CN111232953B - Device and method for converting volatile organic compounds into nano-carbon products - Google Patents
Device and method for converting volatile organic compounds into nano-carbon products Download PDFInfo
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- CN111232953B CN111232953B CN202010095648.7A CN202010095648A CN111232953B CN 111232953 B CN111232953 B CN 111232953B CN 202010095648 A CN202010095648 A CN 202010095648A CN 111232953 B CN111232953 B CN 111232953B
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Abstract
The invention discloses a device and a method for converting volatile organic compounds into nanocarbon products, wherein the device comprises a fluidized bed section at the lower section, a fixed bed section at the upper section, a cyclone separator at the upper part of the fixed bed section, inlets of the volatile organic compounds, water vapor and a catalyst, and outlets of carbon products and gas products; the method comprises the step of filling nano metal supported catalysts with different particle sizes in a fluidized bed section and a fixed bed section respectively. By external heating, conversion energy is provided. The solid (catalyst and carbon product) in the fluidized bed section passes through the solid channel of the fixed bed section together with the gas to supply heat to the fixed bed section; the solid returns to the fluidized bed section through a cyclone separator at the upper part of the fixed bed section; and introducing water vapor below the fixed bed section to control the fixed bed section not to deposit carbon. By utilizing the method, the volatile organic compounds are efficiently converted and directly discharged, and the additional value of the prepared carbon nano material is high. Has the advantages of compact equipment structure, small investment and easy amplification.
Description
Technical Field
The invention relates to the technical field of volatile organic compound conversion, in particular to a device and a method for converting volatile organic compounds into nanocarbon products.
Background
Volatile organic compounds are a particularly large type in waste gas and have the characteristics of complex components, low content and large environmental impact effect. Current methods for treating volatile organic compounds include pre-cooling followed by enrichment by absorption or adsorption. Part of the volatile organics can become liquid after enrichment. A small amount of liquid with simple components can be recycled as a product. However, most of the liquid components are complex and difficult to separate continuously, and can only be reprocessed by incineration or catalytic oxidation. In addition, there are also volatile components with very low boiling points, often in gaseous form, which still have the potential to continue to be vented to the atmosphere. So that it can be changed into carbon dioxide and water only by means of incineration or catalytic oxidation. A large amount of fuel is needed in the incineration process, expensive reagents or catalysts are needed in the catalytic oxidation, and the product has no added value and is unfavorable in economic aspect.
The volatile organic compound can be used as a raw material for preparing carbon nano materials (carbon nano tubes or graphene and carbon nano fibers). The products have large specific surface area, good electrical conductivity, thermal conductivity, mechanical strength and the like, and have good application in the aspects of composite materials, catalysts, adsorbing materials and energy storage and high added value. However, in many published reports, only quality, structure and purity control of carbon products is concerned, and conversion efficiency of carbon sources is rarely concerned. For example, in the production process of carbon nanotubes used as a conductive agent of a lithium ion battery, the conversion rate of the carbon source rarely exceeds 80%. By using the method, even if the enriched volatile organic compounds are changed into carbon products, the tail gas still belongs to the volatile organic compounds and does not meet the emission standard.
Generally, the concentration of the enriched volatile organic compounds is 0.1-100%, and the total hydrocarbon content except methane in the discharged gas after conversion is required not to exceed 50-100mg/Nm3. This corresponds to a conversion efficiency of more than 99.99%, even 99.999%, of the volatile organic compounds in the reaction apparatus. Obviously, the current technology is not satisfactory.
In addition, the volatile organic compound is an industry with large processing capacity, and the scale of the volatile organic compound is much larger than that of the current carbon nano material preparation industry. Therefore, a complex engineering problem is generated, namely the reaction device needs to meet the requirements of continuous conversion and standard conversion all the time. The technology has not been reported.
Disclosure of Invention
Aiming at the defects of the conventional volatile organic compound treatment method and the defects of a carbon nano material preparation technology, the invention provides a device and a method for converting volatile organic compounds into nano carbon products.
