CN110652951A - Photocatalysis tubular reactor - Google Patents
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- CN110652951A CN110652951A CN201911085807.9A CN201911085807A CN110652951A CN 110652951 A CN110652951 A CN 110652951A CN 201911085807 A CN201911085807 A CN 201911085807A CN 110652951 A CN110652951 A CN 110652951A
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 63
- 238000007146 photocatalysis Methods 0.000 title abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000010453 quartz Substances 0.000 claims abstract description 78
- 239000002184 metal Substances 0.000 claims abstract description 68
- 229910052751 metal Inorganic materials 0.000 claims abstract description 68
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000012495 reaction gas Substances 0.000 claims abstract description 11
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- 238000010438 heat treatment Methods 0.000 claims description 29
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- 238000002347 injection Methods 0.000 claims description 12
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 239000007769 metal material Substances 0.000 claims description 5
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- 230000009471 action Effects 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
- B01J3/042—Pressure vessels, e.g. autoclaves in the form of a tube
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
- B01J8/067—Heating or cooling the reactor
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0871—Heating or cooling of the reactor
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
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Abstract
The invention relates to a photocatalytic tubular reactor, which is characterized in that: the quartz glass tube comprises a metal outer cylinder (7) and a quartz inner cylinder (15), wherein the metal outer cylinder (7) and the quartz inner cylinder (15) are of a split structure, and the metal outer cylinder (7) is sleeved outside the quartz inner cylinder (15); the left side and the right side of the metal outer cylinder (7) are provided with light guide cylinders (9), light guide columns (10) are arranged in the light guide cylinders, and light passes through the quartz inner cylinder (15) through the light guide columns (10); the upper end and the lower end of the metal outer cylinder (7) are respectively provided with an upper port connector (3-1) and a lower port connector (3-2); reaction gas and reaction liquid enter the reactor from the upper port connector (3-1) and flow out from the lower port connector (3-2) after reaction. According to the high-temperature high-pressure photocatalytic tubular reactor provided by the invention, quartz is used as a catalyst carrier, and the high-temperature high-pressure photocatalytic tubular reactor is illuminated in left and right directions, and can reach 10MPa in long-term use at the high temperature of 800 ℃. Breaks through the limitation that the photocatalysis tubular reactor can only be used for normal pressure experiments, and enlarges the research range in the photocatalysis field.
Description
Technical Field
The invention relates to the field of chemical reaction devices, in particular to a tubular reactor used in the fields of photocatalysis, gas-solid phase catalysis, carbon dioxide reduction, photo-thermal catalysis, photo-catalytic synthesis, photo-catalytic degradation of organic matters, catalytic degradation of harmful gases (VOCs, NOx, SOx, acetaldehyde, formaldehyde and the like), thermal catalysis, photochemistry and the like.
Background
Photochemical and photocatalytic oxidation methods are currently a more studied advanced oxidation technology. The photocatalytic reaction is a chemical reaction that proceeds by the action of light. Photochemical reactions require molecules to absorb electromagnetic radiation of a particular wavelength, be excited to produce a molecular excited state, and then undergo a chemical reaction to produce a new species, or become an intermediate chemical product that initiates a thermal reaction. The activation energy of photochemical reaction is derived from the energy of photons, and photoelectric conversion and photochemical conversion are always active research fields in the utilization of solar energy.
