CN114634173B - Method for reforming methane-carbon dioxide and preparing carbon nano tube by coal modification catalysis - Google Patents
Method for reforming methane-carbon dioxide and preparing carbon nano tube by coal modification catalysis Download PDFInfo
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- CN114634173B CN114634173B CN202210477192.XA CN202210477192A CN114634173B CN 114634173 B CN114634173 B CN 114634173B CN 202210477192 A CN202210477192 A CN 202210477192A CN 114634173 B CN114634173 B CN 114634173B
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
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- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
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- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
- C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
- C01B2203/0238—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a carbon dioxide reforming step
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Abstract
The invention aims to provide a method for reforming methane-carbon dioxide and preparing carbon nanotubes by modifying and catalyzing coal, which belongs to the technical field of carbon materials. In addition, the invention also uses a solvent modification method to carry out solvent extraction modification treatment on part of macromolecules of the coal to obtain small-molecule benzene compounds, and the small-molecule benzene compounds are used as precursors for the growth of the carbon nanotubes, so that more carbon nanotubes can be generated under the action of a catalyst.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and particularly relates to a method for reforming methane-carbon dioxide and preparing carbon nanotubes by coal modification catalysis.
Background
Methane and carbon dioxide are main greenhouse gases, and methane carbon dioxide reforming reactions can obtain clean energy while alleviating the greenhouse effect.
The carbon nanotube is a tubular carbon molecule, and the current methods for preparing the carbon nanotube include an arc discharge method, a solid phase pyrolysis method, a laser evaporation method and a chemical vapor deposition method. However, in any method, carbon deposition is often generated during the process of generating the carbon nanotubes, and the carbon deposition is attached to the carbon nanotubes to inhibit the carbon nanotubes from continuing to be generated. Therefore, it is critical to solve the problem of carbon deposition of the carbon nanotubes.
Chinese patent CN106946223a discloses a methane carbon dioxide reforming process by contacting methane and carbon dioxide at 600-1000 ℃ with a catalyst formed by loading active component Ni on a SiC-C-N support. This patent, while writing to methane carbon dioxide reforming processes, is not used to produce carbon nanotubes. And the patent catalyst is formed by loading on an active component, and the catalyst is easy to deactivate.
It can be seen from the literature that there is no method for preparing carbon nanotubes by a coal modification method and reforming carbon deposits with methane and carbon dioxide in the process, and thus, there is an urgent need for a method for preparing carbon nanotubes by methane-carbon dioxide reforming with a simple and low-cost coal modification method.
Disclosure of Invention
The invention aims to provide a method for reforming methane-carbon dioxide and preparing carbon nano tubes by modifying coal.
The invention reforms methane and carbon dioxide and simultaneously generates carbon nanotubes, and carbon dioxide is used for removing carbon deposit so that the catalyst keeps activity and generates more carbon nanotubes. In addition, the invention also uses a solvent modification method to carry out solvent extraction modification treatment on part of macromolecules of the coal to obtain small-molecule benzene compounds, and the small-molecule benzene compounds are used as precursors for the growth of the carbon nanotubes, so that more carbon nanotubes can be generated under the action of a catalyst.