In order to achieve the purpose, the invention adopts the following technical scheme:
a device for converting volatile organic compounds into nanocarbon products is characterized in that the lower section of the device is a fluidized bed section 1, the upper section of the device is a fixed bed section 2, a cyclone separator 3 is arranged at the upper part in the fixed bed section, and an outlet of the cyclone separator 3 is communicated with the fluidized bed section 1; a steam jet pipe 4 is arranged below the fixed bed section 2; the bottom of the fluidized bed section 1 is provided with a volatile organic compound inlet 5, the top of the fixed bed section 2 is provided with a gas product outlet 6, the fluidized bed section 1 is provided with a fluidized bed section catalyst inlet 7 and a carbon product outlet 8, and the fixed bed section 2 is provided with a fixed bed section catalyst inlet 9.
The fixed bed section 2 is provided with a plurality of solid channels, so that the solid can reach the upper part of the fixed bed section, the solid channels account for 5-20% of the cross section of the bed layer, and the rest bed layers are filled with catalysts; the solid channels in the fixed bed section are serpentine channels to ensure that the gas can effectively contact the catalyst in the fixed bed section.
The number of the water vapor injection pipes 4 is one or more, and the openings of the water vapor injection pipes are downward.
The height of the fluidized bed section 1 is 1-3 times of the height of the fixed bed section 2.
The catalyst in the fluidized bed section 1 and the fixed bed section 2 is a nano metal supported catalyst, the metal component of the catalyst is one or more of Fe, Co, Ni, W, Cu, Mo and Mn, and the grain size is 1-20 nm; the carrier is one or more of alumina, silica, zirconia and magnesia, the mass fraction of the carrier is 10-90%, and the rest is metal; the nano metal-supported catalyst used in the fluidized bed section 1 has an average particle diameter of 0.05 to 0.5 mm, and the nano metal-supported catalyst used in the fixed bed section 2 has an average diameter of 2 to 10 mm.
The method for converting volatile organic compounds into nano carbon products by the device comprises the following steps:
step 1: filling the catalyst into the fluidized bed section 1 and the fixed bed section 2 through a fluidized bed section catalyst inlet 7 and a fixed bed section catalyst inlet 9 respectively, heating the device to 500-1000 ℃, and controlling the absolute pressure of the gas product outlet (6) to be 0.1-2 MPa;
step 2: volatile organic matter gas is introduced from a volatile organic matter inlet 5 at the bottom of the fluidized bed section 1, and the volatile organic matter gas is cracked on a catalyst in the fluidized bed section 1 to generate a carbon product, methane and hydrogen;
and step 3: the carbon product moves upwards along with the volatile organic compound gas, methane and hydrogen, passes through the fixed bed section 2, and the volatile organic compound gas contacts with the catalyst in the fixed bed section 2 to continue to react;
and 4, step 4: opening a water vapor injection pipe 4, and introducing water vapor accounting for 1-10% of the total mass of the volatile organic gas; after being sprayed downwards, the water vapor can automatically turn over and move upwards, enters the fixed bed section 2, and reacts with volatile organic gas and carbon products on the catalyst; total non-methane in the final gas productHydrocarbons less than 50mg/Nm3The gas product is separated by the cyclone separator 3 and discharged through a gas product outlet 6 after reaching the standard; the spraying of the water vapor ensures that the catalyst on the fixed bed section 2 does not deposit carbon and can be used for a long time;
and 5: the carbon product passes through a solid channel in the fixed bed section 2 and enters the cyclone separator 3 at the upper part, and the carbon product is separated by the cyclone separator 3 and then returns to the fluidized bed section 1;
when the carbon product of the fluidized bed section 1 is excessive, the carbon product is discharged out of the device through a carbon product outlet 8; and fresh catalyst is added through a fluidized bed section catalyst inlet 7; the above process is repeated.
The volatile organic gas is 0.01-90 wt% of organic gas with molecular weight of 26-150, and the balance is inert gas; in the conversion process, the space velocity of the volatile organic gas is 0.1-20 g/gcat/h.
The inert gas is one or more of nitrogen, argon and water vapor.
The carbon product is one or more of carbon nano tube, graphene and carbon nano-fiber.
Compared with the prior art, the invention has the following advantages:
(1) the fluidized bed and the fixed bed with high porosity are integrated together, so that the requirement of high conversion rate of volatile organic compounds is met, and the requirement of solid volume expansion is met. At the same time, the high pressure drop of the conventional fixed bed section is avoided, which is not achieved by any single device. Can save power consumption by 10-20%.
