CN210533974U

CN210533974U - In-situ infrared spectrum reaction device under free radical clustering atmosphere

Info

Publication number: CN210533974U
Application number: CN201920868018.1U
Authority: CN
Inventors: 刘璐; 邓权进; 吕绮韵; 袁寿其; 糜建立; 王军峰; 王爽
Original assignee: Jiangsu University
Current assignee: Jiangsu University
Priority date: 2019-06-11
Filing date: 2019-06-11
Publication date: 2020-05-15
Anticipated expiration: 2029-06-11

Abstract

The utility model provides a normal position infrared spectrum reaction unit under free radical cluster penetrates atmosphere, include: a housing, wherein a closed cavity is formed in the housing; one end of the nozzle electrode extends into the closed cavity from the top of the upper shell, the other end of the nozzle electrode is positioned outside the upper shell, electrode gas is introduced into the nozzle electrode, and the nozzle electrode is connected with a high-voltage power supply; the observation window and the two infrared light path windows are arranged on the upper shell; the reaction tank main body is arranged in the closed cavity, a first groove is formed in the top of the reaction tank main body, and a gap is formed between the reaction tank main body and the inner wall of the lower shell to form a gas channel surrounding the periphery of the reaction tank; the polar plate is arranged in the first groove and is positioned below one end of the nozzle electrode; one end of the first cable extends into the lower shell and is connected with the polar plate, and the other end of the first cable is grounded; wherein, be equipped with two trachea connectors on the casing down, be used for respectively being connected with intake pipe and outlet duct, the utility model provides a current infrared spectrum detection technology be difficult to satisfy the catalytic reaction sign problem that active particle participated in.

Description

In-situ infrared spectrum reaction device under free radical clustering atmosphere

Technical Field

The utility model relates to a diffuse reflection infrared spectroscopy analysis and test technical field especially relates to a normal position infrared spectroscopy reaction unit under atmosphere is penetrated in clusters to free radical.

Background

The diffuse reflection Fourier transform infrared spectrum technology is a testing technology which can trace and characterize the structure of the surface adsorption species, can conveniently obtain the information of reaction intermediate state and product, and is an effective means for analyzing the catalytic reaction mechanism.

With the development of catalytic technology, low-temperature plasma synergetic catalytic technology is widely researched and applied, the role of active particles in catalytic reaction becomes more and more important, however, at present, few related instruments or devices capable of analyzing the role of active particles in surface catalytic reaction exist, and few devices for performing in-situ characterization on the active particles by adopting infrared spectroscopy technology exist, and the main reason is that a high-pressure plasma discharge device is often needed for generating the active particles, so that difficulty is brought to the design of an in-situ reaction tank.

Therefore, research on an in-situ infrared spectrum reaction cell capable of providing an atmosphere of active particles such as free radicals is urgently needed.

SUMMERY OF THE UTILITY MODEL

Exist not enoughly among the prior art, the utility model provides a normal position infrared spectrum reaction unit under free radical cluster penetrates atmosphere has solved the catalytic reaction sign problem that current infrared spectrum detection technology is difficult to satisfy active particle participation.

The utility model discloses a realize above-mentioned technical purpose through following technological means.

An in-situ infrared spectrum reaction device under free radical clustering atmosphere, comprising:

the shell comprises an upper shell and a lower shell, and the upper shell is hermetically connected with the lower shell, so that a closed cavity is formed in the shell;

one end of the nozzle electrode extends into the closed cavity from the top of the upper shell, the other end of the nozzle electrode is positioned outside the upper shell, electrode gas is introduced into the nozzle electrode, and the nozzle electrode is connected with a high-voltage power supply;

the two infrared light path windows are arranged on the upper shell;

the observation window is arranged on the upper shell;

the reaction tank main body is arranged in the closed cavity, a first groove is formed in the top of the reaction tank main body, and a gap is formed between the reaction tank main body and the inner wall of the lower shell to form a gas channel surrounding the periphery of the reaction tank;

the polar plate is arranged in the first groove and is positioned below one end of the nozzle electrode; and

one end of the first cable extends into the lower shell and is connected with the polar plate, and the other end of the first cable is grounded;

the lower shell is provided with two air pipe connectors which are respectively used for being connected with an air inlet pipe and an air outlet pipe.

Preferably, the electromagnetic heating device further comprises an insulating layer and an electromagnetic heating coil, wherein the insulating layer and the electromagnetic heating coil are located in the first groove, the electromagnetic heating coil is located below the polar plate, and the insulating layer is arranged between the polar plate and the electromagnetic heating coil.

Preferably, the device further comprises a thermocouple, wherein the thermocouple is positioned in the insulating layer.

Preferably, a cable channel is arranged on the lower shell, the first cable is connected with the polar plate through the cable channel, and an insulating outer pipeline is sleeved on the outer side of the first cable.

