CN212246905U - Low-temperature plasma catalytic reaction device - Google Patents
Low-temperature plasma catalytic reaction device Download PDFInfo
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- CN212246905U CN212246905U CN202020194079.7U CN202020194079U CN212246905U CN 212246905 U CN212246905 U CN 212246905U CN 202020194079 U CN202020194079 U CN 202020194079U CN 212246905 U CN212246905 U CN 212246905U
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- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000010453 quartz Substances 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000003197 catalytic effect Effects 0.000 claims abstract description 8
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- 239000010935 stainless steel Substances 0.000 claims description 16
- 229910001220 stainless steel Inorganic materials 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 11
- 239000010949 copper Substances 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000002808 molecular sieve Substances 0.000 claims description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical group [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 239000004809 Teflon Substances 0.000 claims 1
- 229920006362 Teflon® Polymers 0.000 claims 1
- 239000000376 reactant Substances 0.000 abstract description 12
- 239000000571 coke Substances 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 150000003254 radicals Chemical class 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 44
- 239000012263 liquid product Substances 0.000 description 10
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 description 8
- 230000006872 improvement Effects 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000002775 capsule Substances 0.000 description 5
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- 229910045601 alloy Inorganic materials 0.000 description 4
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- 239000007769 metal material Substances 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
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- 239000005977 Ethylene Substances 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000001994 activation Methods 0.000 description 2
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- 238000007142 ring opening reaction Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 238000000678 plasma activation Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
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Abstract
The utility model relates to a low-temperature plasma catalytic reaction device, which comprises a quartz tube, a high-voltage electrode which is arranged at the axis of the quartz tube and is coaxial with the quartz tube, and a counter electrode arranged outside the quartz tube; raw materials enter the reaction tube through a top flange and are sealed by a sealing ring; the electrode connector is arranged at the axis of the top flange and is used for connecting a high-voltage electrode and the output end of a high-frequency high-voltage power supply; the product after reaction is condensed and collected from a bottom flange; the catalyst layer is completely arranged in the plasma area and is supported by the support body; when the plasma generator works, low-temperature plasma is generated by dielectric barrier discharge, and required discharge voltage is provided by an alternating-current high-voltage high-frequency power supply. The utility model discloses can utilize plasma to activate gaseous alkane, carbon dioxide and other reactants into the free radical under low temperature and atmospheric pressure, react under the effect of catalyst and generate liquid chemicals. Compared with the traditional thermal catalytic device, the utility model has the advantages of high conversion rate, high liquid yield and low coke yield.
Description
Technical Field
The utility model belongs to the technical field of chemical industry, energy and environmental protection, concretely relates to low temperature plasma catalytic reaction device, it can realize alkane (C) under low temperature and ordinary pressure1-C5Monomer or twoMixtures of species and above), CO2And other reactants into liquid high value-added chemicals.
Background
At present, biogas, natural gas and liquefied petroleum gas are mainly used for house heating, cooking and power generation, but the huge reserves and the output far exceed the demands of the market, so that the conversion of the cheap and easily available resources into high-value-added liquid chemicals becomes a hot spot of current research. Conventional thermocatalytic reaction devices include kettle reactors, fixed bed reactors, fluidized bed reactors, and the like, which primarily employ oxidative or non-oxidative means to convert reactants into syngas, ethane and ethylene, methanol or other oxygenates, and aromatics, and the like. Since these reactions are difficult to perform at low temperatures, conventional thermocatalytic reactors tend to use high temperatures to promote the reaction, resulting in severe coke formation (up to 30% yield) and lower liquid product yields: (<25%). Microwave-assisted heated catalytic reactors are also used to convert these inexpensive and readily available resources, such as methane to ethane and ethylene or syngas and H2Etc., but still fails to solve the serious coke and energy efficiency problems.
Low temperature plasma technology is a promising technology that can facilitate thermodynamically unfavorable chemical reactions at relatively low temperatures. The low temperature plasma generates high energy electrons by applying a high voltage electric field, and the typical electron temperature is 1-10 eV. When the reactant enters the plasma region, the reactant can convert inert molecules into an excited state through ionization, vibration and rotation excitation and the form of free radicals under the action of high-energy electrons, so that various chemical reactions are initiated by overcoming high thermodynamic energy barriers. The utility model discloses combine together low temperature plasma and catalyst, the activation of coupling plasma and the selective catalytic reaction of catalyst and produce synergistic effect, realize high conversion, high liquid product yield and low coke yield.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a low temperature plasma catalytic reaction device.