(2) The steam is introduced, so that the catalyst in the fixed bed section is not deposited with carbon and does not need to be cleaned, the time for dismounting is saved, the time for continuous operation of the device is improved, and the operation cost is saved by 5-10%.
(3) The high-temperature gas and the high-temperature solid in the fluidized bed section are used for heating the catalyst in the fixed bed section, the defect of poor heat transfer effect of the fixed bed catalyst bed layer is overcome, and 80-90% of energy can be saved.
Drawings
FIG. 1 is a schematic diagram of an apparatus for converting volatile organic compounds into nanocarbon products according to the present invention.
Wherein 1, a fluidized bed section; 2. a fixed bed section (black is the catalyst zone; white is the solid channel); 3. a cyclone separator; 4. a water vapor injection pipe; 5. a volatile organic inlet; 6. a gaseous product outlet; 7. a fluidized bed section catalyst inlet; 8. a carbon product outlet; 9. and a catalyst inlet of the fixed bed section.
Detailed Description
The present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments, including but not limited to the following examples and effects.
Example 1
An apparatus as shown in FIG. 1 is used in which the height of the fluidized bed section 1 is 2 times the height of the fixed bed section 2. The solid channels of the fixed bed section occupy 20% of the bed cross section. A steam injection pipe 4 (opening downwards) is arranged below the fixed bed section 2.
The nano metal supported catalyst (90% Fe-10% alumina, 1-6nm grain) with an average particle size of 0.05 mm was charged into the fluidized bed section 1 through the fluidized bed section catalyst inlet 7. A nano metal-supported catalyst (50% Ni-50% silica, 5-15nm in crystal grain) having an average diameter of 10 mm was charged into the fixed bed section 2 through the fixed bed section catalyst inlet 9. The apparatus was heated to 500 ℃ and the absolute pressure at the gaseous product outlet 6 was controlled to 0.5 MPa.
Volatile organic gas (volatile organic gas composition: 0.01% of organic gas with molecular weight of 26-100, 1% of water vapor, and the balance of nitrogen) is introduced from a volatile organic gas inlet 5 at the bottom of the fluidized bed section 1. In the conversion process, the space velocity of the volatile organic compound gas is 0.1g/gcat/h, and carbon products (carbon nano tubes) and products such as methane, hydrogen and the like are generated by cracking on the catalyst. The carbon product moves upward with the gas (volatile organic gas, methane and hydrogen) and passes through the fixed bed section 2, and the volatile organic gas contacts the catalyst in the fixed bed section 2 to continue the reaction.
The steam injection pipe 4 is opened, and steam accounting for 1 percent of the total mass of the volatile organic compound gas is introduced. After the water vapor is sprayed downwards, the water vapor can automatically turn back and move upwards to enter the fixing deviceThe bed section 2 is fixed and reacts with volatile organic compound gas and carbon products on the catalyst. The total non-methane hydrocarbons in the final gas is less than 10mg/Nm3The gas product is separated by the cyclone 3 and discharged through the gas product outlet 6. The spraying of the water vapor enables the catalyst on the fixed bed section 2 not to deposit carbon and to be used for a long time.
The carbon product passes through the solid passage in the fixed bed section 2, enters the cyclone 3 at the upper part, and is returned to the fluidized bed section 1 after being separated by the cyclone 3.
When the carbon product of the fluidized bed section 1 is excessive, the carbon product is discharged out of the device through a carbon product outlet 8; and fresh catalyst is added through a fluidized bed section catalyst inlet 7; the above process is repeated.
Example 2
An apparatus as shown in FIG. 1 was used in which the height of the fluidized bed section 1 was 3 times the height of the fixed bed section 2. The solid channels of the fixed bed section occupy 5% of the bed cross section. Two steam injection pipes 4 (open downwards) are arranged in the lower part of the fixed bed section 2.
A nano-metal supported catalyst (8% Fe-2% Co-90% silica, 3-7nm in grain size) having an average particle size of 0.5 mm was charged into the fluidized bed section 1 through the fluidized bed section catalyst inlet 7. A nano metal-supported catalyst (5% Fe-5% Co-5% Cu-85% zirconia, crystal grains of 2-10nm) having an average diameter of 2 mm was charged into the fixed bed section 2 through the fixed bed section catalyst inlet 9. The apparatus was heated to 1000 ℃ and the absolute pressure at the product gas outlet 6 was controlled to 2 MPa.
