Hydrogen generation method

FIELD: hydrogen production processes.

SUBSTANCE: invention relates to catalytic processes of hydrogen production from hydrocarbon-containing gases. Method of invention comprises elevated-pressure catalytic decomposition of methane and/or natural gas into hydrogen and carbon followed by gasification of the latter with the aid of gasification reagent in several in parallel installed interconnected reactors, each of them accommodating preliminarily reduced catalyst bed. When one of reactors is run in methane and/or natural gas decomposition mode, the other gasifies carbon, the both operation modes being regularly switched. Operation period in one of the modes ranges from 0.5 to 10 h. Carbon gasification reagent is, in particular, carbon dioxide and catalyst utilized is reduced ferromagnetic thermally stabilized product consisting of iron oxides (30-80 wt %) and aluminum, silicon, magnesium, and titanium oxides. Methane and/or natural gas is decomposed at 625-1000°C and overpressure 1 to 40 atm.

EFFECT: ensured environmental safety and increased productivity of process.

3 cl, 1 dwg, 8 ex

 

The invention relates to catalytic processes for producing hydrogen and carbon from hydrocarbon gases. Hydrogen after its separation from the mixture of gases may be used as a reductant in various chemical, metallurgical and other industries, and also as a reagent for fuel cell vehicles and Autonomous sources of electricity.

A known method of producing hydrogen and filamentous carbon by decomposition at elevated temperature hydrocarbon gas on the catalyst, including the recovered hydrogen ferromagnetic thermally stabilized product, isolated by magnetic separation of ash from the combustion of coal in thermal power plants. The catalyst is a structure consisting of 18-90% of iron oxide and containing oxides of aluminum, magnesium and silicon - rest, and the process is conducted at a pressure of 1-40 and at a temperature of 500-1200°With (Application for a patent of the Russian Federation No. 2004137196 from 20.12.04 on CL IPC From 01 31/26).

The main disadvantage of this method is that the process of pyrolysis of methane and/or natural gas is carried out until complete deactivation of the catalyst with a corresponding fall in the time of the release of hydrogen to zero and undefined conditions catalyst regeneration.

Famous t is the train high-temperature method of producing hydrogen by the decomposition of methane on the catalyst Ni/SiO 2gasification deposited on the catalyst to carbon using the CO2(S.Takenaka, K.Otsuka. Specific reactivity of the carbon filaments formed by decomposition of methane over Ni/SiO2catalyst: gasification with CO2. Chem. Lett. 2001. 218-219).

The disadvantages of the method are relatively low catalyst activity and resistance to deactivation.

Closest to the claimed invention is a continuous method of producing hydrogen at a relatively low process temperature (about 650° (C) using methane and/or natural gas and steam, as well as the catalytically active metal of the 8th group of the periodic system of elements (Patent EP No. 1227062, CL 01 In 3/26, B 01 J B 08/06, 2002).

The process is carried out in two parallel reactors, each of which is placed the required amount of catalyst. The catalyst is subjected to restore using the corresponding component, and then one of them serves methane and/or natural gas, and the other pairs with regular switching of the supply of these components from one reactor to another. This combined gas stream contains a sufficient amount of hydrogen. The process is performed at a pressure close to atmospheric. The switching time of the filing of the components in the reactor is 5-15 minutes.

The obvious disadvantages of this method of producing hydrogen are expensive is the used catalysts (through the use of Ni, Co, Zr, etc.), the complexity of their preparation and relatively low activity, low switching time supply of reagents from one reactor to another. In addition, contamination of the combined gas stream oxides of carbon does not allow its use as an energy source for hydrogen fuel cells.

The aim of the present invention is the creation of environmentally friendly hydrogen production resulting from the use of carbon dioxide as an agent, the gasification of the carbon incorporated in the catalyst. This reduces emissions and emissions of carbon dioxide, produced in large quantities when used as the gasification agent, water, and, accordingly, does not affect the increase of the greenhouse effect. In addition, you get a valuable product, which is the oxide of carbon is widely used in various fields of the chemical industry for organic synthesis. Increasing the duration of reactor operation in one mode improves the performance of the process of obtaining the target product.