Photocatalytic oxidation technology utilizes photo-excitation oxidation to oxidize O2、H2O2The oxidizing agent is combined with the light radiation. Photodegradation generally refers to the gradual oxidation of organic substances into low-molecular intermediate products under the action of light to finally generate CO2、H2O and other ions, e.g. NO3 -、PO4 3-、Cl-And the like. The photodegradation of organic substances can be divided into direct photodegradation and indirect photodegradation. The former is a chemical reaction that occurs further after the organic molecules absorb light energy. The latter is a reaction in which some substances existing in the surrounding environment absorb light energy to form an excited state and then induce a series of organic pollution. Indirect photodegradation is more important for organic pollutants that are difficult to biodegrade in the environment. The way of degrading pollutants by photochemical reaction includes photochemical oxidation process without catalyst and with catalyst. The former mostly uses oxygen and hydrogen peroxide as oxygenA chemical agent for oxidatively decomposing the contaminant under the irradiation of ultraviolet light; the latter is also known as photocatalytic oxidation and can be generally classified into two types, homogeneous and heterogeneous catalysis. The common method in homogeneous photocatalytic degradation is Fe2+Or Fe3+And H2O2As a medium, OH is generated through a photo-Fenton reaction to degrade pollutants, in heterogeneous photocatalytic degradation, a certain amount of photosensitive semiconductor material is added into a pollution system, a certain amount of light radiation is combined, the photosensitive semiconductor is excited under the irradiation of light to generate electron-hole pairs, dissolved oxygen, water molecules and the like adsorbed on the semiconductor react with the electron-hole pairs to generate free radicals with strong oxidizability such as OH, and the pollutants are completely or nearly completely mineralized through the addition, substitution and electron transfer equation between the free radicals and the pollutants.
The photochemical tubular reactors commonly used in laboratories at present are single-tube reactors made of high borosilicate glass or quartz glass, the existing single-tube reactor is mostly a quartz straight tube, and due to the limitation of reactor materials, the safety problem of gas leakage caused by reactor fragmentation is often caused in the experimental process; the quartz reactor cannot bear pressure, so that the quartz reactor can only be used for normal-pressure experiments, and the research of photocatalysis in the high-pressure field cannot be carried out. Although the all-metal reactor can meet the experimental requirements of high temperature and high pressure, the all-metal reactor is opaque and cannot be used for photocatalytic experiments, and meanwhile, the metal serving as a catalyst carrier may cause catalyst pollution or participate in catalytic reaction to influence experimental data. The scope of research in the field of photocatalysis is greatly limited by these drawbacks.
When a quartz single-tube reactor needs to be filled with a catalyst, a temperature measuring thermocouple is fixed at the center of the reactor, inert substances such as quartz sand and the like are filled at the bottom of a reaction area to be used as supports, then the weighed catalyst is put in from the top, and a bed layer is uniform by knocking the tube wall. The catalyst in the reactor is very troublesome to fill, can cause wall hanging when being thrown from a high position, is not uniformly distributed and easy to control, and has low utilization rate; and the repeatability of multiple experiments is poor. After the experiment is finished, residual substances in the reaction tube are difficult to clean, and catalyst residues are easy to block a gas circuit and pollute a new catalyst.
The external pipelines connected with the reactor are mostly stainless steel pipelines, and the quartz reactor and the stainless steel pipelines need to be connected by means of a complex sealing structure, so that the installation and the replacement are very inconvenient. And therefore, the design and structure of the quartz reactor cannot be changed at will. Meanwhile, the quartz reactor has the problem of inconvenient vertical fixation.
The light-transmitting holes of the original light source are arranged in the middle of the heating furnace and transmit light from front to back. Due to the existence of the light through holes, no furnace wire is arranged in the middle of the furnace for heating, no heat insulation material is arranged at the light through holes, and the heat dissipation is fast. This results in a large temperature gradient in the reaction zone of the reactor.
In view of the above-mentioned defects of the existing photocatalytic quartz reactor, the present inventors have made active research and innovation to create a high-temperature high-pressure photocatalytic tubular reactor with a novel structure, so that the reactor has higher practicability.
Disclosure of Invention
The invention provides a photocatalytic tubular reactor, which aims to solve the technical problems as follows: (1) the safety problem that the existing reactor is easy to crack in the experimental process to generate gas leakage is solved; (2) the tubular reactor can meet the requirements that the existing tubular reactor can only carry out a normal pressure test and cannot carry out a high pressure test; (3) the problems that the wall hanging and the uneven distribution of the catalyst are caused by the fact that the original catalyst is thrown from a high position, and the control is not easy are solved; (4) the problems that residual substances in a reaction tube are difficult to clean, a gas circuit is blocked due to catalyst residues, and a new catalyst is polluted are solved; (5) the problem that the quartz reactor is inconvenient to connect with an external pipeline through a stainless steel pipeline is solved; (6) the problem that the reactor is inconvenient to install and replace is solved; (7) the problem that the quartz reactor is inconvenient to vertically fix is solved; (8) the problem of large temperature gradient of a reaction area of a quartz reactor is solved.