Volatile organic gas (volatile organic gas composition: 30% of organic gas with molecular weight of 80-150, 70% of nitrogen) is introduced from a volatile organic inlet 5 at the bottom of the fluidized bed section 1. In the conversion process, the space velocity of the volatile organic compound gas is 15g/gcat/h, and the volatile organic compound gas is cracked on a catalyst to generate carbon products (90% of carbon nano tubes and 10% of carbon nano fibers) and products such as methane, hydrogen and the like. The carbon product moves upward with the gas (volatile organic gas, methane and hydrogen) and passes through the fixed bed section 2, and the volatile organic gas contacts the catalyst in the fixed bed section 2 to continue the reaction.
The steam injection pipe 4 is opened, and steam accounting for 10 percent of the total mass of the volatile organic compound gas is introduced. After being sprayed downwards, the water vapor can automatically turn over and move upwards, enters the fixed bed section 2, and reacts with volatile organic gas and carbon products on the catalyst. The total non-methane hydrocarbons in the final gas is less than 20mg/Nm3The gas product is separated by the cyclone 3 and discharged through the gas product outlet 6. The spraying of the water vapor enables the catalyst on the fixed bed section 2 not to deposit carbon and to be used for a long time.
The carbon product passes through the solid passage in the fixed bed section 2, enters the cyclone 3 at the upper part, and is returned to the fluidized bed section 1 after being separated by the cyclone 3.
When the carbon product of the fluidized bed section 1 is excessive, the carbon product is discharged out of the device through a carbon product outlet 8; and fresh catalyst is added through a fluidized bed section catalyst inlet 7; the above process is repeated.
Example 3
An apparatus as shown in FIG. 1 is used in which the height of the fluidized bed section 1 is 3 times the height of the fixed bed section 1.5. The solid channels of the fixed bed section occupy 15% of the bed cross section. Two steam injection pipes 4 (open downwards) are arranged in the lower part of the fixed bed section 2.
A nano metal supported catalyst (30% Fe-20% Cu-5% Mn-45% magnesium oxide, crystal grain 5-15nm) with an average particle size of 0.1-0.3 mm is loaded into the fluidized bed section 1 through a fluidized bed section catalyst inlet 7. A nano metal supported catalyst (20% Ni-5% Mn-5% W-70% zirconia, crystal grain 3-20nm) having an average diameter of 3-5 mm was charged into the fixed bed section 2 through the fixed bed section catalyst inlet 9. The apparatus was heated to 800 ℃ and the absolute pressure at the gaseous product outlet 6 was controlled to 0.1 MPa.
Volatile organic gas (volatile organic gas composition: 30% of organic gas with molecular weight of 78-102, 2% of water vapor, and the balance of nitrogen) is introduced from a volatile organic inlet 5 at the bottom of the fluidized bed section 1. In the conversion process, the space velocity of the volatile organic compound gas is 1.3g/gcat/h, and the volatile organic compound gas is cracked on a catalyst to generate carbon products (90% of graphene and 10% of carbon nanotubes) and products such as methane, hydrogen and the like. The carbon product moves upward with the gas (volatile organic gas, methane and hydrogen) and passes through the fixed bed section 2, and the volatile organic gas contacts the catalyst in the fixed bed section 2 to continue the reaction.
The steam injection pipe 4 is opened, and steam accounting for 3 percent of the total mass of the volatile organic compound gas is introduced. After being sprayed downwards, the water vapor can automatically turn over and move upwards, enters the fixed bed section 2, and reacts with volatile organic gas and carbon products on the catalyst. The total non-methane hydrocarbons in the final gas is less than 50mg/Nm3The gas product is separated by the cyclone 3 and discharged through the gas product outlet 6. The spraying of the water vapor enables the catalyst on the fixed bed section 2 not to deposit carbon and to be used for a long time.
The carbon product passes through the solid passage in the fixed bed section 2, enters the cyclone 3 at the upper part, and is returned to the fluidized bed section 1 after being separated by the cyclone 3.
When the carbon product of the fluidized bed section 1 is excessive, the carbon product is discharged out of the device through a carbon product outlet 8; and fresh catalyst is added through a fluidized bed section catalyst inlet 7; the above process is repeated.
