CN113634119A - Low-pressure carbon dioxide reduction device and manufacturing and using method thereof - Google Patents
Low-pressure carbon dioxide reduction device and manufacturing and using method thereof Download PDFInfo
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- CN113634119A CN113634119A CN202111016160.1A CN202111016160A CN113634119A CN 113634119 A CN113634119 A CN 113634119A CN 202111016160 A CN202111016160 A CN 202111016160A CN 113634119 A CN113634119 A CN 113634119A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 274
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 137
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 131
- 230000009467 reduction Effects 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 155
- 239000010453 quartz Substances 0.000 claims abstract description 87
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 87
- 239000003054 catalyst Substances 0.000 claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000007086 side reaction Methods 0.000 claims abstract description 11
- 238000006722 reduction reaction Methods 0.000 claims description 97
- 239000007789 gas Substances 0.000 claims description 89
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 47
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 10
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 10
- 238000007598 dipping method Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 230000000295 complement effect Effects 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 3
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- 238000000576 coating method Methods 0.000 claims description 3
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- 230000001699 photocatalysis Effects 0.000 abstract description 27
- 238000006555 catalytic reaction Methods 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 26
- 239000004408 titanium dioxide Substances 0.000 description 10
- 239000011941 photocatalyst Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
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- 239000012071 phase Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
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- 239000004215 Carbon black (E152) Substances 0.000 description 2
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- 239000002156 adsorbate Substances 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
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- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical group OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- 239000003638 chemical reducing agent Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/80—Type of catalytic reaction
- B01D2255/802—Photocatalytic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention provides a low-pressure carbon dioxide reduction device and a manufacturing and using method thereof, wherein the low-pressure carbon dioxide reduction device comprises a reaction cavity, a top reaction cavity wall or a side reaction cavity wall, a bottom reaction cavity wall, an air inlet, a reaction cavity barometer, a first air outlet and a second air outlet, the reaction cavity is of a closed cavity structure, the top reaction cavity wall arranged at the top of the reaction cavity is of a flat structure and is made of quartz materials, and the side reaction cavity wall arranged at the side of the reaction cavity is of a flat structure. The device is used for photocatalytic carbon dioxide reduction, and the catalytic reaction of the device is generated on the gas-solid interface of carbon dioxide and a catalyst, so that the photocatalytic efficiency can be enhanced, and the selectivity of the product can be improved.
Description
Technical Field
The invention belongs to the technical field of carbon neutralization, and particularly relates to a low-pressure carbon dioxide reduction device and a manufacturing and using method thereof, which are particularly suitable for the technical field of environment and the field of carbon dioxide resource utilization.
Background
The environmental problems and the energy shortage problems accompanied by rapid development of economy and rapid expansion of industrial scale are becoming more serious. However, the excessive use of fossil fuels causes the concentration of carbon dioxide in the atmosphere to increase year by year and causes serious environmental problems. Statistically, the content of CO2 in the atmosphere increases by more than 30% before and after the industrial revolution, and the reduction of CO2 into a hydrocarbon product or carbon monoxide having an energy utilization value and an industrial production value can not only alleviate environmental problems but also contribute to the development of clean energy. To address this problem, the fixation and conversion of carbon dioxide has become a research hotspot in recent years. The existing carbon dioxide conversion technology can be divided into biological catalysis, thermal catalysis, electric catalysis, photocatalysis and the like. Due to the advantages of mild reaction conditions, no need of secondary energy assistance and the like, the photocatalytic technology for converting carbon dioxide into fuel or other valuable chemicals by utilizing solar energy has become an ideal method for fixing and converting carbon dioxide, and is favored by numerous researchers at home and abroad.
At present, researches find that when light is irradiated on materials such as carbon materials, metal sulfides, metal oxides and the like, a photocatalytic carbon dioxide reduction process can be generated, so that people can know the feasibility of photocatalytic carbon dioxide reduction. However, the photo-generated electrons and holes usually have high recombination efficiency in the process of photocatalytic carbon dioxide reduction, so that the carbon dioxide reduction efficiency of the materials is still at a low level.
In addition, the photocatalytic carbon dioxide reduction device developed and researched at present has the problems of complex system structure, high price and very complex product.
Therefore, the development of a novel, stable and efficient carbon dioxide reduction device is of great significance.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides a low-pressure carbon dioxide reduction device and a manufacturing and using method thereof.