In order to solve the technical problems, the invention adopts the following technical scheme:
(1) a photocatalysis tubular reactor comprises a metal outer cylinder and a quartz inner cylinder, wherein the metal outer cylinder and the quartz inner cylinder are of split structures, the metal outer cylinder is sleeved outside the quartz inner cylinder, and the quartz inner cylinder can be taken out independently; the left side and the right side of the metal outer cylinder are provided with light guide cylinders, light guide columns are arranged in the light guide cylinders, and light passes through the quartz inner cylinder through the light guide columns; the upper end and the lower end of the metal outer cylinder are respectively provided with an upper port connector and a lower port connector; reaction gas and reaction liquid enter the reactor from the upper port joint and flow out from the lower port joint after reaction.
(2) According to the photocatalytic tubular reactor described in (1), the quartz inner cylinder is provided with a flat-mouth quartz reactor, a straight tube sand plate reactor or a slant quartz sand plate reactor (the specific structure of the quartz inner cylinder with the slant quartz sand plate reactor is referred to in the prior application 201920970907.9 of the present applicant), and is used for filling a catalyst.
(3) According to the photocatalytic tubular reactor in (1) or (2), the light guide cylinders on the left and right sides of the metal outer cylinder form a cross structure; the light guide column is of a T-shaped structure.
(4) The photocatalytic tubular reactor as set forth in any one of (1) to (3), wherein the metal outer cylinder is provided with a fixed wing (8).
(5) The photocatalytic tubular reactor according to any one of (1) to (4), wherein the upper port fitting is sealed by an SAE split flange (SAE is an SAE flange manufactured in accordance with SAE standards for short by the society of mechanical Engineers), and the lower port fitting is sealed by an SAE split flange; the left and right light guide cylinders are sealed by flanges; the external connecting pipeline adopts a clamping sleeve structure.
(6) The photocatalytic tubular reactor as set forth in any one of (1) to (5), wherein the photocatalytic tubular reactor is clamped with the heating furnace through the fixed wings, and the light guide cylinder and the pressing flange are arranged in the heating furnace.
(7) The photocatalytic tubular reactor as set forth in any one of (1) to (6), wherein the upper port connector is provided with a liquid injection port and an air inlet, and both the liquid injection port and the air inlet are metal ferrule connectors; the lower port connector is provided with an air outlet, a temperature control port and a thermocouple sleeve, and the air outlet and the temperature control port are both metal ferrule interfaces.
(8) The photocatalytic tubular reactor according to any one of (1) to (7), wherein a thermocouple sleeve is arranged in the temperature control port, the thermocouple sleeve is a metal blind pipe with one end sealed, and the thermocouple sleeve and the temperature control port are hermetically connected by a metal ferrule; the temperature measuring thermocouple is placed in the thermocouple sleeve.
(9) The photocatalytic tubular reactor as set forth in any one of (1) to (8), wherein two annular grooves are formed in the outer position of the lower port joint and are matched with the close rings; and standard straight threads are reserved in the lower port connector.
(10) The photocatalytic tubular reactor according to any one of (1) to (9), wherein the metal outer cylinder is a seamless tube made of a high-temperature and high-pressure resistant metal material; the light guide cylinder is made of high-temperature and high-pressure resistant metal materials and is welded with the metal outer cylinder.
(11) The photocatalytic tubular reactor as set forth in any one of (1) to (10), wherein the light guide column is of a T-shaped structure and is integrally formed and made of quartz or sapphire light-transmitting material.
(12) The photocatalytic tube reactor as set forth in any one of (1) to (11), wherein the light guide cylinder and the light guide column are hermetically connected by a flange structure, and the hermetically connected structure comprises a welding flange, a high-temperature pad, a copper ring and a pressing flange.
