to a method of producing carbon nanofibers by pyrolysis conventional and halogen-substituted hydrocarbons on Nickel-containing catalysts. It can be used in the chemical and petrochemical industry, hydrogen energy for the disposal of hydrocarbons and kalogeropoulou, when receiving filters, sorbents, catalysts and composite materials.

A method of obtaining nanocolonies carbon through the decomposition of methane at a temperature of 700-750°C, or other hydrocarbons at 500-600°C in the catalyst containing Nickel, copper and trudnovosplamenjaemy oxides such as aluminum oxide, silicon oxide, zirconium oxide, magnesium oxide, titanium oxide or their mixture (EN 2312059, C01B 3/26, B01J 23/72, 10.12.2007).

A method of obtaining fibrous carbon structures by decomposition of hydrocarbons on the powdered catalyst containing Nickel and magnesium oxide (10 wt.%) or aluminum (5 wt.%) (EN 2296827, D01F 9/127, 10.04.2007).

There is a method of producing carbon fibers by catalytic pyrolysis of hydrocarbons on the powdery catalyst composition, wt.%: 70-90 Ni, 10-30 MgO; or 40-60% Co, 40-60% Al2O3; or Mo:Co:Mg with a molar ratio of 1:5:94, respectively, (EN 2258031, C01B 31/02, B82B 3/00, 10.08.2005).

A method of obtaining carbon nanotube the fluidized bed of catalyst (Claim US 2004234445, B01J 23/745, B01J 37/02, SW 31/02, SS 16/442, 25.11.2004). Using catalysts with the active component from 1 to 5 wt.%, and as the carrier is Al2O3.

There is a method of producing carbon nanofibers by decomposition of carbon-containing compounds on the catalyst consisting of Fe and/or modified Ti, V, Cr, Mn, W or Mo and deposited on Al2O3, MgO, SiO2, TiO2, CaO (Application WO 2009153970, B01J 23/76, SW 31/02, D01F 9/127, 23.12.2009).

The disadvantage of the above methods is that the used catalysts in addition to the active component contain insoluble oxides, such as: Al2O3, MgO, SiO2, TiO2, CaO, ZrO2. Thus obtained carbon material in its composition contains more impurities, which requires a more thorough cleaning of the final product.

There is a method of producing carbon nanofibers by decomposition of hydrocarbons on iron-vanadium catalysts (Application US 20090008611, B01J 21/18, D01F 9/12, NV 1/24, 08.01.2009). As a carrier of the active component used carbon black.

The disadvantage of this method is that the resulting carbon product in its composition also contains black carbon, used as a carrier of the active component.

The closest in technical essence is the fast method of obtaining carbon nanofibers by decomposition of methane catalysts, representing the Nickel particles deposited on carbon nanofibres (I.A.Maslov, A.A.Kamenev, I.G.Solomonik et al., Solid Fuel Chemistry, 2007, Vol.41, No.5, pp.307-312). Used catalysts obtained by impregnation of the carbon nanofiber aqueous solution of Nickel nitrate and subsequent annealing. This stage can significantly complicates the process of cooking and is the source of wastewater and emissions.

The present invention was to develop a more simplified method of producing carbon nanofibers, does not contain any additional additives, in addition to the active ingredient, and the use of a wide range of hydrocarbons, including halogen-substituted hydrocarbons.

The problem is solved by carrying out the synthesis of carbon nanofibers on the catalysts prepared carbon dispersion massive Nickel or an alloy based on it.

Carbon nanofibers produced by the catalytic pyrolysis of hydrocarbons using a catalyst obtained by dispersion of the products of massive Nickel as a result of interaction with pairs of 1,2-dichloroethane containing dispersed active particles of Nickel, mounted on carbon fibers with a diameter of 0.1-0.4 μm. The active catalyst particles are Nickel alloy, which, along with Nickel can the t contain other metals, such as Cr, Fe.

The process of obtaining carbon nanofibers is carried out in the temperature range 500-750°C.

As a source of raw materials used brominated or chlorinated hydrocarbons.