The proposed method of continuous production of hydrogen involves the catalytic decomposition at a temperature 625-1000°and pressure of 1-40 ATI methane and/or natural gas into hydrogen and carbon in several parallel installed and connected with the OI reactors. In each of the reactors placed previously restored a layer of iron-containing catalyst in which iron is presented in the form of oxides. The iron oxides are part of the restored ferromagnetic thermally stabilized product isolated from the ash from the combustion of coal in thermal power plants by magnetic separation with subsequent particle size distribution and hydrodynamic classification and consisting of iron oxide in the amount of 30-80 wt.% the composition of the oxides of aluminum, silicon, magnesium, titanium. Further, in one of the reactor for 0.5-10 hours serves methane and/or natural gas, and it operates in a mode decomposition of methane and/or natural gas. After that, the flow of methane and/or natural gas ceased, the reactor switch mode gasification and serves carbon dioxide as a reactant the gasification of carbon. And the flow of methane and/or natural gas beginning in another reactor. Switching supply of reagents from one reactor to another exercise as deactivation of the catalyst, which is restored after the gasification of a carbon containing gas leaving the first reactor.

Distinctive features of the proposed technical solutions are: duration of operation of the reactor in one of the modes of decomposition of methane and/or natural gas regasification carbon component 0.5 to 10 hours, is used as the gasification of carbon reagent carbon dioxide, and as a catalyst for the decomposition of methane and/or natural gas recovered ferromagnetic thermally stabilized product consisting of iron oxide in the amount of 30-80 wt.%, oxides of aluminum, silicon, magnesium, titanium.

Other distinctive features are the process of decomposition of methane at a temperature of 625-1000°and pressure of 1-40 ATI.

In addition, the restored ferromagnetic thermally stabilized product is obtained from the ash obtained by burning coal at thermal power plants by magnetic separation with subsequent particle size distribution and hydrodynamic classification.

The combination of the above essential features of the invention will reduce emissions and the emissions of carbon dioxide, produced in large quantities when used as the gasification agent is water. You get a valuable product, which is the oxide of carbon is widely used in various fields of chemical industry, organic synthesis, and also to improve the performance of the process of obtaining the target product.

Gasification formed during the catalytic pyrolysis of methane and/or natural gas coal the ode using as the gasification agent, carbon dioxide allows you to regenerate in the future reuse of the catalyst, usefully applied in the process of producing hydrogen greenhouse gas (CO2), thereby reducing its emission into the atmosphere, to produce valuable chemical and other industries product.

The drawing shows a schematic diagram of an installation for implementing the method of continuous production of hydrogen.

Installation includes: reactors 1 and 2, placed in layers 3 and 4 of the restored iron-containing catalyst, the nozzles 5 and 6 for feeding methane and/or natural and carbon dioxide, multi-way valve 7 to switch the incoming reactants, the pipes 8 and 9 for feeding the reactants in the reactors 1 and 2, the pipes 10 and 11 for the output of the reactor hydrogen and carbon monoxide, respectively, of a multi-way valve 12 to switch output reagents and evacuate them by pipes 13 and 14 of the process.

The method is as follows.

Methane and/or natural gas by pipe 5 through the multi-way valve 7 from a source (not shown) and the pipe 8 into the reactor 1, where the catalyst layer 3 flows through the reaction of the decomposition of the hydrocarbons with the formation of carbon and hydrogen. The hydrogen-containing gas through the pipe 10 through the multi-way valve 12 and the pipe 13 leaves the installation. The duration of operation of the reactor 1 in the mode decomposition of methane and/or natural gas is 0.5-10 hours. After that, the reactor through the multi-way valve 7 from a source (not shown) through the pipe 5 and the pipe 8 serves the carbon dioxide gasification of carbon. The formed carbon monoxide through the multi-way valve 12 and the pipe 13 is removed from the installation.