Example 4
An apparatus as shown in FIG. 1 is used in which the height of the fluidized bed section 1 is 1 times the height of the fixed bed section 2. The solid channels of the fixed bed section occupy 10% of the bed cross section. Five steam injection pipes 4 (open downwards) are arranged in the lower part of the fixed bed section 2.
A nano metal supported catalyst (50% Fe-2% Mo-48% alumina, 5-10nm grain size) with an average particle size of 0.05-0.3 mm was charged into the fluidized bed section 1 through the fluidized bed section catalyst inlet 7. A nano metal supported catalyst (29% Ni-1% Mo-70% silica, crystal grain 4-18nm) having an average diameter of 4-8 mm was charged into the fixed bed section 2 through the fixed bed section catalyst inlet 9. The apparatus was heated to 700 ℃ and the absolute pressure at the gaseous product outlet 6 was controlled to 0.4 MPa.
Volatile organic gas (volatile organic composition: 5% of organic substance with molecular weight of 26-80, 70% of nitrogen, 20% of argon, 5% of water vapor) is introduced from a volatile organic inlet 5 at the bottom of the fluidized bed section 1. In the conversion process, the space velocity of the volatile organic compound gas is 4g/gcat/h, and the volatile organic compound gas is cracked on a catalyst to generate carbon products (5 percent of carbon nano fibers and 95 percent of carbon nano tubes), methane, hydrogen and other products. The carbon product moves upward with the gas (volatile organic gas, methane and hydrogen) and passes through the fixed bed section 2, and the volatile organic gas contacts the catalyst in the fixed bed section 2 to continue the reaction.
The steam injection pipe 4 is opened, and steam accounting for 8 percent of the total mass of the volatile organic compound gas is introduced. After being sprayed downwards, the water vapor can automatically turn over and move upwards, enters the fixed bed section 2, and reacts with volatile organic gas and carbon products on the catalyst. The total non-methane hydrocarbons in the final gas is less than 40mg/Nm3The gas product is separated by the cyclone 3 and discharged through the gas product outlet 6. The spraying of the water vapor enables the catalyst on the fixed bed section 2 not to deposit carbon and to be used for a long time.
The carbon product passes through the solid passage in the fixed bed section 2, enters the cyclone 3 at the upper part, and is returned to the fluidized bed section 1 after being separated by the cyclone 3.
When the carbon product of the fluidized bed section 1 is excessive, the carbon product is discharged out of the device through a carbon product outlet 8; and fresh catalyst is added through a fluidized bed section catalyst inlet 7; the above process is repeated.
Claims (9)
1. A device for converting volatile organic compounds into nanocarbon products is characterized in that the lower section of the device is a fluidized bed section (1), the upper section of the device is a fixed bed section (2), a cyclone separator (3) is arranged at the upper part in the fixed bed section, and the outlet of the cyclone separator (3) is communicated with the fluidized bed section (1); a steam jet pipe (4) is arranged below the fixed bed section (2); a volatile organic compound inlet (5) is arranged at the bottom of the fluidized bed section (1), a gas product outlet (6) is arranged at the top of the fixed bed section (2), a fluidized bed section catalyst inlet (7) and a carbon product outlet (8) are arranged on the fluidized bed section (1), and a fixed bed section catalyst inlet (9) is arranged on the fixed bed section (2); the fixed bed section (2) is provided with a plurality of solid channels, so that the solid can reach the upper part of the fixed bed section, the solid channels account for 5-20% of the cross section of the bed layer, and the rest bed layers are filled with the catalyst.
2. The apparatus for converting volatile organic compounds into nanocarbon products as claimed in claim 1, wherein the solid channels in the fixed bed section are zigzag channels to ensure effective contact of the gas with the catalyst in the fixed bed section.
3. The apparatus for converting volatile organic compounds into nanocarbon products as claimed in claim 1, wherein the number of the water vapor injection pipes (4) is one or more, and the openings of the water vapor injection pipes are downward.
4. An apparatus for converting volatile organic compounds into nanocarbon products as claimed in claim 1, wherein the height of the fluidized bed section (1) is 1 to 3 times the height of the fixed bed section (2).