(13) The photocatalytic tube reactor as set forth in any one of (1) to (12), wherein the quartz inner cylinder is mounted on a port fitting, the port fitting is provided with an annular groove, and a seal ring is provided in the groove.
(14) The photocatalytic tubular reactor as set forth in any one of (1) to (6), wherein the heating furnace is an open furnace, and the cross-shaped groove matched with the reactor is positioned on the opening plane of the heating furnace; and the heating furnace controls the temperature in three sections, and supplements and adjusts the middle section through the upper section and the lower section, so as to ensure the length of the constant temperature area.
The photocatalytic tubular reactor provided by the invention has the following beneficial technical effects:
1. the photocatalysis tubular reactor comprises a metal outer cylinder and a quartz inner cylinder, wherein the metal outer cylinder and the quartz inner cylinder are of a split structure, and the metal outer cylinder is sleeved outside the quartz inner cylinder. The metal outer cylinder and the light guide cylinder are used for bearing the pressure difference inside and outside the reactor in the experimental process; the quartz inner cylinder made of quartz is used as a catalyst carrier and is positioned in the metal outer cylinder, the internal and external pressure difference is equal, and the pressure is not born in the experimental process. The problem of original pure quartz reactor because of pressure floats in the reaction process, the safety such as cracked gas of reactor reveals is solved.
The metal outer cylinder and the light guide cylinder are both formed by processing high-temperature and high-pressure resistant seamless pipes, and the metal outer cylinder and the light guide cylinder are welded in a reinforcing mode. The upper end and the lower end of the metal outer cylinder are hermetically connected with the port joint by adopting SAE split flanges. The inside of the light guide cylinder and the light guide column are sealed by adopting a flange structure, and the T-shaped structure of the light guide column is convenient for the sealing installation of the high-temperature pad. The material and structure determine that the reactor can be illuminated in left and right directions by taking quartz as a catalyst carrier, and the pressure can reach 10MPa after long-term use at the high temperature of 800 ℃. The tubular reactor can be used for solving the requirements that the existing tubular reactor can only carry out a normal pressure experiment and cannot carry out a high pressure experiment. The research range of the photocatalysis field is enlarged. The catalyst is positioned on the quartz inner cylinder, and the transparent quartz inner cylinder does not influence the illumination and does not contact with the metal outer cylinder to influence the experimental data.
2. The metal outer cylinder and the quartz inner cylinder are of a split structure, and the quartz inner cylinder can be taken out independently. The quartz inner cylinder is very convenient for filling the catalyst after being taken out, and the filling mode, the filling amount, the filling thickness and the uniformity can be accurately controlled. The problem of original catalyst through from the eminence put in cause the wall built-up, catalyst distributes inhomogeneous, not good control, experiment inconsistency many times is solved.
3. The upper port connector is provided with a liquid injection port and an air inlet, and the liquid injection port and the air inlet are metal ferrule connectors. The lower port connector is provided with an air outlet, a temperature control port and a thermocouple sleeve, and the air outlet and the temperature control port are metal ferrule interfaces. A thermocouple sleeve is arranged in the temperature control port, the thermocouple sleeve is a metal blind pipe with one end sealed, and the thermocouple sleeve and the temperature control port are hermetically connected by a metal clamping sleeve. The clamping sleeve is simple and convenient in connection mode and high in compressive strength, and the problem that the quartz reactor is inconvenient to connect with an external pipeline stainless steel pipeline is solved.
4. The quartz sand plate on the quartz inner cylinder is positioned at the top of the quartz inner cylinder, so that the residual substances of the sand plate can be conveniently cleaned. Solves the problems of gas path blockage and new catalyst pollution caused by catalyst residue.
5. The port connects the outside position and has annular groove, and the sealing washer is placed to annular groove, and the user can be according to the demand, and different quartzy inner tubes of installation, easy operation is convenient, and the manual installation and the dismantlement of accomplishing quartzy inner tube can be done. The problem of inconvenient installation and replacement of the reactor is solved. Meanwhile, standard straight threads are reserved in the port connector, so that the connection of other types of reactors is facilitated.