The utility model discloses a following technical scheme realizes:
a low-temperature plasma catalytic reaction device comprises a quartz tube, a high-voltage electrode, a counter electrode and a gas-liquid separator, wherein one end of the high-voltage electrode is arranged at the axis of the quartz tube and is coaxial with the quartz tube, and the other end of the high-voltage electrode extends out of the quartz tube and is tightly wound on the outer side of the quartz tube; wherein,
the upper end of the quartz tube is sealed by a top flange and a sealing ring, and is provided with a gas inlet and a liquid inlet, and the electrode connector is arranged at the axis of the top flange and is used for connecting a high-voltage electrode and the output end of an alternating-current high-frequency high-voltage power supply; a bottom flange at the lower end of the quartz tube is sealed with a sealing ring and is provided with a product outlet;
the catalyst layer and the support body are arranged in the quartz tube, and the catalyst layer is supported by the support body in the quartz tube and is completely arranged in the plasma area; the quartz tube and the plasma region are used for being arranged in the heating furnace; when the plasma generator works, low-temperature plasma is generated by dielectric barrier discharge, and required discharge voltage is provided by an alternating-current high-voltage high-frequency power supply.
The utility model discloses further improvement lies in, and the mains voltage for producing low temperature plasma is 1-1000kV, and alternating current frequency is 5-100 kHz.
The further improvement of the utility model lies in that the distance between the discharge gap, namely the high-voltage electrode, and the inner wall of the quartz tube is 1-10 mm.
The further improvement of the utility model is that the catalyst is a molecular sieve or oxide which is loaded or not loaded with metal, and the oxide is SiO2，Al2O3，TiO2Or ZrO2。
The utility model discloses further improvement lies in, and the quartz capsule can be replaced for the ceramic reaction pipe.
The utility model discloses further improvement lies in, and the material of top flange and bottom flange is polytetrafluoroethylene, pottery, or stainless steel.
The utility model discloses further improvement lies in, high-voltage electrode's material is iron, copper or stainless steel.
The utility model discloses further improvement lies in, and the material of counter electrode is iron, copper or stainless steel.
The utility model discloses at least, following profitable technological effect has:
the utility model discloses combine together low temperature plasma and catalyst, thereby coupling plasma activation and catalyst catalytic reaction produce synergistic effect, realize high conversion, high liquid product yield and low coke productivity. Compared with the traditional thermal catalytic reaction device, the novel low-temperature plasma catalytic reaction device can greatly improve the conversion rate of methane, and the conversion rate of pure methane can reach about 30% at low temperature and normal pressure. Under the condition of loading the catalyst, the novel low-temperature plasma catalytic reaction device can obviously improve the yield of converting methane, natural gas or liquefied petroleum gas into liquid products with high added values, and the yield of the liquid products can be improved to more than 50%. Meanwhile, the coke production rate can be greatly reduced and can be controlled to be about 5 percent.
Drawings
Fig. 1 is a schematic view of a low-temperature plasma catalytic reaction apparatus of the present invention.
FIG. 2 is a schematic view of a process flow of a low temperature plasma catalytic reaction of the present invention.
Description of reference numerals:
1-sealing ring, 2-quartz tube, 3-counter electrode, 4-catalyst layer, 5-top flange, 6-high voltage electrode, 7-support, 8-bottom flange, 9-heating furnace, 10-electrode connector, 11-multifunctional oscilloscope, 12-high voltage detector, 13-stainless steel mesh enclosure, 14-current detector, 15-liquid product collector, 16-high voltage high frequency power supply, 17-high voltage electrode a, 18-mixer, 19-quartz tube, 20-low voltage electrode, 21-soap bubble flowmeter, 22-gas chromatography.
Detailed Description
The catalytic reaction apparatus of the present invention will be described in further detail with reference to the accompanying drawings and examples.
The utility model provides a more effectively from the cheap reaction unit who easily obtains the liquid chemical of high added value of the resource. As shown in FIG. 1, the utility model provides a pair of low temperature plasma catalytic reaction device, its main unit mainly is the quartz capsule of making by dielectric material, 2 axle centers of quartz capsule department and with the coaxial stainless steel high voltage electrode 6 of quartz capsule, closely twine the copper coil in the quartz capsule outside and constitute for counter electrode 3. The upper end of the quartz tube is sealed by a top flange 5 and a sealing ring 1, and an electrode connector 10 is arranged at the axis of the top flange and is used for connecting a high-voltage electrode and the output end of an alternating-current high-frequency high-voltage power supply. The lower end of the quartz tube is sealed by a bottom flange 8 and a sealing ring. The length of the copper coil wound around the outer wall of the quartz tube determines the length of the low temperature plasma region, and the catalyst layer 4 is inside the quartz tube and supported by the support body 7 and completely placed inside the plasma region. The quartz tube and the plasma region may be placed in a heating furnace 9 to be heated to a prescribed temperature. When the plasma generator works, low-temperature plasma is generated by dielectric barrier discharge, and required high-voltage is provided by an alternating-current high-voltage high-frequency power supply.