The invention adopts the following technical scheme:
a method for reforming methane-carbon dioxide and preparing carbon nanotubes by modifying coal, comprising the following steps:
the first step: selecting any one or a combination of a plurality of long flame coal or lignite, uniformly mixing the coal, crushing and screening to obtain coal particles A with the particle size of 1-10.0 mm;
and a second step of: 10-20 parts of coal particles A are selected for modification treatment, N-methyl pyrrolidone (NMP) solvent is used for soaking coal, and then toluene and 20-40 parts of dimethylbenzene with the volume ratio of 1:1 are added for solvent extraction, so that modified coal B is obtained. The main purpose is to carry out solvent extraction modification treatment on part of macromolecules of coal to obtain benzene series compounds of small molecules;
and a third step of: 30-60 parts of modified coal B is selected, then 30-180 parts of potassium hydroxide and barium hydroxide carbon nano-growth catalyst are added, wherein the mass part ratio of the potassium hydroxide to the barium hydroxide is 1:0-0.5, and the mixture C is obtained after uniform mixing. Placing the mixture C into a carbon nanotube preparation reactor, heating to 900-950 ℃ at a heating rate of 3-5 ℃/min, and keeping the temperature for 6-8 hours at the constant temperature to prepare a coal-based carbon nanotube D;
fourth step: weighing 20-40 parts of coal-based carbon nano tube D, putting into a methane carbon dioxide reforming reactor, and when the temperature is slowly stabilized to 850-970 ℃, keeping the temperature for 3-6 hours and introducing gas with the volume airspeed of 8000-30000 hours -1 Methane and carbon dioxide mixed gas, wherein the volume ratio of methane and carbon dioxide is 1:1, and reforming reaction is carried out to obtain mixed gas mainly comprising carbon monoxide and hydrogen;
fifth step: slowly stabilizing the methane carbon dioxide reforming reactor again, raising the temperature to 880-950 ℃, keeping the temperature constant for 0.5-1.5h, and introducing the methane carbon dioxide reforming reactor into the methane carbon dioxide reforming reactor for 8000-10000 h at a volume airspeed -1 Carbon dioxide gas is introduced to eliminate carbon deposit;
sixth step: on the basis of the completion of the step five, carrying out one or more times of circulation from the step four to the step five according to the reaction process until the conversion rate of methane carbon dioxide reforming is reduced or the carbon nano tube is stopped when no longer grows, and obtaining the treated coal-based carbon nano tube E;
seventh step: weighing 20-30 parts of coal-based carbon nanotubes E, soaking the coal-based carbon nanotubes E with 15-40 parts of tetralin hydrogen-supplying solvent, and removing residual carbon deposit to obtain purer coal-based carbon nanotubes F;
eighth step: and on the basis of the completion of the step seven, carrying out 1-3 times of circulation processes by taking the steps four to seven as one process to obtain the purer coal-based carbon nano tube G.
The beneficial effects of the invention are as follows:
the method breaks the large space network structure of coal by carrying out solvent soaking, extraction and modification treatment, adds a carbon nano tube growth catalyst to obtain coal-based carbon nano tubes, introduces methane and carbon dioxide mixed gas to react to generate carbon monoxide and hydrogen, continuously introduces carbon dioxide to eliminate carbon deposit, generates carbon nano tubes, and repeatedly and circularly introduces methane and carbon dioxide gas until the conversion rate of methane and carbon dioxide reforming is reduced or the carbon nano tubes are not grown any more, and finally, impregnates with hydrogen supply solvent to remove carbon deposit to obtain the carbon nano tubes.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Fig. 2 is a TEM image of a carbon nanotube prepared according to the present invention.
Fig. 3 is a TEM image of a carbon nanotube prepared according to the present invention.
Detailed Description
For a more particular understanding of the technical content, features and effects of the present invention, the present invention will now be described in further detail with reference to the accompanying drawings and examples.