According to a first aspect of the technical scheme of the invention, a low-pressure carbon dioxide reduction device is provided, which comprises a reaction chamber, a top reaction chamber wall or a side reaction chamber wall, a bottom reaction chamber wall, an air inlet, a reaction chamber barometer, a first air outlet and a second air outlet, wherein the reaction chamber is of a closed chamber structure, the top reaction chamber wall arranged at the top of the reaction chamber is of a relatively flat structure and is made of quartz materials, and the side reaction chamber wall arranged at the side of the reaction chamber is of a relatively flat structure.
The bottom reaction cavity wall arranged at the bottom of the reaction cavity is in a grid shape and is made of a metal plate or quartz or other materials; an air inlet, a first air outlet and a second air outlet are arranged on the bottom reaction cavity wall, and the bottom reaction cavity wall is connected with a reaction cavity barometer.
Further, the reaction chamber barometer is used for detecting the air pressure in the reaction chamber in real time and judging the air input and the gas production data information according to the air pressure. Preferably, the second gas outlet is used for exhausting miscellaneous gas in the reaction cavity or other gas which does not need to be collected.
Furthermore, the low-pressure carbon dioxide reduction device comprises a first vacuum pump, a gas collecting port, a second vacuum pump and an exhaust port, wherein one end of the first vacuum pump is connected with the first gas outlet, and the other end of the first vacuum pump is connected with the gas collecting port; one end of the second vacuum pump is connected with the second air outlet, and the other end of the second vacuum pump is connected with the air exhaust port.
According to a second aspect of the present invention, there is provided a method for manufacturing a low-pressure carbon dioxide reduction device, comprising the steps of:
step S1, manufacturing a carbon dioxide reduction reaction cavity, wherein the top wall and the side wall of the reaction cavity are made of quartz plates, and the bottom of the reaction cavity is made of a metal plate or other materials including but not limited to quartz plates;
step S2, building a quartz plate in the carbon dioxide reduction reaction cavity, obliquely placing the quartz plate in the reaction cavity, building one end (high end) of a first quartz plate on the upper part of the side wall of the reaction cavity, building the other end (low end) of the first quartz plate on the opposite side wall of the reaction cavity, and enabling the first quartz plate to form a certain included angle with the horizontal plane; similar to the way of erecting the first quartz plate, one end (high end) of the second quartz plate is erected on the upper part of the side wall of the reaction chamber, and the other end (low end) of the second quartz plate is erected on the opposite side wall of the reaction chamber, so that the second quartz plate forms a certain included angle with the horizontal plane;
step S3, adjusting the angle between the quartz plates in the reaction chamber, wherein the lower end of the first quartz plate is close to the upper end of the second quartz plate, so that the included angle between the first quartz plate and the horizontal plane is complementary with the included angle between the second quartz plate and the horizontal plane;
step S4, coating catalyst, preparing catalyst powder on the inner side of the reaction cavity by methods of sputtering, dipping, spraying and the like; further, the catalyst powder is prepared on the two sides of the quartz plate of the reaction cavity by methods such as sputtering, dipping, spraying and the like; preferably, the catalytic layer is between 1 nanometer and 100 micrometers thick;
step S5, installing an air inlet at the bottom of the reaction cavity;
step S6, installing a reaction cavity barometer at the bottom of the reaction cavity, and monitoring the air pressure condition in the reaction cavity in real time;
and step S7, installing a first air outlet and a second air outlet at the bottom of the reaction cavity.
According to a third aspect of the present invention, there is provided a method for using a low-pressure carbon dioxide reduction apparatus, comprising the steps of:
step Z1, adjusting the working parameters of the low-pressure carbon dioxide reduction device to ensure that the low-pressure carbon dioxide reduction device can work normally;
step Z2, closing the air inlet and the first air outlet, and opening the second air outlet; opening a second vacuum pump to vacuumize the reaction cavity until the absolute pressure of a barometer of the reaction cavity is lower than-100 kPa (megapascal);
step Z3, closing the second gas outlet, opening the gas inlet, and introducing gas containing carbon dioxide until the pressure of the reaction chamber barometer is increased to a specified required pressure value;
step Z4, placing the reaction chamber under the sunlight or other light source matched with the catalyst, and enabling the carbon dioxide reduction reaction in the reaction chamber to last for a preset time so as to generate enough preset products;
step Z5, closing the gas inlet, opening the first gas outlet and the first vacuum pump, and collecting a predetermined product or a predetermined gas through the gas collecting port, wherein the predetermined product or the predetermined gas contains a mixed gas of introduced carbon dioxide, methane and carbon monoxide;
and step Z5, when the low-pressure carbon dioxide reduction device is closed, sequentially closing the air inlet, the first air outlet and the first vacuum pump, then opening the second air outlet and the second vacuum pump, and exhausting miscellaneous gases in the cavity of the reaction cavity or exhausting other gases which do not need to be collected from the air outlet.