5. The apparatus for converting volatile organic compounds into nanocarbon products according to claim 1, wherein the catalyst in the fluidized bed section (1) and the fixed bed section (2) is a nano metal supported catalyst, the metal component of the nano metal supported catalyst is one or more of Fe, Co, Ni, W, Cu, Mo and Mn, and the crystal grain is 1-20 nm; the carrier is one or more of alumina, silica, zirconia and magnesia, the mass fraction of the carrier is 10-90%, and the rest is metal; the nano metal supported catalyst used in the fluidized bed section (1) has an average particle diameter of 0.05 to 0.5 mm, and the nano metal supported catalyst used in the fixed bed section (2) has an average diameter of 2 to 10 mm.
6. A method for converting volatile organic compounds into nanocarbon products by using the device of any one of claims 1 to 5, characterized by the following steps:
step 1: filling the catalyst into the fluidized bed section (1) and the fixed bed section (2) respectively through a fluidized bed section catalyst inlet (7) and a fixed bed section catalyst inlet (9), heating the device to 500-1000 ℃, and controlling the absolute pressure of the gas product outlet (6) to be 0.1-2 MPa;
step 2: volatile organic matter gas is introduced from a volatile organic matter inlet (5) at the bottom of the fluidized bed section (1), and the volatile organic matter gas is cracked on a catalyst in the fluidized bed section (1) to generate a carbon product, methane and hydrogen;
and step 3: the carbon product moves upwards along with the volatile organic compound gas, methane and hydrogen, passes through the fixed bed section (2), and the volatile organic compound gas contacts with the catalyst in the fixed bed section (2) to continue to react;
and 4, step 4: opening a steam jet pipe (4), and introducing steam accounting for 1-10% of the total mass of the volatile organic gas; after being sprayed downwards, the water vapor can automatically turn over and move upwards, enters the fixed bed section (2), and reacts with volatile organic gas and carbon products on the catalyst; the final gas product has less than 50mg/Nm of non-methane total hydrocarbons3The gas product is separated by the cyclone separator (3) and discharged through a gas product outlet (6) after reaching the standard; the spraying of the water vapor ensures that the catalyst on the fixed bed section (2) does not deposit carbon and can be used for a long time;
and 5: the carbon product passes through a solid channel in the fixed bed section (2) and enters the cyclone separator (3) at the upper part, and the carbon product is separated by the cyclone separator (3) and then returns to the fluidized bed section (1);
when the carbon product of the fluidized bed section (1) is excessive, discharging the carbon product out of the device through a carbon product outlet (8); and fresh catalyst is added through a fluidized bed section catalyst inlet (7); the above process is repeated.
7. The method according to claim 6, wherein the volatile organic gas is 0.01-90 wt% of organic gas with molecular weight of 26-150, and the rest is inert gas; in the conversion process, the space velocity of the volatile organic gas is 0.1-20 g/gcat/h.
8. The method of claim 7, wherein the inert gas is one or more of nitrogen, argon and water vapor.
9. The method of claim 6, wherein the carbon product is one or more of carbon nanotubes, graphene and carbon nanofibers.
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| CN1327943A (en) * | 2001-05-25 | 2001-12-26 | 清华大学 | Process and reactor for continuously preparing nm carbon tubes with fluidized bed |
| CN2728602Y (en) * | 2004-09-28 | 2005-09-28 | 中国科学院广州地球化学研究所 | High efficiency flowing type photocatalytic reaction for treating volatile organic matter in air |
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| CN109715269A (en) * | 2016-10-14 | 2019-05-03 | 黄华丽 | A kind of purifying agent for harmful gases and its preparation and purification method |
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| US9687802B2 (en) * | 2011-04-04 | 2017-06-27 | Lg Chem, Ltd. | Apparatus and method for continuously producing carbon nanotubes |
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| CN1327943A (en) * | 2001-05-25 | 2001-12-26 | 清华大学 | Process and reactor for continuously preparing nm carbon tubes with fluidized bed |
| CN2728602Y (en) * | 2004-09-28 | 2005-09-28 | 中国科学院广州地球化学研究所 | High efficiency flowing type photocatalytic reaction for treating volatile organic matter in air |
| CN101959793A (en) * | 2008-03-07 | 2011-01-26 | 日立化成工业株式会社 | Carbon nano-tube manufacturing method and carbon nano-tube manufacturing apparatus |
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