6. A circular fixed wing is welded at the upper middle position of the metal outer cylinder and clamped at the upper part of the heating furnace. Solves the problem of inconvenient vertical fixation of the reactor.
7. The heating furnace is an open furnace, and the cross-shaped groove matched with the reactor is positioned on the opening plane of the furnace, so that the heating of furnace wires in the middle of the furnace is not influenced; the light-transmitting parts such as the cross light guide cylinder, the light guide column, the welding flange, the pressing flange and the like are all positioned in the reaction furnace, so that the heat dissipation is reduced to the maximum extent; meanwhile, the heating furnace is controlled by three sections of temperature, and the problem of large temperature gradient of the reaction area of the reactor is solved by supplementing and adjusting the middle section by the upper section and the lower section.
8. The light guide column in the light guide cylinder is made of light-transmitting materials such as quartz and sapphire, is integrally formed, one end of the light guide column is connected with the light source through the flange, and the other end of the light guide column is connected with the quartz reactor, so that light loss is reduced, and illumination efficiency is improved.
The photocatalytic tubular reactor provided by the invention can effectively combine an external pipeline, a light path and a heating furnace, and is an ideal reactor in a high-temperature high-pressure photocatalytic environment.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic diagram of a photocatalytic tube reactor of the present invention;
reference numbers in the figures: a is a reaction gas flow inlet, B is a quartz inner cylinder, C is a reaction gas flow outlet, and D is a light source.
FIG. 2 is a 2D view of a photocatalytic tube reactor of the present invention;
reference numbers in the figures: the device comprises a liquid injection port 1-1, a temperature control port 1-2, an air inlet 2-1, an air outlet 2-2, an upper port joint 3-1, a lower port joint 3-2, an SAE split flange 4-1, an SAE split flange 4-2, an upper O-ring 5-1, a lower O-ring 5-2, an upper seat flange 6-1, a lower seat flange 6-2, a metal outer cylinder 7, a fixed wing 8, a light guide cylinder 9, a light guide cylinder 10, a welding flange 11, a high temperature pad 12, a copper ring 13, a compression flange 14, a quartz inner cylinder 15, a sealing ring 16, a thermocouple sleeve 17 and a thermocouple 18.
FIG. 3 is a practical structure diagram of a photocatalytic tubular reactor according to the present invention;
the reference numbers in the figures are: 1-1 part of a liquid injection port, 1-2 parts of a temperature control port, 2-1 parts of an air inlet, 2-2 parts of an air outlet, 3-1 parts of an upper port connector, 3-2 parts of a lower port connector, 4-1 parts of SAE split flanges, 4-2 parts of SAE split flanges, 5-1 parts of upper O-rings, 5-2 parts of lower O-rings, 6-1 parts of upper seat flanges, 6-2 parts of lower seat flanges, 7 parts of metal outer cylinders, 8 parts of fixed wings, 9 parts of light guide cylinders, 10 parts of light guide columns, 11 parts of welding flanges, 12 parts of high-temperature pads, 13 parts of copper rings, 14 parts of pressing flanges, 15 parts of quartz inner cylinders, 16 parts of sealing rings, 17 parts of thermocouple sleeves, 18 parts of thermocouples, 19 parts of furnace tiles and 20 parts of a heating furnace.
FIG. 4a is a schematic diagram of a quartz inner cylinder in the form of a flat tube reactor.
FIG. 4b is a schematic diagram of a reactor model in which the quartz inner cylinder is a beveled quartz sand plate.
FIG. 4c is a schematic diagram of a quartz inner cylinder in the form of a straight tube sand plate reactor.
Detailed Description
Example (b):
FIG. 1 is a schematic diagram of a photocatalytic tubular reactor of the present invention, where A is a reaction gas inlet, B is a quartz inner cylinder, C is a reaction gas outlet, and D is a light source.