Compared with the prior art, the low-pressure carbon dioxide reduction device and the manufacturing and using methods thereof have the following beneficial effects.
First, the present invention proposes a low-pressure carbon dioxide reduction device, which is used for photocatalytic carbon dioxide reduction in a gas phase, has a simple system configuration, is inexpensive, and has a more unitary product than a liquid-phase system, and a technique for manufacturing and using the same.
Secondly, the low-pressure carbon dioxide reduction device provided by the invention can enable the carbon dioxide reduction reaction to be efficiently and stably carried out, and the yield of the product is higher and the selectivity is higher than that of the catalytic reaction under the atmospheric pressure.
Thirdly, the low-pressure carbon dioxide reduction device provided by the invention can be applied to carbon dioxide reduction, methane preparation, carbon monoxide preparation or other gas phase catalysis such as nitrogen reduction; compared with the prior device, the device has wider application range.
Drawings
FIG. 1 is a schematic view showing the construction of a low-pressure carbon dioxide reduction apparatus according to the present invention.
FIG. 2 is a schematic view of the reaction chamber of FIG. 1 with a quartz plate disposed therein.
FIG. 3-1 is a schematic diagram of a first arrangement of quartz and catalyst.
Fig. 3-2 is a schematic diagram of a second arrangement of quartz and catalyst.
Fig. 4 is a graph of photocurrent using the low pressure carbon dioxide reduction unit of the present invention and the catalyst was titania.
FIG. 5 is a graph of photocatalytic carbon dioxide performance at low pressure using the low pressure carbon dioxide reduction apparatus of the present invention, the catalyst being titanium dioxide.
FIG. 6 is a plot of methane selectivity of photocatalytic carbon dioxide at low pressure using the low pressure carbon dioxide reduction unit of the present invention, the catalyst being titanium dioxide.
FIG. 7 is a plot of methane accumulation and methane yield for photocatalytic carbon dioxide at low pressure using the low pressure carbon dioxide reduction unit of the present invention, the catalyst being titanium dioxide.
FIG. 8 is a graph showing the yield of photocatalytic carbon dioxide in the case of low pressure using the low pressure carbon dioxide reducing apparatus of the present invention.
FIG. 9 is a graph showing the yield of photocatalytic carbon dioxide in the case of high pressure using the low pressure carbon dioxide reduction apparatus of the present invention.
Wherein the reference numerals of the components indicate: the device comprises a reaction chamber 1, a top or side reaction chamber wall 2, a bottom reaction chamber wall 3, an air inlet 4, a reaction chamber barometer 5, a first air outlet 6, a first vacuum pump 7, an air collecting port 8, a second air outlet 9, a second vacuum pump 10, an air outlet 11, a quartz wall 2-1 and a photocatalyst 2-2.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Additionally, the scope of the present invention should not be limited to only the specific experimental procedures or specific parameters described below.
The application utilizes semiconductor photocatalyst and solar energy to carry out photocatalytic CO2 reduction technology, and adopts a green and sustainable CO2 chemical conversion method. The photocatalytic CO2 reduction technology utilizes the characteristics that a semiconductor catalyst with a proper energy band structure absorbs photons and excites valence band electrons to jump to a conduction band to form photo-generated electrons, and can convert light energy into chemical energy to obtain a hydrocarbon product or carbon monoxide.
The low-pressure carbon dioxide reduction device is based on photocatalytic carbon dioxide gas-phase reduction reaction, and the photocatalyst adopts titanium dioxide or other semiconductor materials or composite materials with photocatalytic effect, such as C3N4, iron oxide, noble metals and composite catalysts thereof and the like. The low-pressure carbon dioxide reduction device achieves the effects of improving the yield and selectivity of the product by reducing the environmental pressure of carbon dioxide reduction, and can achieve good effect under the condition of low-concentration carbon dioxide gas.