Example 1
A method for reforming methane-carbon dioxide and preparing carbon nanotubes by modifying coal, comprising the following steps:
the first step: selecting long flame coal of Shenmu, uniformly mixing the coal, crushing and screening to obtain coal particles A with the particle size of 1-10.0 mm;
and a second step of: and (3) selecting 20 parts of the coal particles A obtained in the step (I) for modification treatment, soaking the coal in an N-methylpyrrolidone (NMP) solvent, and then adding 20 parts of toluene and xylene in a volume ratio of 1:1 for solvent extraction to obtain modified coal B. The main purpose is to carry out solvent extraction modification treatment on part of macromolecules of coal to obtain benzene series compounds of small molecules;
and a third step of: selecting 30 parts of modified coal B obtained in the second step, then adding 30 parts of potassium hydroxide and barium hydroxide carbon nanotube growth catalyst, wherein the mass part ratio of the potassium hydroxide to the barium hydroxide is 1:0, and uniformly mixing to obtain a mixture C. Putting the mixture C into a carbon nanotube preparation reactor, heating to 950 ℃ at a heating rate of 3 ℃/min, and keeping the temperature for 8 hours at the constant temperature to prepare a coal-based carbon nanotube D;
fourth step: weighing 20-40 parts of the coal-based carbon nano tube D obtained in the step three, putting the coal-based carbon nano tube D into a methane carbon dioxide reforming reactor, and when the temperature is slowly increased to 970 ℃, keeping the temperature for 6 hours and introducing gas with the volume space velocity of 30000 hours -1 Methane and (2)The mixed gas of carbon dioxide and methane is subjected to reforming reaction to obtain mixed gas mainly comprising carbon monoxide and hydrogen, wherein the volume ratio of methane to carbon dioxide is 1:1;
fifth step: slowly stabilizing the temperature of the methane carbon dioxide reforming reactor again to 880 ℃, keeping the temperature for 0.5h, and introducing the air velocity of the volume to 8000h -1 Carbon dioxide gas is introduced to eliminate carbon deposit;
sixth step: on the basis of the completion of the step five, carrying out one or more times of circulation from the step four to the step five according to the reaction process until the conversion rate of methane carbon dioxide reforming is reduced or the carbon nano tube is stopped when no longer grows, and obtaining the treated coal-based carbon nano tube E;
seventh step: weighing 20 parts of coal-based carbon nanotubes E obtained in the step six, and soaking the coal-based carbon nanotubes E with 15 parts of tetralin hydrogen-supplying solvent to remove residual carbon deposit, so as to obtain purer coal-based carbon nanotubes F;
eighth step: and on the basis of the completion of the step seven, carrying out 1-3 times of circulation processes by taking the steps four to seven as one process to obtain the purer coal-based carbon nano tube G.
The yield of carbon nanotubes obtained by this process was 18wt%.
Example 2
A method for reforming methane-carbon dioxide and preparing carbon nanotubes by modifying coal, comprising the following steps:
the first step: selecting the Hulenbeier lignite, uniformly mixing, crushing and screening the coal to obtain coal particles A with the particle size of 1-10.0 mm;
and a second step of: and (3) selecting 15 parts of the coal particles A obtained in the step (I) for modification treatment, soaking the coal in an N-methylpyrrolidone (NMP) solvent, and then adding 40 parts of toluene and xylene in a volume ratio of 1:1 for solvent extraction to obtain modified coal B. The main purpose is to carry out solvent extraction modification treatment on part of macromolecules of coal to obtain benzene series compounds of small molecules;
and a third step of: 45 parts of modified coal B obtained in the second step is selected, 135 parts of potassium hydroxide and barium hydroxide carbon nano tube growth catalyst are added, wherein the mass part ratio of the potassium hydroxide to the barium hydroxide is 1:0.5, and the mixture C is obtained after uniform mixing. Putting the mixture C into a carbon nanotube preparation reactor, heating to 900 ℃ at a heating rate of 5 ℃/min, and keeping the temperature for 6 hours at the constant temperature to prepare a coal-based carbon nanotube D;
fourth step: weighing 20-40 parts of the coal-based carbon nanotube D obtained in the step three, putting the coal-based carbon nanotube D into a methane carbon dioxide reforming reactor, and when the temperature is slowly increased to 900 ℃, keeping the temperature for 4.5 hours and introducing gas with the volume airspeed of 20000 hours -1 Methane and carbon dioxide mixed gas, wherein the volume ratio of methane and carbon dioxide is 1:1, and reforming reaction is carried out to obtain mixed gas mainly comprising carbon monoxide and hydrogen;
fifth step: slowly stabilizing the methane carbon dioxide reforming reactor again, raising the temperature to 950 ℃, keeping the temperature for 1h, and introducing the methane carbon dioxide reforming reactor into the methane carbon dioxide reforming reactor with the volume space velocity of 10000h -1 Carbon dioxide gas is introduced to eliminate carbon deposit;
sixth step: on the basis of the completion of the step five, carrying out one or more times of circulation from the step four to the step five according to the reaction process until the conversion rate of methane carbon dioxide reforming is reduced or the carbon nano tube is stopped when no longer grows, and obtaining the treated coal-based carbon nano tube E;
seventh step: weighing 25 parts of coal-based carbon nanotubes E obtained in the step six, and soaking the coal-based carbon nanotubes E with 25 parts of tetralin hydrogen-supplying solvent to remove residual carbon deposit, so as to obtain purer coal-based carbon nanotubes F;
eighth step: and on the basis of the completion of the step seven, carrying out 1-3 times of circulation processes by taking the steps four to seven as one process to obtain the purer coal-based carbon nano tube G.