As shown in figure 2, the photocatalysis tubular reactor comprises a liquid injection port 1-1, a temperature control port 1-2, an air inlet 2-1, an air outlet 2-2, an upper port joint 3-1, a lower port joint 3-2, an SAE split flange 4-1, an SAE split flange 4-2, an upper O-shaped ring 5-1, a lower O-shaped ring 5-2, an upper seat flange 6-1, a lower seat flange 6-2, a metal outer cylinder 7, a fixed wing 8, a light guide cylinder 9, a light guide cylinder 10, a welding flange 11, a high-temperature pad 12, a copper ring 13, a pressing flange 14, a quartz inner cylinder 15, a sealing ring 16, a thermocouple sleeve 17, a thermocouple 18, a furnace tile 19 and a heating furnace 20. The metal outer cylinder 7 and the quartz inner cylinder 15 are of a split structure, the metal outer cylinder 7 is sleeved outside the quartz inner cylinder 15, and the quartz inner cylinder 15 can be taken out independently; the left side and the right side of the metal outer cylinder 7 are provided with light guide cylinders 9, light guide columns 10 are arranged in the light guide cylinders, and light passes through the quartz inner cylinder 15 through the light guide columns 10; the upper end and the lower end of the metal outer cylinder 7 are respectively provided with an upper port connector 3-1 and a lower port connector 3-2; reaction gas and reaction liquid enter the reactor from the upper port connector 3-1 and flow out from the lower port connector 3-2 after reaction. The light guide cylinders 9 on the left side and the right side of the metal outer cylinder 7 form a cross structure; the light guide pillar 10 has a T-shaped structure. And the metal outer cylinder 7 is provided with a fixed wing 8. The light guide cylinder 9 and the light guide column 10 are in sealing connection through a flange structure, and the sealing connection structure comprises a welding flange 11, a high-temperature pad 12, a copper ring 13 and a pressing flange 14. The quartz inner cylinder 15 is arranged on the port connector 3-2, the port connector 3-2 is provided with an annular groove, and a sealing ring 16 is arranged in the groove.
The quartz inner cylinder 15 is provided with a flat-mouth quartz reactor, a straight tube sand plate reactor or an inclined plane quartz sand plate reactor for filling a catalyst. The catalyst is positioned in the quartz inner cylinder 15, and the transparent quartz inner cylinder 15 does not influence the illumination and does not contact with the metal outer cylinder 7 to influence the experimental data. The quartz inner cylinder 15 is of a detachable design (the prior applications 201920970907.9 and 201920970911.5 of the applicant of the present invention are incorporated in their entirety as the content of the present invention), and can be used in different styles according to the needs: (1) the flat tube reactor (as shown in figure 4 a) has small catalyst filling thickness and can receive double-sided illumination; (2) the concrete structure of the quartz inner cylinder of the inclined quartz sand plate reactor (as shown in fig. 4 b) is described in the prior application 201920970907.9 of the applicant of the present invention, the inclined surface is provided with a quartz sand plate, the quartz sand plate is designed to be inclined, and the cofferdam is arranged on the quartz sand plate to prevent the catalyst from falling off; the top end of the temperature measuring thermocouple is contacted with the bottom of the quartz sand plate, and the contact part is just the central position of the reactor, so that the central temperature of the reactor can be accurately measured; (3) the straight tube sand plate reactor (as shown in figure 4 c) is provided with sand plates, so that the cost is low and the catalyst loading is large.
The upper port joint 3-1 is sealed by an SAE split flange 4-1, and the lower port joint 3-2 is sealed by an SAE split flange 4-2; the left and right light guide cylinders 9 are sealed by flanges 14; the external connecting pipeline adopts a clamping sleeve structure. The upper port connector 3-1 is provided with a liquid injection port 1-1 and an air inlet 2-1, and the liquid injection port 1-1 and the air inlet 2-1 are both metal ferrule connectors; the lower port connector 3-2 is provided with an exhaust port 2-2, a temperature control port 1-2 and a thermocouple sleeve 17, and the exhaust port 2-2 and the temperature control port 1-2 are both metal ferrule connectors. A thermocouple sleeve 17 is arranged in the temperature control port 1-2, the thermocouple sleeve 17 is a metal blind pipe with one end sealed, and the thermocouple sleeve 17 is hermetically connected with the temperature control port 1-2 by a metal ferrule; the temperature measuring thermocouple 18 is placed in the thermocouple sleeve 17.