As shown in fig. 1, the low-pressure carbon dioxide reduction device of the present invention includes a reaction chamber 1, a top reaction chamber wall or a side reaction chamber wall 2, a bottom reaction chamber wall 3, an air inlet 4, a reaction chamber barometer 5, a first air outlet 6, and a second air outlet 9, wherein the reaction chamber 1 is a closed chamber structure, the cross section of which preferably adopts a rectangular structure, the top reaction chamber wall 2 arranged at the top of the reaction chamber 1 adopts a relatively flat structure and is made of a quartz material, and the side reaction chamber wall 2 arranged at the side of the reaction chamber 1 adopts a relatively flat structure; the reaction chamber 1 is a main place for carbon dioxide reduction, and ultraviolet rays in sunlight contribute to photocatalytic reaction through the top or side reaction chamber wall 2. The bottom reaction chamber wall 3 arranged at the bottom of the reaction chamber 1 is grid-shaped and is preferably made of a metal plate, is used for reflecting the reaction gas into the reaction chamber to promote the reaction gas to further generate a photocatalytic reaction, and can also be made of quartz or other materials; an air inlet 4, a first air outlet 6 and a second air outlet 9 are arranged on the bottom reaction chamber wall 3, and are connected with a reaction chamber barometer 5. The reaction cavity barometer 5 is used for detecting the air pressure in the reaction cavity in real time; preferably, the reaction chamber barometer 5 is arranged between the air inlet 4 and the first air outlet 6, and is used for detecting the air pressure in the reaction chamber in real time and judging data information such as air inflow and air production according to the air pressure. Carbon dioxide and carbon dioxide mixed gas enter the reaction cavity from the gas inlet 4; the gas generated after the reduction of carbon dioxide is collected by the first gas outlet 6, and the gas generated after the reduction of carbon dioxide comprises carbon dioxide (or carbon dioxide mixed gas), methane, carbon monoxide and the like. The second gas outlet 9 is used for emptying miscellaneous gas in the cavity of the reaction cavity or removing other gas which does not need to be collected; preferably, the second gas outlet 9 is disposed at an end far away from the gas inlet, that is, the first gas outlet 6 is disposed between the second gas outlet 9 and the gas inlet 4, and the second gas outlet 9 is used for evacuating the impurity gas in the reaction cavity or removing other gases that do not need to be collected. The junction between top reaction chamber wall and the side reaction chamber wall adopts concave surface connection structure, preferably adopts smooth concave surface connection structure, and concave surface connection structure further promoted photocatalysis carbon dioxide gas phase reduction reaction efficiency with the ultraviolet ray scattering to the reaction chamber in.
Furthermore, the grid-shaped bottom reaction chamber wall 3 adopts a grid plate which is obliquely arranged on the bottom reaction chamber wall, catalyst layers are coated on two sides of the grid plate, and the efficiency of the reduction reaction is further improved through the reflection of the grid plate; the grid plates and the horizontal surfaces of the bottom reaction chamber walls form an angle of 20-75 degrees, preferably an angle of 35-60 degrees, and more preferably an angle of 40-55 degrees. In preferred embodiments, 30-, 40-, 45-, 50-, 65-angle angles are employed, respectively. Further, the grill plate is provided only at the interval between the air inlet, the first air outlet, and the second air outlet. In another embodiment, the bottom reaction chamber wall 3 is a wave plate structure, and the wave plate structure is used to scatter the ultraviolet rays upwards to improve the efficiency of the reduction reaction.
Furthermore, the low-pressure carbon dioxide reduction device further comprises a first vacuum pump 7, an air collecting port 8, a second vacuum pump 10 and an exhaust port 11, wherein one end of the first vacuum pump 7 is connected with the first air outlet 6, and the other end of the first vacuum pump 7 is connected with the air collecting port 8; one end of the second vacuum pump 10 is connected to the second air outlet 9, and the other end of the second vacuum pump 10 is connected to the exhaust port 11.
The first vacuum pump 7 assists the first gas outlet 6 to extract gas products from the reaction chamber, and the second vacuum pump 10 assists the second gas outlet 9 to extract useless gases such as miscellaneous gases from the reaction chamber. The reaction chamber is ensured to be operated in a negative pressure environment, preferably a micro-negative pressure environment, under the auxiliary pumping or suction of the first vacuum pump 7 and the second vacuum pump 10. The external container is connected to the end of the gas collecting port 8 and is used for collecting gas generated after carbon dioxide reduction through the gas collecting port 8. Unnecessary gases such as miscellaneous gases are discharged through the exhaust port 11.