Preferably, an insulating sealing gasket is arranged on the lower shell corresponding to the inlet of the cable channel, so that the cable channel is closed.

Preferably, a second groove is formed in the inner wall of the bottom of the lower shell, the reaction tank main body is located in the second groove, and the second groove is matched with the reaction tank main body.

Preferably, the distance between the nozzle electrode and the polar plate is 2-15 mm.

Preferably, one end of the nozzle electrode is provided with one or more nozzles.

The utility model has the advantages that:

1. the utility model discloses combined normal position diffuse reflection infrared spectroscopy technique and free radical cluster corona discharge, provided the normal position reaction unit of catalyst surface reaction research under the free radical cluster atmosphere, compensatied the problem that lacks relevant testing arrangement at present

2. The utility model discloses a free radical shower is shot this plasma form of discharging, compares in other plasma forms of discharging, and the nozzle electrode can be led into electrode gas, and required discharge space is little, active particle productivity is high, the regional controllable of discharging. Meanwhile, the free radical shower can generate specific types of free radicals by adjusting the components of the electrode gas, thereby being beneficial to the deep research on the reaction mechanism.

3. The utility model discloses real-time heating and temperature monitoring function have still been integrated, can directly be gone on by this device to the catalyst that needs the preliminary treatment, need not extra equipment.

4. For the whole simplification of realizing the device, the utility model discloses the reaction tank adopts electromagnetic heating, and the permeable insulating layer carries out the direct heating to the polar plate to the realization is to the preliminary treatment of catalyst. The electromagnetic heating device has the following characteristics: 1) the electromagnetic induction heating mode enables the heated body to be heated by electromagnetic induction, so that heat conduction loss does not exist, and compared with a traditional resistance wire heating ring (plate), the power density is high and the heat conversion efficiency is high. 2) The heating body self-heating mode makes the temperature gradient of the heating body in the radial direction smaller, and the catalyst powder is heated uniformly. 3) Compared with an electric heating ring heating mode, the preheating and temperature rising are fast, the heating efficiency is improved, and the time cost is reduced. 4) The electromagnetic induction heating coil is a customized high-temperature wire, has good insulating property, is high-temperature resistant, does not generate heat, does not have the problem of high-temperature oxidation, has long service life and basically has no maintenance cost in the later period.

Drawings

Fig. 1 is a schematic structural diagram of a preferred embodiment of an in-situ infrared spectroscopy reaction apparatus under a free radical clustering atmosphere according to the present invention.

FIG. 2 is a plan view of the reaction apparatus shown in FIG. 1.

FIG. 3 is a top view of the lower shell of the reactor apparatus shown in FIG. 1.

FIG. 4 is a schematic view of the inside of the reaction apparatus shown in FIG. 1.

Fig. 5 is an enlarged view of fig. 4 at C.

Fig. 6 is an enlarged view of fig. 4 at D.

FIG. 7 is an enlarged view of E in FIG. 4

FIG. 8 is a schematic structural view of a reaction tank body according to another preferred embodiment of the present invention.

Reference numerals:

1-upper shell, 2-lower shell, 3-infrared light path window, 4-cable channel, 5-air pipe connector, 6-observation window, 7-connecting screw, 8-reaction tank main body, 9-insulating sleeve, 10-stud, 11-nut, 12-nozzle electrode, 13-insulating outer pipeline, 14-polar plate, 15-insulating layer, 16-electromagnetic heating coil, 17-thermocouple, 18-sealing rubber gasket and 19-first cable.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are exemplary and intended to be used for explaining the present invention, and should not be construed as limiting the present invention.

In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "axial", "radial", "vertical", "horizontal", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used merely for convenience of description and for simplicity of description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.

In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

The following specifically describes an in-situ infrared spectrum reaction device under a free radical clustering atmosphere according to an embodiment of the present invention with reference to the accompanying drawings.

Specifically, referring to fig. 1 to 8, an in-situ infrared spectrum reaction apparatus under a free radical clustering atmosphere according to an embodiment of the present invention includes a housing, a nozzle electrode 12, two infrared light path windows 3, an observation window 6, a reaction tank main body 8, a polar plate 14, an insulating sealing washer 18, and a cable 19.

The casing includes casing 1 and casing 2 down, and casing 1 is the circular cone end cover in this embodiment, and casing 2 is the cylinder shape down, casing 1 with casing 2 is down carried out sealing connection by the screw for form airtight cavity in the casing. The housing in this embodiment is made of an insulating material, and in consideration of the requirements of convenience in processing and sealing, the housing may be made of a metal that is conductive and is not easily heated by electromagnetic heating due to sufficient insulating measures.