Two annular grooves are formed in the outer position of the lower port connector 3-2 and matched with the tight ring 16; and standard straight threads are reserved in the lower port connector 3-2. The metal outer cylinder 7 is a seamless tube made of a high-temperature and high-pressure resistant metal material; the light guide tube 9 is made of high-temperature and high-pressure resistant metal and is welded with the metal outer tube 7. The light guide column 10 is of a T-shaped structure and is integrally formed and made of quartz and sapphire light-transmitting materials.
As shown in FIG. 3, the photocatalytic tubular reactor is clamped with the heating furnace 20 through the fixing wings 8, and the light guide tube 9 and the pressing flange 14 are positioned in the heating furnace 20. The heating furnace 20 is an open furnace, and a cross-shaped groove matched with the reactor is positioned on an opening plane of the heating furnace 20; the heating furnace 20 is controlled in three sections, and the length of the constant temperature area is ensured by supplementing and adjusting the middle section through the upper section and the lower section. The reactor is vertically provided with a fixed wing 8 which is clamped on the upper part of the heating furnace 20. The heating furnace 20 is an open furnace, and a cross-shaped groove matched with the reactor is positioned on an opening plane of the furnace, so that the heating of furnace wires in the middle of the furnace is not influenced; the light-transmitting parts such as the cross light guide cylinder 9, the pressing flange 14 and the like are all positioned in the heating furnace 20, so that the heat dissipation is reduced to the maximum extent; meanwhile, the heating furnace 20 is controlled by three sections of temperature, and the length of the constant temperature area is ensured by supplementing and adjusting the middle section through the upper section and the lower section.
When the photocatalytic tube reactor is used, a light source directly irradiates a catalyst on a quartz inner cylinder 15 through a light guide column 10 in a light guide cylinder 9, and reaction gas enters from an air inlet 2-1 and is discharged from an air outlet 2-2; reaction liquid enters from a liquid injection port 1-1; the catalyst is spread on the top of the quartz inner cylinder 15. The reaction gas introduced from above passes through the catalyst particles, and after reaction, flows out from the exhaust port 2-2, and the catalyst can be sufficiently contacted with the reaction gas in this process. Meanwhile, the quartz inner cylinder can completely receive the illumination from the side direction, the illumination is uniform, and the illumination area is large.
In the experiment, the quartz inner cylinder 15 is positioned in the reactor, and no pressure difference exists between the inside and the outside of the quartz inner cylinder 15, so that the quartz inner cylinder is not broken. The metal outer cylinder 7 and the light guide cylinder 9 are made of temperature-resistant and high-pressure-resistant metal materials, the left light through hole and the right light through hole are sealed by flanges, and the upper port joint and the lower port joint are sealed by SAE split flanges. The high-temperature high-pressure photocatalysis tubular reactor can be illuminated in left and right directions by taking quartz as a catalyst carrier, the long-term use pressure can reach 10MPa at the high temperature of 800 ℃, the limitation that the photocatalysis tubular reactor can only be used for a normal-pressure experiment is broken through, and the research range of the photocatalysis field is expanded.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.
Claims (14)
1. A photocatalytic tubular reactor, characterized in that: the quartz glass tube comprises a metal outer cylinder (7) and a quartz inner cylinder (15), wherein the metal outer cylinder (7) and the quartz inner cylinder (15) are of a split structure, and the metal outer cylinder (7) is sleeved outside the quartz inner cylinder (15); the left side and the right side of the metal outer cylinder (7) are provided with light guide cylinders (9), light guide columns (10) are arranged in the light guide cylinders, and light passes through the quartz inner cylinder (15) through the light guide columns (10); the upper end and the lower end of the metal outer cylinder (7) are respectively provided with an upper port connector (3-1) and a lower port connector (3-2); reaction gas and reaction liquid enter the reactor from the upper port connector (3-1) and flow out from the lower port connector (3-2) after reaction.