Further, in the low-pressure carbon dioxide reduction device, in the carbon dioxide reduction process, under the illumination condition, the photocatalyst absorbs photons, electrons on the valence band are excited and jump to an empty conduction band, and a corresponding hole is left on the valence band to form a hole-electron pair. Subsequently, since the exciton lifetime is short, a part of the holes and electrons are quickly recombined, but a part of the holes and electrons slowly move to the surface of the catalyst. Electrons in the conduction band can move to the semiconductor surface to act as a reducing agent; holes in the valence band can move to the surface of the catalyst to act as a strong oxidant, and a photocatalytic reaction, which is essentially a redox reaction, occurs. In the gas phase reaction, 1 carbon dioxide molecule is combined with 2 protons and 2 electrons to generate 1 carbon monoxide molecule; continuing to combine 6 protons and 6 electrons, 1 molecule of methane can be generated.
The low-pressure carbon dioxide reduction chemical reaction of the invention is as follows:
CO2+2H++2e→HCOOH*
HCOOH*+H++e→CO*+H2O
when carbon monoxide is produced:
CO*→CO
when methane is produced:
CO*+6H++6e→CH4*
CH4*→CH4
in order to further improve the technical effect of the low-pressure carbon dioxide reduction reaction, the invention provides the reaction device shown in fig. 2, that is, a quartz plate is obliquely arranged in the reaction chamber shown in fig. 1, one end (high end) of the first quartz plate is erected on the upper part of the side wall of the reaction chamber, and the other end (low end) of the first quartz plate is erected on the opposite side wall of the reaction chamber, so that the first quartz plate forms a certain included angle with the horizontal plane. Similar to the way of erecting the first quartz plate, one end (high end) of the second quartz plate is erected on the upper part of the side wall of the reaction chamber, and the other end (low end) of the second quartz plate is erected on the opposite side wall of the reaction chamber, so that a certain included angle is formed between the second quartz plate and the horizontal plane. Furthermore, the lower end of the first quartz plate is close to the upper end of the second quartz plate; and the later quartz plates are erected by analogy. The number and size of the quartz plates can be further designed according to the size of the cavity and the light source. Preferably, the photocatalyst is coated on both sides of the quartz plate inside the reaction chamber. The quartz plate which is erected plays a role of supporting the photocatalyst and contributes to the reduction reaction of carbon dioxide. According to multiple tests, the angle between the quartz plate and the horizontal plane is preferably 10-60 degrees, preferably 20-45 degrees, so that the reduction reaction of carbon dioxide is increased, and light absorption is not hindered due to too many quartz plates. Preferably, the angle between the first quartz plate and the horizontal plane is complementary to the angle between the second quartz plate and the horizontal plane, so that the carbon dioxide reduction reaction between the quartz plates is optimal.
In the present invention, the catalyst used is preferably a semiconductor photocatalyst. The preparation structure diagrams of the catalyst layer are shown in fig. 3-1 and fig. 3-2, which show the structure schematic diagrams of quartz and the catalyst layer, and the prepared catalyst powder is prepared inside the reaction chamber, i.e. inside the quartz chamber, by sputtering, dipping, spraying and the like. The thickness of the catalyst layer is between 1 nanometer and 100 micrometers. The semiconductor photocatalyst is preferably an oxynitride, sulfide, titanate, niobate, tantalate or chromate, and more preferably TiO2-XNX or the like.
In more detail, as shown in fig. 3-1, the catalyst 2-2 is coated in the reaction chamber, i.e., the catalyst 2-2 is coated inside the quartz wall 2-1. As shown in FIG. 3-2, a catalyst 2-2 is coated on a quartz plate 2-1 which is staggered inside the reaction chamber, that is, the catalyst is coated on both sides of the quartz wall 2-1. In one embodiment, the catalyst is titanium dioxide or other semiconductor materials or composite materials with photocatalytic effect, such as C3N4, iron oxide, noble metals and composite catalysts thereof, and the like. According to different kinds of catalysts and different preparation methods, different optimal light sources are selected. For example, when the catalyst is titanium dioxide or iron oxide, the ultraviolet light source is preferably selected; when the catalyst is cadmium sulfide, a visible light source is preferably selected. The catalyst can be coated on the quartz plate by sputtering, dipping, spraying and the like. The catalyst layer thickness is preferably between 1 nm and 100 μm in terms of carbon dioxide reduction reaction efficiency; the catalyst layer is too thin, the amount of the catalyst is small, and the reduction effect of carbon dioxide is poor; the catalyst layer is too thick, light is blocked in the cavity, and the carbon dioxide reduction effect is not good.