Simultaneously start the flow of methane and/or natural gas through the pipe 6 through the multi-way valve 7 from a source (not shown) and the pipe 9 into the reactor 2, where the catalyst layer 4 flows through the reaction of the decomposition of the hydrocarbons with the formation of carbon and hydrogen. The hydrogen-containing gas through the pipe 11 through the multi-way valve 12 to the pipe 14 leaves the installation. The duration of operation of the reactor 2 in the mode decomposition of methane and/or natural gas is 0.5-10 hours. After that, the reactor 2 through the multi-way valve 7 from a source (not shown) through the pipe 6 and the pipe 9 serves the carbon dioxide gasification of carbon. The formed carbon monoxide through the multi-way valve 12 to the pipe 14 is removed from the installation. Then there is the switch the supply of raw threads.

The invention is illustrated by the following examples.

Example 1 (the prototype). The process is carried out in two parallel reactors, each of which is placed the required amount of catalyst. The catalyst restore using the appropriate component, and then one of them serves methane and/or natural gas, and the other pairs with regular switching of the supply of these components from one reactor to another. Catalysis is the PR, consisting of NiO-ZrO2(the molar ratio of Ni/Zr=1,0), restore nitric mixture (5 mol % N2) at 601°and a bulk velocity of the mixture 4230 cm3/gcat.hour for 10 hours. Then the nitrogen-hydrogen mixture is replaced by attometer (71,4 mol % SN4) and at a temperature of 613°To carry out the process of producing hydrogen for 5 minutes. Then into the reactor instead of a nitrogen-methane mixture serves water vapor (83.7 mol % nitrogen) and at a temperature of 610°hold delete (gasification) previously formed carbon within 5 minutes. Performance on hydrogen derived from methane and/or natural gas, is to 91.6 mmol./gcat.hour. However due to the reaction of steam gasification of carbon leads to the formation of CO (6.1 mmol/gcat.hour), and CO2(to 39.6 mmol/gcat.hours).

Example 2 (the prototype). Similar to example 1. Differences: when recovering a catalyst space velocity of nitric mixture is 15050 cm3/gcat.the hour when the hydrogen content of 20 mol %, the temperature 520°s With a recovery period of 1 hour; if the reaction pyrolysis of methane and/or natural gas volumetric rate of the nitrogen-methane mixture is 10320 cm3/gcat.the hour when the methane content of 50 mol % and 590°; gasification of carbon space velocity is areatotal mixture (80,9 mol %) is 6773 cm 3/gcat.hour, the temperature 587°C. the Period of time between the switching of commodity flows is 7 minutes. Performance on hydrogen derived from methane is 75 mmol/gcat.hour. Due to the reaction of gasification is education or 37.4 mmol/gcat.h CO2.

Example 3 (according to the invention). The catalyst containing wt.%: 59,2 Fe2About3, 8,8 Al2About3, 26,0 SiO2of 1.5 MgO, 0,69 TiO2, recover hydrogen for 5 hours at a flow rate 45000 cm3/gcat.an hour and a temperature of 650°C. Then hydrogen is replaced by methane and/or natural gas and at a temperature of 650°and a pressure of 15 MPa carry out the process of producing hydrogen for 10 hours. Then into the reactor instead of methane and/or natural gas serves the carbon dioxide with a volume rate of 45,000 cm3/gcat.hour and at a temperature of 800°and 1 MPa for 10 hours to carry out the gasification of the previously formed carbon to form CO. Performance on hydrogen derived from methane and/or natural gas, is 180,8 mmol/gcat.hour. The average emission of carbon monoxide is also 180,8 mmol/gcat.hour.

Example 4. Similar to example 3. Differences: temperature recovery of the catalyst 600°C; temperature pyrolysis of methane and/or natural gas 650°S, length is lnost 4 hours; the temperature of the gasification process 750°time 4 hours. The performance of hydrogen and carbon monoxide 200,9 mmol/gcat.hour.

Example 5. Similar to example 3. Differences: temperature recovery of the catalyst 750°C; temperature pyrolysis of methane and/or natural gas - 750°S, the duration of operation of the reactor 4 hours; the duration of the gasification process 4 hours. The performance of hydrogen and carbon monoxide 421,9 mmol/gcat.hour.