2. A photocatalytic tube reactor as in claim 1 wherein: the quartz inner cylinder (15) is provided with a flat-mouth quartz reactor, a straight tube sand plate reactor or an inclined plane quartz sand plate reactor for filling a catalyst.
3. A photocatalytic tube reactor as in claim 2 wherein: the light guide cylinders (9) on the left side and the right side of the metal outer cylinder (7) form a cross structure; the light guide column (10) is of a T-shaped structure.
4. A photocatalytic tube reactor as in claim 3 wherein: and the metal outer cylinder (7) is provided with a fixed wing (8).
5. The photocatalytic tube reactor as set forth in claim 4 wherein: the upper port joint (3-1) is sealed by adopting an SAE split flange (4-1); the lower port joint (3-2) is sealed by adopting an SAE split flange (4-2); the left and right light guide cylinders (9) are sealed by flanges (14); the external connecting pipeline adopts a clamping sleeve structure.
6. The photocatalytic tube reactor of claim 5 wherein: the photocatalytic tubular reactor is clamped with the heating furnace (20) through the fixed wings (8), and the light guide cylinder (9) and the pressing flange (14) are positioned in the heating furnace (20).
7. A photocatalytic tube reactor as in claim 1 wherein: the upper port connector (3-1) is provided with a liquid injection port (1-1) and an air inlet (2-1), and the liquid injection port (1-1) and the air inlet (2-1) are both metal ferrule connectors; the lower port connector (3-2) is provided with an exhaust port (2-2), a temperature control port (1-2) and a thermocouple sleeve (17), and the exhaust port (2-2) and the temperature control port (1-2) are both metal ferrule interfaces.
8. The photocatalytic tube reactor of claim 7 wherein: a thermocouple sleeve (17) is arranged in the temperature control port (1-2), the thermocouple sleeve (17) is a metal blind pipe with one end sealed, and the thermocouple sleeve (17) is hermetically connected with the temperature control port (1-2) by a metal ferrule; the temperature measuring thermocouple (18) is arranged in the thermocouple sleeve (17).
9. A photocatalytic tube reactor as in claim 1 wherein: two annular grooves are formed in the outer position of the lower port connector (3-2), and the annular grooves are matched with the tight rings (16); and standard straight threads are reserved in the lower port connector (3-2).
10. A photocatalytic tube reactor as in claim 1 wherein: the metal outer cylinder (7) is a seamless tube made of a high-temperature and high-pressure resistant metal material; the light guide tube (9) is made of high-temperature and high-pressure resistant metal and is welded with the metal outer tube (7).
11. A photocatalytic tube reactor as in claim 1 wherein: the light guide column (10) is of a T-shaped structure and is integrally formed, and the material is quartz or sapphire light-transmitting material.
12. A photocatalytic tube reactor as set forth in claim 11 wherein: the light guide cylinder (9) and the light guide column (10) are in sealing connection through a flange structure, and the sealing connection structure comprises a welding flange (11), a high-temperature pad (12), a copper ring (13) and a pressing flange (14).
13. A photocatalytic tube reactor as set forth in any of claims 1-12 wherein: the quartz inner cylinder (15) is arranged on the port joint (3-2), the port joint (3-2) is provided with an annular groove, and a sealing ring (16) is arranged in the groove.
14. The photocatalytic tube reactor of claim 6 wherein: the heating furnace (20) is an open furnace, and a cross-shaped groove matched with the reactor is positioned on an opening plane of the heating furnace (20); the heating furnace (20) is controlled by three sections of temperature, and the length of the constant temperature area is ensured by supplementing and adjusting the middle section through the upper section and the lower section.
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| CN201911085807.9A CN110652951A (en) | 2019-11-08 | 2019-11-08 | Photocatalysis tubular reactor |
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| CN111229133A (en) * | 2020-02-29 | 2020-06-05 | 湖南华思仪器有限公司 | Constant temperature furnace for photo-thermal synergistic reaction |
| CN112246201A (en) * | 2020-09-21 | 2021-01-22 | 华中科技大学 | Double-beam double-channel photo-thermal catalytic reaction equipment |
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