Further, a method for manufacturing a low-pressure carbon dioxide reduction device is provided, which comprises the following steps:
step S1, manufacturing a carbon dioxide reduction reaction cavity, wherein the top wall and the side wall of the reaction cavity are made of quartz plates, and the bottom of the reaction cavity is made of a metal plate or other materials including but not limited to quartz plates;
step S2, building a quartz plate in the carbon dioxide reduction reaction cavity, obliquely placing the quartz plate in the reaction cavity, building one end (high end) of a first quartz plate on the upper part of the side wall of the reaction cavity, building the other end (low end) of the first quartz plate on the opposite side wall of the reaction cavity, and enabling the first quartz plate to form a certain included angle with the horizontal plane; similar to the way of erecting the first quartz plate, one end (high end) of the second quartz plate is erected on the upper part of the side wall of the reaction chamber, and the other end (low end) of the second quartz plate is erected on the opposite side wall of the reaction chamber, so that the second quartz plate forms a certain included angle with the horizontal plane;
step S3, adjusting the angle between the quartz plates in the reaction chamber, wherein the lower end of the first quartz plate is close to the upper end of the second quartz plate, so that the included angle between the first quartz plate and the horizontal plane is complementary with the included angle between the second quartz plate and the horizontal plane;
step S4, coating catalyst, preparing catalyst powder on the inner side of the reaction cavity by methods of sputtering, dipping, spraying and the like; further, the catalyst powder is prepared on the two sides of the quartz plate of the reaction cavity by methods such as sputtering, dipping, spraying and the like; preferably, the catalytic layer is between 1 nanometer and 100 micrometers thick;
step S5, installing an air inlet at the bottom of the reaction cavity;
step S6, installing a reaction cavity barometer at the bottom of the reaction cavity, and monitoring the air pressure condition in the reaction cavity in real time;
and step S7, installing a first air outlet and a second air outlet at the bottom of the reaction cavity.
Further, step S7 of the method for manufacturing a low-pressure carbon dioxide reduction device further includes the steps of:
step S71, installing a first vacuum pump and a second vacuum pump, connecting the first vacuum pump to the first air outlet, and connecting the second vacuum pump to the second air outlet;
step S72, adjusting the parameters of the first vacuum pump or/and the second vacuum pump to match the working parameters of the reaction chamber;
step S73, installing a gas collecting port to connect the gas collecting port with a first vacuum pump, wherein the gas collecting port is used for collecting gas products after carbon dioxide reduction;
and step S74, installing an exhaust port to connect the exhaust port with a second vacuum pump, wherein the exhaust port is used for exhausting miscellaneous gas in the cavity of the reaction cavity or exhausting other gas which does not need to be collected.
Furthermore, the invention provides a use method of the low-pressure carbon dioxide reduction device, which comprises the following steps:
step Z1, adjusting the working parameters of the low-pressure carbon dioxide reduction device to ensure that the low-pressure carbon dioxide reduction device can work normally;
step Z2, closing the air inlet and the first air outlet, and opening the second air outlet; opening a second vacuum pump to vacuumize the reaction cavity until the absolute pressure of a barometer of the reaction cavity is lower than-100 kPa (megapascal);
step Z3, closing the second gas outlet, opening the gas inlet, and introducing gas containing carbon dioxide until the pressure of the reaction chamber barometer is increased to a specified required pressure value;
step Z4, placing the reaction chamber under the sunlight or other light source matched with the catalyst, and enabling the carbon dioxide reduction reaction in the reaction chamber to last for a preset time so as to generate enough preset products;
step Z5, closing the gas inlet, opening the first gas outlet and the first vacuum pump, and collecting a predetermined product or a predetermined gas through the gas collecting port, wherein the predetermined product or the predetermined gas contains a mixed gas of introduced carbon dioxide, methane and carbon monoxide;
and step Z5, when the low-pressure carbon dioxide reduction device is closed, sequentially closing the air inlet, the first air outlet and the first vacuum pump, then opening the second air outlet and the second vacuum pump, and exhausting miscellaneous gases in the cavity of the reaction cavity or exhausting other gases which do not need to be collected from the air outlet.