As a source of raw materials use alkanes or olefins or alkynes, or aromatic hydrocarbons, or mixtures thereof, such as, ethane, propane, acetylene, benzene, etc.

The essence of the method of preparation of the catalyst lies in the dispersion of metal (Ni or its alloy with Cr or Fe) foil having a thickness of 0.1 mm and a wire diameter of 0.1 mm as a result of interaction with a gas mixture of vapors of 1,2-dichloroethane (6%), hydrogen (40%vol.) and argon (54%) at a temperature of 550°C, leading to the growth of the carbon fibers and the separation of the dispersed metal particles from the surface of bulk metal. The process is similar to what happens when the surface treatment of metal (Ni, Fe, Co) in the usual hydrocarbon (S. Du, N. Pan, Materials Letters, 2005, Vol.59, N 13, 1678-1682; Martínez-Hansen V., N. Latorre, C. Royo et al. Catalysis Today, 2009, vol.147S, S71-S75), however, the use of mixtures containing 1,2-dichloroethane and hydrogen allows to intensify this process, leading to the complete massive transition metal in the catalytically active particles.

Obtained in this way, the catalyst contains a dispersion of the active particles of Nickel, mounted on carbon fibers with a diameter of 0.1-0.4 microns, and which can be used for decomposition as conventional hydrocarbons, such as alkanes, olefins, alkynes, aromatics and mixtures thereof, and halogen-substituted hydrocarbons.

The invention is illustrated by the following examples.

Example 1

The catalyst containing the dispersed active particles of Nickel, mounted on carbon fibers with a diameter of 0.1-0.4 μm composition 7.4% Ni/UNV, obtained by dispersion make massive Nickel metal pairs 1,2-dichloroethane, in the amount 16.11 mg load in a flow quartz reactor with weights Mac-Bains heat for 25-30 min in an argon flow of 10 l/h to a temperature of 550°C and restore the Ni particles within 15 min by feeding the reactor with hydrogen volumetric rate of 10 l/h of the Synthesis of carbon nanofibers is carried out in the reaction medium of the following composition,%: 1,2-dichloroethane - 6, ar - 54 hydrogen - 40. The volume flow of the reaction mixture is 16 l/h, the Average rate of growth of the carbon nanofibers is 3.2 gUNV/gNi·the hours that are recorded using weights Mac-Bains.

The resulting product consists of carbon nanofibers with a diameter of 0.1-0.5 μm (Figure 1).

Figure 1 presents a snapshot of the SEM (scanning electron microscopy) of the carbon product obtained by the decomposition of 1,2-dichloroethane on a Nickel catalyst at a temperature of 550°C.

Example 2

Similar to example 1, characterized in that as catalyzatoroprovod dispersed alloy of Nickel with chromium (20,0-23,0%) and iron (no more than 1.5%). Hanging the catalyst composition of 9.5% [Ni-Cr-Fe]/UNV is 34.3 mg the Rate of growth of the carbon nanofibers is 9.4 gUNV/gmeth·h.

Example 3

Similar to example 2, characterized in that the synthesis of carbon nanofibers is carried out at a temperature of 500°C. the addition of catalyst is 30.5 mg of the Rate of growth of the carbon nanofibers is 0.29 gUNV/gmeth·h.

Example 4

Similar to example 2, characterized in that the synthesis of carbon nanofibers is carried out at a temperature of 700°C. the addition of catalyst is 39.9 mg the Rate of growth of the carbon nanofibers is 46.87 gUNV/gmeth·h.

Example 5

Similar to example 2, characterized in that for obtaining carbon nanofibers use a mixture of the following composition,%: 1-rambutan - 6, ar - 54 hydrogen - 40. The temperature of the synthesis 750°C. the addition of catalyst 30.2 mg the Rate of growth of the carbon nanofibers is 14.0 gUNV/gMeg·h.