The yield of carbon nanotubes obtained by this process was 25wt%.
Example 3
A method for reforming methane-carbon dioxide and preparing carbon nanotubes by modifying coal, comprising the following steps:
the first step: selecting any one or a combination of a plurality of long flame coal or lignite, uniformly mixing the coal, crushing and screening to obtain coal particles A with the particle size of 1-5 mm;
and a second step of: and (3) selecting 20 parts of the coal particles A obtained in the step (I) for modification treatment, soaking the coal in an N-methylpyrrolidone (NMP) solvent, and then adding 30 parts of toluene and xylene in a volume ratio of 1:1 for solvent extraction to obtain modified coal B. The main purpose is to carry out solvent extraction modification treatment on part of macromolecules of coal to obtain benzene series compounds of small molecules;
and a third step of: 60 parts of modified coal B obtained in the second step is selected, 180 parts of potassium hydroxide and barium hydroxide carbon nano tube growth catalyst are added, wherein the mass part ratio of the potassium hydroxide to the barium hydroxide is 1:0.25, and the mixture C is obtained after uniform mixing. Putting the mixture C into a carbon nanotube preparation reactor, heating to 930 ℃ at a heating rate of 4 ℃/min, and keeping the temperature for 7 hours at the constant temperature to prepare a coal-based carbon nanotube D;
fourth step: weighing 20-40 parts of the coal-based carbon nanotube D obtained in the step three, putting the coal-based carbon nanotube D into a methane carbon dioxide reforming reactor, and when the temperature is slowly increased to 850 ℃, keeping the temperature for 6 hours, and introducing gas with the volume space velocity of 8000 hours -1 Methane and carbon dioxide mixed gas, wherein the volume ratio of methane and carbon dioxide is 1:1, and reforming reaction is carried out to obtain mixed gas mainly comprising carbon monoxide and hydrogen;
fifth step: slowly stabilizing the methane carbon dioxide reforming reactor again, raising the temperature to 880 ℃, keeping the temperature for 1h, and introducing the methane carbon dioxide reforming reactor into the methane carbon dioxide reforming reactor for 9000h -1 Carbon dioxide gas is introduced to eliminate carbon deposit;
sixth step: on the basis of the completion of the step five, carrying out one or more times of circulation from the step four to the step five according to the reaction process until the conversion rate of methane carbon dioxide reforming is reduced or the carbon nano tube is stopped when no longer grows, and obtaining the treated coal-based carbon nano tube E;
seventh step: weighing 30 parts of coal-based carbon nanotubes E obtained in the step six, and soaking the coal-based carbon nanotubes E with 40 parts of tetralin hydrogen-supplying solvent to remove residual carbon deposit, so as to obtain purer coal-based carbon nanotubes F;
eighth step: and on the basis of the completion of the step seven, carrying out 1-3 times of circulation processes by taking the steps four to seven as one process to obtain the purer coal-based carbon nano tube G.