As shown in fig. 4 and 5, one end of the nozzle electrode 12 extends into the sealed cavity from the top of the upper housing 1, the other end is located outside the upper housing 1, electrode gas is introduced, and the nozzle electrode 12 is connected to high voltage electricity. The nozzle electrode 12 is in contact connection with an external cable through the stud bolt 10, the high-voltage cable is connected through one end of the stud bolt 10 and fastened by the nut 11, and the lower portion of the stud bolt 10 is also in threaded connection with the nozzle electrode 12. Since the nozzle electrode 12 is electrically connected to a high voltage, the exterior of the nozzle electrode 12 is wrapped with an insulating outer pipe 13 to ensure the safety of the apparatus. One end of the nozzle electrode 12 is provided with one or a plurality of nozzles, and if the nozzles are a plurality of nozzles, the nozzles are arranged in parallel, and the bottoms of the nozzles are positioned on the same horizontal plane. The nozzle electrode 12 also serves as a passage for electrode gas that enters from the other end of the nozzle electrode 12 and passes into the nozzle at one end of the nozzle electrode 12.

Two infrared light path windows 3 are arranged on the upper shell 1, and the infrared light path windows 3 adopt ZnSe, ZnS and CaF₂The infrared detection device is made of materials and used for infrared beam passing and in-situ infrared spectrum detection. The observation window 6 is arranged on the upper shell 1, so that a researcher can observe the discharge situation in real time and know the experiment progress, and the glass of the observation window 6 is quartz glass.

The reaction tank main body 8 is arranged in the closed cavity, and the insulating material in the reaction tank main body is made of high-temperature-resistant insulating material, such as quartz glass, ceramics, resin and the like. Be equipped with the second recess on the bottom inner wall of lower casing 2, reaction tank main part 8 is placed in the second recess, and the second recess cooperatees with reaction tank main part 8 for the second recess provides the stable support of location for reaction tank main part 8.

As shown in fig. 8, the top of the reaction cell main body 8 is provided with a first groove for placing the electrode plate 14, and the electrode plate 14 is matched with the first groove and is located below one end of the nozzle electrode 12. The distance between the nozzle electrode 12 and the polar plate 14 is not easy to be too small so as to leave a gap for placing a catalyst sample; not too wide, otherwise discharge is difficult to occur. Typically, a distance of 1-10mm is left between the nozzle electrode 12 and the catalyst sample, and a distance of 2-15mm is left between the nozzle electrode 12 and the electrode plate 14.

Further, reaction tank main part 8 with be equipped with the space down between the inner wall of casing 2, form and encircle reaction tank main part 8 gas passage all around is equipped with two trachea connectors 5 down on casing 2, be used for respectively being connected with intake pipe and outlet duct, and gas is gone out by the outlet duct after getting into gas passage from the intake pipe again to provide the ambient gas atmosphere for the experiment. The further air inlet pipe and the air outlet pipe are respectively in threaded connection with the corresponding air pipe connecting ports 5 so as to ensure the sealing property of the closed cavity.

Preferably, as shown in fig. 6, the embodiment of the present invention further includes an insulating layer 15, an electromagnetic heating coil 16, and a thermocouple 17, wherein the electromagnetic heating coil 16 is located below the pole plate 14, the insulating layer 15 is disposed between the pole plate 14 and the electromagnetic heating coil 16, and the thermocouple 17 is located in the insulating layer 15, the present invention is implemented by having two cable channels 4, one of which is used for the first cable 19 to pass through, the other is used for the second cable to pass through, and the second cable is connected to the thermocouple 17. The catalyst sample is placed on the polar plate 14, and for the catalyst sample needing to be heated for pretreatment or providing a certain reaction temperature, the catalyst sample on the polar plate 14 is indirectly heated by the electromagnetic heating coil 16 through the heating polar plate, and in addition, the heating temperature is measured in real time through the thermocouple 17 and is adjusted according to the experiment requirement.

Further, as shown in fig. 4 and 7, the lower case 2 is provided with a cable channel 4, and the first cable 19 is connected to the pole plate 14 through the cable channel 4. An insulating outer pipeline 13 is sleeved outside the cable 19, and an insulating sealing washer 18 is arranged on the lower shell 2 corresponding to the inlet of the cable channel 4, so that the cable channel 4 is closed. Because the nozzle electrode 12 and the pole plate 14 are respectively electrified with high voltage and grounded, the electrode gas is sprayed out from the nozzle electrode 12 and directly enters a corona area formed by the pole plate 14 and the nozzle electrode 12, and high-energy electrons collide with the electrode gas and background gas to generate various active particles, so that free radical cluster-jet discharge is formed near a nozzle opening.