In addition, the material of the reaction tube may be quartz, ceramic or other dielectric materials. The power supply voltage for generating low-temperature plasma is 1-1000kV, and the alternating current frequency is 5-100 kHz. The distance between the discharge gap, i.e. the high-voltage electrode, and the inner wall of the quartz tube is 1-10 mm. The catalyst is a molecular sieve or oxide with or without metal, and the oxide is SiO2，Al2O3，TiO2Or ZrO2. The top flange 5 and the bottom flange 8 are made of polytetrafluoroethylene, ceramic or stainless steel. The high-voltage electrode is made of oxidation-resistant conductive metal materials such as stainless steel, copper, alloy and the like. The counter electrode is made of conductive metal materials such as stainless steel, copper, alloy and the like.
Referring to fig. 2, a process flow diagram of a low-temperature plasma catalytic reaction is shown, after reactants (gas or liquid vapor) are mixed thoroughly and uniformly by a mixer 18, the reactants are introduced into the quartz tube from a top flange at the upper end of the quartz tube 19 and enter a catalyst bed and a plasma region. The high voltage electrode a17 is made of stainless steel, and the low voltage electrode 20 is composed of a copper coil wound on the outer side of the quartz tube. The power supply for generating the plasma body is a high-voltage high-frequency alternating current power supply 16, and the voltage and the current in the plasma reaction process are respectively measured by a high-voltage detector 12 and a current detector 14 in real time and displayed on a multifunctional oscilloscope 11 so as to monitor the current and voltage conditions in the reaction process in real time. The reactant is activated into free radicals under the action of plasma, and then liquid products with high added values are selectively generated under the action of a catalyst. The liquid product exits the lower end of the quartz tube and is collected by condensation in a liquid product collector 15. The stainless steel mesh enclosure 13 serves to shield the entire quartz tube and plasma region to increase the operational safety of the reactor. The composition and flow of the reacted gas product are analyzed and detected by gas chromatography 22 and bubble flowmeter 21, respectively.
In the device of the utility model, the power voltage for generating plasma is 1-1000kV, and the alternating current frequency is 5-100 kHz. The low-temperature plasma discharge gap (the distance between the high-voltage electrode and the inner wall of the quartz tube) is 1-10 mm. The catalyst is a molecular sieve or oxide (SiO) with or without metal loading2，Al2O3，TiO2，ZrO2) And the like. The material of the reaction tube can be quartz, ceramic and other dielectric materials. The top flange and the bottom flange are made of polytetrafluoroethylene, ceramics, stainless steel and the like. The high-voltage electrode is made of oxidation-resistant conductive metal materials such as stainless steel, copper, alloy and the like. The counter electrode is made of conductive metal materials such as stainless steel, copper, alloy and the like.
Example 1: conversion effect of low-temperature plasma of methane under different power supply frequencies and output voltages/powers without catalyst
TABLE 1 Effect of reaction time on Low temperature plasma conversion of methane at the same frequency and output
TABLE 2 methane conversion performance of low temperature plasma at the same power frequency and different voltage/power
TABLE 3 conversion Performance of low temperature plasma to methane at different power frequencies and different voltages/powers
TABLE 4 conversion Performance of low temperature plasma to methane at different power frequencies and different voltages/powers
As can be seen from tables 1 to 4, the product of methane tends to be stable after 30 or 60 minutes of low temperature plasma reaction. The temperature of the inner and outer surfaces of the quartz tube was measured by a thermocouple and the reaction temperature was below 150 ℃, indicating that the activation and conversion of methane was caused by low temperature plasma rather than thermal decomposition. In the absence of catalyst, the main product of the simple methane conversion is H2And ethane. The yields of propane and butane were very low, 0.9-1.4% and 1.7-2.5%, respectively, and no liquid product formation was observed. Compare with traditional thermal catalysis, under the same temperature the utility model discloses reaction unit makes the conversion rate of methane improve 17-35% greatly, and methane conversion rate is relevant with power output or frequency. High output power or frequency increases methane conversion but also favors coke formation, resulting in severe carbon loss. Lower output power (e.g., 12W) and higher frequency (e.g., 25KHz) help to improve hydrocarbon production.