The yield of the carbon nano tube obtained by the process is 15wt percent.
The above embodiments may be combined with each other.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same; while the invention has been described in detail with reference to the preferred embodiments, those skilled in the art will appreciate that: modifications may be made to the specific embodiments of the present invention or equivalents may be substituted for part of the technical features thereof; without departing from the spirit of the invention, it is intended to cover the scope of the invention as claimed.
Claims (5)
1. A method for reforming methane-carbon dioxide and preparing carbon nanotubes by modifying coal, which is characterized in that: the method comprises the following steps:
firstly, uniformly mixing, crushing and screening selected coal to obtain coal particles A with the particle size of 1-10.0 mm;
secondly, taking 10-20 parts of coal particles A for modification treatment to obtain modified coal B;
thirdly, selecting 30-60 parts of modified coal B, adding 30-180 parts of carbon nano-growth catalyst, uniformly mixing to obtain a mixture C, placing the mixture C into a carbon nano-tube preparation reactor, heating to 900-950 ℃, and keeping the temperature for 6-8 hours at the temperature to obtain coal-based carbon nano-tubes D;
step four, weighing 20 to 40 parts of coal-based carbon nano tubes D, putting the coal-based carbon nano tubes D into a methane carbon dioxide reforming reactor, keeping the temperature constant for 3 to 6 hours when the temperature reaches 850 to 970 ℃, introducing mixed gas of methane and carbon dioxide, and carrying out reforming reaction to obtain mixed gas mainly comprising carbon monoxide and hydrogen;
fifthly, slowly stabilizing the methane carbon dioxide reforming reactor again at 880-950 ℃ for 0.5-1.5h, and introducing carbon dioxide gas;
step six, on the basis of the completion of the step five, carrying out one or more cycles from the step four to the step five according to the reaction process until the conversion rate of methane carbon dioxide reforming is reduced or the carbon nanotubes are stopped when no longer grow, so as to obtain the treated coal-based carbon nanotubes E;
seventh, weighing 20-30 parts of coal-based carbon nanotubes E, soaking the coal-based carbon nanotubes E with 15-40 parts of hydrogen-supplying solvent, and removing residual carbon deposit to obtain purer coal-based carbon nanotubes F;
eighth, based on the completion of the seventh step, taking the fourth step to the seventh step as a process, and performing 1-3 times of circulation processes to obtain purer coal-based carbon nanotubes G;
the coal in the first step comprises any one or a combination of a plurality of long flame coal or lignite;
the second step of coal modification treatment is to soak coal with N-methyl pyrrolidone solvent and then to extract the solvent;
in the third step, the carbon nano-growth catalyst is a mixture of potassium hydroxide and barium hydroxide, wherein the mass ratio of the potassium hydroxide to the barium hydroxide is 1:0-0.5;
the hydrogen donor solvent in the seventh step is tetralin.
2. The method for coal-modified catalytic methane-carbon dioxide reforming and carbon nanotube production according to claim 1, wherein: the solvent extraction is to add 20-40 parts of toluene and xylene in a volume ratio of 1:1.
3. The method for coal-modified catalytic methane-carbon dioxide reforming and carbon nanotube production according to claim 1, wherein: and in the third step, the heating rate is 3-5 ℃/min.
4. The method for coal-modified catalytic methane-carbon dioxide reforming and carbon nanotube production according to claim 1, wherein: the volume airspeed of the methane and carbon dioxide gas introduced in the fourth step is 8000-30000 h -1 The volume ratio of the introduced methane to the carbon dioxide gas is 1:1.
5. The method according to claim 1A method for reforming methane-carbon dioxide and preparing carbon nanotubes by modifying coal, which is characterized in that: in the fifth step, the volume space velocity of the carbon dioxide gas is 8000-10000 h -1 。
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