Example 6. Similar to example 3. Differences: the recovery of the catalyst is a mixture of hydrogen and argon (10,2% about. H2) when flow rate 30000 cm3/gcat.hour and at a temperature of 688°C for 1 hour; duration of pyrolysis of methane and/or natural gas, 3 hours; duration gasification 3 hours. The performance of hydrogen and carbon monoxide 502,2 mmol/gcat.hour.

Example 7. Similar to example 3. Differences: the composition of the used catalyst, wt.%: 69,5 Fe2O3, 7,5 Al2About3, 22,2 SiO2, 2,0 MgO, 0,8 TiO2. The performance of hydrogen and carbon monoxide 221,0 mmol/gcat.hour.

Example 8. Similar to example 3. Differences: temperature recovery of the catalyst 600°S; the duration of the pyrolysis of methane and/or natural gas for 2 hours at 700°and a pressure of 1 MPa; the duration of the gasification process 2 hours. Performance on water is an ode and carbon monoxide to 130.6 mmol/g cat.hour.

Thus, the analysis of the above experimental results shows that the iron-containing catalysts, characterized by a strong interaction of the active ingredient with the carrier, in this cyclic process is highly active and stable level of performance over many cycles. In the process of gasification of the resulting carbon is carbon dioxide consumption belonging to the class of the greenhouse, and intensive formation of carbon monoxide, which is a valuable chemical product. The selected interval duration of the cycle contributes to the improvement of technological process.

1. Method for continuous production of hydrogen, comprising the catalytic decomposition at elevated temperatures of methane and/or natural gas into hydrogen and carbon gasification last through the gasification agent in several parallel installed and interconnected reactors, each of which is placed a pre-restored the catalyst bed, and when one of the reactors operating in the mode of decomposition of methane and/or natural gas, the other at this time operates in the mode of gasification of carbon, while the reactors regularly switch from one mode to another, characterized in that the length of p is bots reactor in one of the modes of decomposition methane and/or natural gas or gasification of carbon is 0.5-10 h, as the gasification of carbon reagent use carbon dioxide as catalyst for the decomposition of methane and/or natural gas use restored ferromagnetic thermally stabilized product consisting of iron oxide in the amount of 30-80 wt.%, oxides of aluminum, silicon, magnesium, titanium.

2. Method for continuous production of hydrogen according to claim 1, characterized in that the decomposition of methane and/or natural gas is carried out at a temperature 625-1000°and pressure of 1-40 ATI.

3. Method for continuous production of hydrogen according to claim 1, characterized in that the recovered ferromagnetic thermally stabilized product is obtained from the ash obtained by burning coal at thermal power plants by magnetic separation with subsequent particle size distribution and hydrodynamic classification.



 

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3 cl, 3 ex, 1 tbl

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4 dwg

FIELD: chemical industry; methods of extraction of fullerenes.

SUBSTANCE: the invention is pertaining to the field of chemical industry, in particular, to the method of extraction of fullerenes. The method provides that the fullerene-containing soot is mixed with the natural vegetable essential oil. The preferable ratio is 1:(50-200) accordingly. It is possible to use a turpentine oil, camphoric or menthol oil. The mixture is placed in the ultrasonic bath and in the volume of the indicated mixture find a resonant frequency, for example, within 20-50 kHz. It is possible to use the ultrasonic radiation with the sinusoidal, rectangular or sawtooth form of impulses and to affect on the mixture by the selected frequency for no less than 20 minutes at the temperature of 40-80°C. The formed slurry is subjected to centrifuging, preferably, during 30-40 minutes at 20 000-40 000 g, where g is the acceleration of gravity. The supernatant liquid is filtered through the membrane filter with the pores diameter of no more than 0,2 microns. The solution is subjected to evaporation up to a permanent weight, for example, at the temperature of 130-140°C. The invention allows to extract effectively fullerenes, using nontoxic natural extractants.

EFFECT: the invention ensures effective extraction of fullerenes using the nontoxic natural extractants.

11 cl, 2 dwg, 4 ex

FIELD: atomic power; methods of utilization of substandard materials.