Fig. 4 is a graph of photocurrent using the low pressure carbon dioxide reduction unit of the present invention and the catalyst was titania. The photocurrent curve in fig. 4 shows that at constant pressure of 6V, the photocurrent at low pressure is much greater than the photocurrent at high pressure, which shows the competitive action of electron/hole recombination and surface adsorbate elimination; at low pressures, the electron-eliminating effect of the surface adsorbate is reduced and hence the photocurrent is increased. The catalyst can accumulate electrons more effectively under low pressure, and the efficiency of the carbon dioxide reduction reaction is improved.
FIG. 5 is a graph of photocatalytic carbon dioxide performance at low pressure using the low pressure carbon dioxide reduction apparatus of the present invention, the catalyst being titanium dioxide. As shown in fig. 5, it can be seen that methane yield is higher with lower pressure, both in pure carbon dioxide and in low carbon dioxide concentration, and fig. 5 shows that reducing carbon dioxide at low pressure is more efficient than at high pressure.
FIG. 6 is a graph showing methane selectivity of photocatalytic carbon dioxide at low pressure using the low pressure carbon dioxide reduction apparatus of the present invention, the catalyst being titanium dioxide, and FIG. 6 showing the methane selectivity after four reactions; fig. 7 is a graph showing the accumulation amount of methane and the methane yield of photocatalytic carbon dioxide at a low pressure using the low-pressure carbon dioxide reduction apparatus of the present invention, the catalyst being titanium dioxide, and fig. 7 shows the fluctuation in the methane yield as a function of the illumination time/hour. As can be seen from fig. 6 and 7, at a relative gas pressure of-80 kPa, the selectivity of the titania catalyst to methane was higher than 91%, and the methane yield was stable; fig. 6 and 7 show that the reduced carbon dioxide is stable at low pressure.
Fig. 8 is a graph showing the yield of photocatalytic carbon dioxide in the case of low pressure using the low-pressure carbon dioxide reduction apparatus of the present invention, and fig. 9 is a graph showing the yield of photocatalytic carbon dioxide in the case of high pressure using the low-pressure carbon dioxide reduction apparatus of the present invention. In the test environment of fig. 8 and 9, the catalyst used was a mixed catalyst of titanium dioxide and platinum nanoparticles. FIG. 8 is a graph of methane yield and accumulation at subatmospheric pressure-80 kPa; FIG. 9 is the methane yield and accumulation at high pressure 0 kPa. It can be seen that the methane yield at low pressure is-80 kPa is much higher than at high pressure, 0 kPa.
In summary, the low-pressure carbon dioxide reduction device and the manufacturing and using method thereof of the present invention have the following advantages compared with the prior art.
First, the present invention proposes a low-pressure carbon dioxide reduction device, which is used for photocatalytic carbon dioxide reduction in a gas phase, has a simple system configuration, is inexpensive, and has a more unitary product than a liquid-phase system, and a technique for manufacturing and using the same.
Secondly, the low-pressure carbon dioxide reduction device provided by the invention can enable the carbon dioxide reduction reaction to be carried out efficiently and stably, and the yield of the product is higher and the selectivity is higher for the catalytic reaction under higher pressure.
Thirdly, the low-pressure carbon dioxide reduction device provided by the invention can be applied to carbon dioxide reduction, methane preparation, carbon monoxide preparation or other gas phase catalysis such as nitrogen reduction; compared with the prior device, the device has wider application range.
Particularly, the catalytic reaction of the low-pressure carbon dioxide reduction device provided by the invention is carried out on a gas-solid interface of carbon dioxide and a catalyst, so that the photocatalysis efficiency can be enhanced, and the selectivity of a product can be improved.
It should also be noted that the shapes and dimensions of the respective components in the drawings do not reflect actual sizes and proportions, but merely illustrate the contents of the embodiments of the present invention.
The invention has not been described in detail and is part of the common general knowledge of a person skilled in the art. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. The utility model provides a low pressure carbon dioxide reduction device, its characterized in that, it includes reaction chamber (1), top reaction chamber wall or side reaction chamber wall (2), bottom reaction chamber wall (3), air inlet (4), reaction chamber barometer (5), first gas outlet (6) and second gas outlet (9), and reaction chamber (1) is airtight chamber structure, sets up reaction chamber wall (2) at the top of reaction chamber (1) adopt flat structure and make by quartz material to and set up and be in side reaction chamber wall (2) of the side of reaction chamber (1) adopt flat structure.
2. The low-pressure carbon dioxide reduction device according to claim 1, wherein the bottom reaction chamber wall (3) arranged at the bottom of the reaction chamber (1) is grid-shaped and made of metal plate or quartz or other materials; an air inlet (4), a first air outlet (6) and a second air outlet (9) are arranged on the bottom reaction cavity wall (3), and the bottom reaction cavity wall (3) is connected with a reaction cavity barometer (5).