Example 2: conversion of methane and methylnaphthalene in the presence of a catalyst in a low temperature plasma catalytic reactor
TABLE 5 reactivity of methane and methylnaphthalene at the same voltage and different output frequencies/powers
As seen from table 5, as the frequency and output power increased, both the methane conversion and the mono-aromatic yield increased, and the coke formation decreased, probably because the higher output power increased the plasma intensity, thus enhancing the methylnaphthalene ring-opening reaction. Further increases in output yield more mono-aromatics, but the ring opening efficiency of methylnaphthalene decreases slightly, probably due to more coke formation.
Example 3 reaction Performance of different reactant systems in a Low temperature plasma catalytic reactor with catalyst loading
TABLE 6 reactivity of different reactant systems in a low temperature plasma catalyst reactor
Aiming at different reactant systems, such as methane, natural gas, liquefied petroleum gas and the like, the low-temperature plasma catalytic reaction device can convert the reactants into liquid chemicals with high added values, the produced coke amount is less, and the added value increment of cheap and easily-obtained resources is realized.
Claims (7)
1. A low-temperature plasma catalytic reaction device is characterized by comprising a quartz tube (2), a high-voltage electrode (6) with one end arranged at the axis of the quartz tube (2) and coaxial with the quartz tube, and a counter electrode (3) which is tightly wound outside the quartz tube, wherein the other end of the high-voltage electrode (6) extends out of the quartz tube (2); wherein,
the upper end of the quartz tube (2) is sealed by a top flange (5) and a sealing ring (1), and is provided with a gas inlet and a liquid inlet, and an electrode connector (10) is arranged at the axis of the top flange and is used for connecting a high-voltage electrode and the output end of an alternating-current high-frequency high-voltage power supply; a bottom flange (8) at the lower end of the quartz tube (2) is sealed with a sealing ring (1) and is provided with a product outlet;
a catalyst layer (4) and a support body (7) are arranged in the quartz tube (2), and the catalyst layer (4) is supported by the support body (7) in the quartz tube (2) and is completely arranged in the plasma region; the quartz tube (2) and the plasma region are used for being arranged in a heating furnace (9); when the plasma generator works, low-temperature plasma is generated by dielectric barrier discharge, and required discharge voltage is provided by an alternating-current high-voltage high-frequency power supply.
2. The apparatus of claim 1, wherein the distance between the discharge gap (i.e., the high voltage electrode) and the inner wall of the quartz tube is 1-10 mm.
3. The low-temperature plasma catalytic reactor as claimed in claim 1, wherein the catalyst carrier is molecular sieve or oxide, and the oxide is SiO2，Al2O3，TiO2Or ZrO2。
4. A low temperature plasma catalytic reaction device according to claim 1, characterized in that the quartz tube (2) can be replaced with a ceramic reaction tube.
5. A low temperature plasma catalytic reactor device according to claim 1, wherein the top flange (5) and the bottom flange (8) are made of teflon, ceramic, or stainless steel.
6. A low temperature plasma catalytic reactor as claimed in claim 1 wherein the high voltage electrode (6) is made of iron, copper or stainless steel.
7. A low temperature plasma catalytic reactor as claimed in claim 1 wherein the counter electrode (3) is of iron, copper or stainless steel.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118398475A (en) * | 2024-03-27 | 2024-07-26 | 青岛市产品质量检验研究院(青岛市产品质量安全风险监测中心) | Mass spectrum detection device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118398475A (en) * | 2024-03-27 | 2024-07-26 | 青岛市产品质量检验研究院(青岛市产品质量安全风险监测中心) | Mass spectrum detection device and method |
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Effective date of registration: 20240212 Address after: 710000, Building 8-N501, R&D Pilot Plant 8, Collaborative Innovation Port, Fengdong New City, Xi'an City, Shaanxi Province Patentee after: XI'AN SINO-GREEN HI-TECH Co.,Ltd. Country or region after: China Address before: 710086 8-n501, No.8 building, collaborative innovation port, Fengdong new town, Xi'an City, Shaanxi Province Patentee before: Shaanxi Huada Jiaoyang energy and Environmental Protection Development Group Co.,Ltd. Country or region before: China |