Example 6

Similar to example 2, characterized in that for obtaining carbon nanofibers use a mixture of the following composition,%: ethane - 6, ar - 54 hydrogen - 40. Hanging the catalyst composition 24.0% [Ni-Cr-Fe]/UNV is 30.2 mg. of synthesis Temperature to 600°C. the Rate of growth of the carbon nanofibers is 3.4 gUNV/gmeth·the hour. As a result, the image is tsya carbon nanofibers with a diameter of 0.1-1 µm (Figure 2).

Figure 2 presents a snapshot of SAM carbon product resulting from decomposition of ethane at a temperature of 600°C.

Example 7

Similar to example 6, characterized in that for obtaining carbon nanofibers used acetylene. The composition of the catalyst 5.4% [Ni-Cr-Fe]/UNV, hanging the catalyst 15.2 mg of the Rate of growth of the carbon nanofibers is 12.4 gUNV/gmeth·h.

Example 8

Similar to example 6, characterized in that for obtaining carbon nanofibers use a mixture of the following composition,%: benzene - 8, ar - 69 and hydrogen - 23. The addition of catalyst 23.7 mg the Rate of growth of the carbon nanofibers is 11.9 gUNV/gmeth·h.

Example 9

Similar to example 7, characterized in that as a hydrocarbon, a mixture of the following composition,%: propane - 80 and butane - 20. The temperature of the synthesis of 700°C. the addition of catalyst 20.5 mg the Rate of growth of the carbon nanofibers is 9.8 gUNV/gmeth·h.

Thus, it is shown that this method can be used to produce carbon nanofibers by catalytic pyrolysis of conventional and halogen-substituted hydrocarbons. The yield of carbon nanofibers in some cases up to 600 g per 1 g of the metal and more.

As the catalyst precursor can be used for sovan massive Nickel or an alloy based on it. The temperature range in which it is possible processes is 500-750°C.

1. Method of producing carbon nanofibers by catalytic pyrolysis of hydrocarbons, characterized in that the process is carried out using a catalyst obtained by dispersion of the products of massive Nickel as a result of interaction with pairs of 1,2-dichloroethane, and containing dispersed active particles of Nickel, mounted on carbon fibers with a diameter of 0.1-0.4 microns.

2. The method according to claim 1, wherein the used catalyst, obtained by dispersion of a massive Nickel alloy with other metals, such as Cr and Fe.

3. The method according to claim 1, characterized in that the process of obtaining carbon nanofibers is carried out in the temperature range 500-750°C.

4. The method according to claim 1, characterized in that the feedstock used bromine - or chlorine-containing hydrocarbons.

5. The method according to claim 1, characterized in that the feedstock used alkanes or olefins or alkynes, and aromatic hydrocarbons, such as ethane, propane, acetylene, benzene.



 

Same patents:

FIELD: chemistry.

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EFFECT: invention enables continuous synthesis of carbon fibre materials.

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FIELD: chemistry.

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FIELD: chemistry.

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15 cl, 3 dwg, 4 ex

FIELD: chemistry.

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is obtained with output 44-68%.

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FIELD: nanotechnologies.

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3 cl, 6 dwg

FIELD: process engineering.

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3 cl, 1 dwg, 6 tbl, 15 ex

FIELD: chemistry.

SUBSTANCE: invention can be used in medicine, biology, nanoelectronics, when manufacturing optical devices, as well as in standardisation and metrology. An initial fullerene extract containing C60, C60O, C70 C76/78 and C84 is enriched with fullerene C60 to 96±2% via fractional concentration. The solution of the obtained concentrate then undergoes chromatographic purification on activated carbon in an aromatic solvent until achieving concentration of fullerene C60 in the eluate of not less than 99.7%. The solid C60-rich product is extracted from the eluate and then subjected to vacuum sublimation heat treatment at pressure 10-2-10-3 torr and temperature 700-800°C for 90±30 minutes.

EFFECT: obtaining with minimal losses fullerene C60 with purity of 99,90-99,99%, ie, superhigh purity, which virtually does not contain oxide impurities, which can be seen on dwg 1.

3 tbl, 6 dwg

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