SUBSTANCE: the invention is pertaining to the field of atomic power, to the methods of utilization of substandard materials such as the reactor black lead and a solid fuel, in particular, to production of fullerene. The invention provides for preparation of a mixture from the solid fuel and the spent reactor black lead ground up to the size of the fraction of no more than 2 mm at their ratio from 1:2 to 1:10 accordingly. Intermix it up to production of the uniform mass. In addition introduce MgO,Al2О, SiO2,CaF2 andC20-28 in amountof 5 % from the total mass of the mixture. The prepared mixture feed to the reaction zone of the installation. Conduct the thermal sublimation first at the temperature of 1800÷2700°C with the subsequent temperature rise up to 3500-5000°C. The reprocess product is withdrawn to the ultracentrifuge for separation. The separated solid material is withdrawn for usage as the target product - fullerene. The gaseous phases are subjected to the bubbling process through the alkaline solution with the subsequent conservation of a deposit. The final treatment of the gas is conducted using the screen of Petrjanov's system. The invention allows to expand the source base of raw materials for production of fullerenes, allows to utilize sub-standard materials and to improve ecology.

EFFECT: the invention ensures expansion of the source base of raw materials for production of fullerenes, utilization of sub-standard materials for the purpose and to improve ecology.

2 cl

FIELD: chemical industry; methods of separation (extraction) of the natural and synthetic materials.

SUBSTANCE: the invention is pertaining to the field of chemical industry, to the methods of separation (extraction) of the natural and synthetic materials, in particular, to separation and purification of the most wide-spread fullerenes - C60 andC70 from the natural fullerene-containing soot of schungite carbon. The purpose of the offered invention is to simplify the method of separation of fullerenes from schungite, to increase the amount of the treated raw, to decrease the power input costs in terms of the costs per a unit of weight of the target product. The substance of the invention is that the processes of extraction and crystallization are combined in one production cycle, that allows considerably to reduce the solvent concentration. The purpose in view is realized by extraction from the water-schungite suspension using the sulfur-carbon bisulfide solution and the subsequent crystallization purification of the near-surface volumes of the produced solution. Besides an increase of effectiveness of the extraction according to the offered method is achieved by an anodic pickling of the schungite powder and irradiation by short-range UDV-light of the water-schungite suspensions.

EFFECT: the invention allows to simplify the method of separation of fullerenes from schungite, to increase the amount of the treated raw, to decrease the power input costs in terms of the costs per a unit of weight of the target product.

3 cl, 3 dwg, 6 dwg

FIELD: high-temperature superconductivity physics, chemistry, biophysics, medicine, biology, electronics, optoelectronics and material technology.

SUBSTANCE: graphite specimen 1, either monolythic or in form of tube is placed in radioparent tube 3 with high-frequency inductor 4 located along its axis and connected with RH oscillator 5. These units of plant are combined in heating system 2 made in form of closed space. It is connected with inert gas supply system 6 through flow meter 7 and gas former 8 connected in series; gas former 8 has helical thread for forming twisted flow. Carbon from surface of specimen 1 is directed in flow of inert gas to storage reservoir 9 hermetically connected with heating system 2 and inert gas discharge system 12. Storage reservoir 9 is provided with soot collector 10 located outside heating system 2 and provided with cooling system 11. Productivity of plant is increased by 10 times with no impairment of quality.

EFFECT: enhanced efficiency; increased productivity.

7 cl, 1 dwg

FIELD: metallurgy, aircraft industry, power engineering, semiconductor technique.

SUBSTANCE: plate tar cake is ground to produce fractional makeup having at least 97 mass % of <0.09 mm-fraction and at least 91 % of <0.045 mm-fraction. Grinded cake is mixed with 35-40 % of coal-tar asphalt and 0.015-1.5 mass % of organic additive at 120-130°C. As organic additive space-hindered phenols and/or phenylphosphites are used. Obtained mass is formed, cooled and crushed followed by pressing to produce semimanufactured article with density of1.01-1.06 g/cm3. Said articles are sintered at 800-1300°C and black-leaded at 3000°C. Finished black-leaded material has bulk density of 1760-1950 kg/cm3, compression strength of 90-105 MPa and blending strength of 60-75 MPa. Material of present invention is useful in production of electrodes, seal assembly and material of high purity.

EFFECT: black-leaded material with improved physical characteristics.

1 tbl, 10 ex

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