The utility model discloses in situ infrared spectrum reaction unit's under free radical cluster penetrates atmosphere working process:

the upper nozzle electrode 12 of the device is connected with high voltage electricity through a high voltage cable, the polar plate 14 is grounded through a first cable 19, the conical end cover 1 is opened, a sample is placed in a sample area on the polar plate 14, the upper shell 1 and the lower shell 2 are hermetically connected, and air in the inert gas discharging device is introduced through an air inlet pipe. Then, the electromagnetic heating coil 16 is started to heat, the sample is heated at 200 ℃, and the sample is pretreated to remove weakly adsorbed species on the surface of the catalyst sample. After the sample is processed, the electromagnetic heating coil 16 is turned off and the sample is waited for cooling.

After the reaction tank is stabilized, infrared light is emitted from one side of the infrared light path window 3, reflected by a catalyst sample above the reaction tank body and emitted from the infrared light path window 3 on the other side, and an infrared spectrum is received and detected by external equipment. In the above process, the inert gas is kept in a continuous flow state. And obtaining a test result by an external infrared light detector, and deducting the initial gas phase background from the test result to obtain a real infrared spectrum.

Then introducing reaction gas from the gas inlet pipe, and measuring infrared spectrum information of the sample in the reaction atmosphere. The nozzle electrode 12 is supplied with high voltage electricity while electrode gas is introduced. The electrode gas is ejected from the nozzle electrode 12 and directly enters the corona region formed by the electrode plate 14 and the nozzle electrode 12, and is decomposed into various active particles by the collision of high-energy electrons, thereby forming radical shower near the electrode gas outlet of the nozzle electrode 12. The free radical shower state can be observed from the glass window 6, and after stabilization, the test information of the sample in the plasma environment under the reaction gas condition is measured.

In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

Although embodiments of the present invention have been shown and described, it is to be understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art without departing from the principles and spirit of the present invention.

Claims

1. an in-situ infrared spectroscopy reaction device under a radical shower atmosphere, is characterized in that, comprising:

A casing, the casing comprises an upper casing (1) and a lower casing (2), the upper casing (1) is sealedly connected with the lower casing (2), so that a closed space is formed in the casing cavity;

A nozzle electrode (12), one end protrudes into the airtight cavity from the top of the upper casing (1), the other end is located outside the upper casing (1), and is fed with electrode gas, the nozzle The electrode (12) is connected with the high voltage power supply;

Two infrared light path windows (3) are arranged on the upper casing (1);

an observation window (6), arranged on the upper casing (1);

The reaction tank main body (8) is arranged in the airtight cavity, the top of the reaction tank main body (8) is provided with a first groove, the reaction tank main body (8) and the lower shell (2) There is a gap between the inner walls of the reactor to form a gas channel around the main body (8) of the reaction tank;

a pole plate (14), disposed in the first groove and below one end of the nozzle electrode (12); and

a first cable (19), one end of which extends into the lower casing (2) and is connected to the pole plate (14), and the other end is grounded;

Wherein, the lower casing (2) is provided with two air pipe connection ports (5), which are respectively used for connection with the air inlet pipe and the air outlet pipe.

2. The in-situ infrared spectroscopy reaction device under a free radical shower atmosphere according to claim 1, characterized in that, further comprising an insulating layer (15) and an electromagnetic heating coil (16) located in the first groove, The electromagnetic heating coil (16) is located below the pole plate (14), and the insulating layer (15) is arranged between the pole plate (14) and the electromagnetic heating coil (16).

3. The in-situ infrared spectroscopy reaction device under a radical shower atmosphere according to claim 2, characterized in that, further comprising a thermocouple (17), wherein the thermocouple (17) is located in the insulating layer (15) .

4. The in-situ infrared spectroscopy reaction device under a free radical shower atmosphere according to claim 2, wherein a cable channel (4) is provided on the lower casing (2), and the first cable (19) ) is connected to the pole plate (14) through a cable channel (4), and the outer side of the first cable (19) is sleeved with an insulating outer pipe (13).

5. The in-situ infrared spectroscopy reaction device under a radical shower atmosphere according to claim 4, characterized in that, an insulating seal is provided on the lower casing (2) corresponding to the entrance of the cable channel (4) Gasket (18) to seal the cable channel (4).

6. The in-situ infrared spectroscopy reaction device under the free radical shower atmosphere according to claim 1, wherein the bottom inner wall of the lower shell is provided with a second groove, and the reaction tank main body (8) It is located in the second groove, and the second groove is matched with the main body (8) of the reaction tank.

7 . The in-situ infrared spectroscopy reaction device under a radical shower atmosphere according to claim 1 , wherein the distance between the nozzle electrode ( 12 ) and the electrode plate ( 14 ) is 2-15 mm. 8 .

8. The in-situ infrared spectroscopy reaction device under a radical shower atmosphere according to claim 1, wherein one or more nozzles are provided at one end of the nozzle electrode (12).