3. The low-pressure carbon dioxide reduction device according to claim 2, wherein the reaction chamber barometer (5) is used for detecting the air pressure in the reaction chamber in real time and judging the data information of air inflow and air production according to the air pressure.
4. A low-pressure carbon dioxide reduction apparatus according to claim 2, wherein the second gas outlet (9) is used to evacuate the reaction chamber cavity of miscellaneous gases or other gases that do not need to be collected.
5. The low-pressure carbon dioxide reduction device according to claim 2, further comprising a first vacuum pump (7), a gas collection port (8), a second vacuum pump (10), and a gas exhaust port (11), wherein one end of the first vacuum pump (7) is connected to the first gas outlet (6), and the other end of the first vacuum pump (7) is connected to the gas collection port (8); one end of the second vacuum pump (10) is connected with the second air outlet (9), and the other end of the second vacuum pump (10) is connected with the exhaust port (11).
6. A method for manufacturing a low-pressure carbon dioxide reduction device comprises the following steps:
step S1, manufacturing a carbon dioxide reduction reaction cavity, wherein the top wall and the side wall of the reaction cavity are made of quartz plates, and the bottom of the reaction cavity is made of a metal plate or other materials including but not limited to quartz plates;
step S2, erecting a quartz plate in the carbon dioxide reduction reaction cavity, obliquely placing the quartz plate in the reaction cavity, erecting the high end of the first quartz plate on the upper part of the side wall of the reaction cavity, erecting the low end of the first quartz plate on the opposite side wall of the reaction cavity, and making the first quartz plate form a certain included angle with the horizontal plane; similar to the erecting mode of the first quartz plate, the high end of the second quartz plate is erected at the upper part of the side wall of the reaction chamber, and the low end of the second quartz plate is erected on the opposite side wall of the reaction chamber, so that a certain included angle is formed between the second quartz plate and the horizontal plane;
step S3, adjusting the angle between the quartz plates in the reaction chamber, wherein the lower end of the first quartz plate is close to the upper end of the second quartz plate, so that the included angle between the first quartz plate and the horizontal plane is complementary with the included angle between the second quartz plate and the horizontal plane;
step S4, coating catalyst, preparing catalyst powder on the inner side of the reaction cavity by sputtering, dipping and spraying;
step S5, installing an air inlet at the bottom of the reaction cavity;
step S6, installing a reaction cavity barometer at the bottom of the reaction cavity, and monitoring the air pressure condition in the reaction cavity in real time;
and step S7, installing a first air outlet and a second air outlet at the bottom of the reaction cavity.
7. The method of manufacturing a low-pressure carbon dioxide reduction device according to claim 6, wherein the catalytic layer has a thickness of between 1 nm and 100 μm.
8. The method of claim 6, wherein the catalyst powder is formed on both sides of the quartz plate of the reaction chamber by sputtering, dipping, or spraying.
9. A use method of a low-pressure carbon dioxide reduction device comprises the following steps:
step Z1, adjusting the working parameters of the low-pressure carbon dioxide reduction device to ensure that the low-pressure carbon dioxide reduction device can work normally;
step Z2, closing the air inlet and the first air outlet, and opening the second air outlet; opening a second vacuum pump to vacuumize the reaction cavity until the absolute air pressure of the air pressure gauge of the reaction cavity is lower than-100 kPa;
step Z3, closing the second gas outlet, opening the gas inlet, and introducing gas containing carbon dioxide until the pressure of the reaction chamber barometer is increased to a specified required pressure value;
step Z4, placing the reaction chamber under the sunlight or other light source matched with the catalyst, and enabling the carbon dioxide reduction reaction in the reaction chamber to last for a preset time so as to generate enough preset products;
step Z5, closing the gas inlet, opening the first gas outlet and the first vacuum pump, and collecting a predetermined product or a predetermined gas through the gas collecting port, wherein the predetermined product or the predetermined gas contains a mixed gas of introduced carbon dioxide, methane and carbon monoxide;
and step Z5, when the low-pressure carbon dioxide reduction device is closed, sequentially closing the air inlet, the first air outlet and the first vacuum pump, then opening the second air outlet and the second vacuum pump, and exhausting miscellaneous gases in the cavity of the reaction cavity or exhausting other gases which do not need to be collected from the air outlet.
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