CN110514593A - A kind of Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge - Google Patents
A kind of Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge Download PDFInfo
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- CN110514593A CN110514593A CN201910790928.7A CN201910790928A CN110514593A CN 110514593 A CN110514593 A CN 110514593A CN 201910790928 A CN201910790928 A CN 201910790928A CN 110514593 A CN110514593 A CN 110514593A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/0332—Cuvette constructions with temperature control
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
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Abstract
The invention discloses the Energetic Materials by In-Situ Diffuse Reflection devices of a kind of generation and fortifying catalytic agent surface-discharge, are related to infrared spectrum analysis test macro field, including lower case and upper end cover；The lower case and upper end cover form closed space；Infrared light incident window and infrared light exit window are offered on the upper end cover, infrared incident and outgoing unit is by infrared light incident window and the incidence of infrared light exit window and outgoing；High-temperature insulation body is provided in the lower case；The high-temperature insulation position hollow structure, bracket is provided in hollow structure, pedestal upper end is provided with temperature-resistant insulation layer, is provided with high-field electrode and grounding electrode on temperature-resistant insulation layer, it is provided with medium between high-field electrode and grounding electrode, is provided with spherical medium and catalyst between medium.The present apparatus can real-time detection plasma-catalytic surface reaction diffusing reflection in situ.
Description
Technical field
The present invention relates to infrared spectrum analysis test macro, especially a kind of original of generation and fortifying catalytic agent surface-discharge
Position diffusing reflection infrared spectroscopy device.
Background technique
Low temperature plasma-catalysis technique is the method for the degradation volatile organic contaminant of great prospect, but due to anti-
Answer process extremely complex, the mechanism that influences each other between reaction mechanism, reactant is not yet clear.Reaction process is in addition to general
Gas-solid phase reaction, there are also the reaction that electronics, ion, free radical and metastable state molecule participate in, this kind of reaction is very rapid, for research
Bring difficulty.Mainly pass through analysis gas-phase product ingredient, anti-for the research of low temperature plasma-catalytic reaction process at present
It answers rear catalyst characterization to carry out, is to guess intermediate reaction process by analyzing indirect testing result.Even if part researcher
It is reacted using emission spectrum, via Laser-induced Fluorescence Method in situ detection reaction process plasma with vapor-phase reactant,
But these methods cannot detect the surface-catalyzed reactions of plasma participation.However, the surface catalysis that plasma participates in is anti-
Should there are great differences and low temperature plasma-catalysis technique key with gas phase reaction, therefore, it is quite necessary to provide
A kind of device and method of surface-catalyzed reactions process that capableing of the participation of in situ detection plasma.
In conclusion the catalyst surface species knot in plasma environment is capable of providing there are no relevant apparatus at this stage
The in situ detection of structure.
Summary of the invention
The present invention provides the Energetic Materials by In-Situ Diffuse Reflection device of a kind of generation and fortifying catalytic agent surface-discharge, this hairs
It is bright to be achieved by following technical solution:
A kind of Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge, including lower case and upper end
Lid；The lower case and upper end cover form closed space；Infrared light incident window and infrared light are offered on the upper end cover
Exit window, infrared incident and outgoing unit is by infrared light incident window and the incidence of infrared light exit window and outgoing；It is described
High-temperature insulation body is provided in lower case；The high-temperature insulation position hollow structure is provided with bracket, bracket in hollow structure
Upper end is provided with temperature-resistant insulation layer, and high-field electrode and grounding electrode, high-field electrode and ground connection are provided on temperature-resistant insulation layer
It is provided with medium between electrode, is provided with catalyst between medium.
Further, it is additionally provided with electric heating layer in the high-temperature insulation body, is used for heatable catalyst.
Further, it is additionally provided with spherical medium between the medium, is equipped with catalyst on spherical medium.
Further, the external side of the high-temperature insulation is provided with cooling water pipeline.
Further, the high-field electrode is connect with high-field electrode lead；The grounding electrode and grounding electrode lead connect
It connects.
Further, thermocouple is installed in the temperature-resistant insulation layer.
Further, gas vent is offered in the lower case；Gas access is offered on upper end cover.
Further, cooling water inlet and cooling water outlet are opened up on the cooling water pipeline.
Further, watch window is also provided on the upper end cover；Pressure gauge is provided at gas access.
Further, medium is aluminium oxide or quartz glass, and spherical medium is alumina balls, glass marble, quartz ball, iron
Electric body.
It is reaction unit inside spectral device, main body is that the high-temperature insulation body of connection is inlayed with metal shell, internal
It is hollow, and it is placed with a bracket.It is temperature-resistant insulation layer above bracket, there are a spacings with insulator head plane for insulating layer
From for placing spherical medium and catalyst.Insulator body two sides medium required when being electric discharge, top of media and insulation
Body top planes are concordant, and lower part is embedded in insulating layer, so as to the fixation of position.Electrode is placed between medium and insulator body, is situated between
Matter is matched with electrode can carry out dielectric barrier discharge, condition needed for creation is tested.The spherical medium of region of discharge can promote
Surface-discharge makes the surface streamer generated travel to catalyst surface.
The embedded annular electric heating layer of insulator, for being pre-processed to certain catalyst: i.e. in atmosphere of inert gases
Continuous heating several hours to remove the moisture and carbon dioxide gas in catalyst, while can carry out certain journey to catalyst
The activation of degree.Thermocouple is embedded in insulating layer, for the real-time detection to temperature in heating process.Insulator surrounding is surrounded with cold
But pipeline reduces the waiting time of experiment for the catalyst after fast cooling heat pre-treatment.
Closed metal shell outside spectral device, be divided into up and down two parts, top set there are two infrared window,
One watch window and a gas passage；Lower part is then equipped with cable passage, a cooling water inlet, a cooling water go out
Mouth and a gas passage.Two parts are attached shell by the screw of shell surrounding up and down.
Two infrared windows of upper part are located at mutually opposite, to allow IR light beam to pass through and reflect, carry out in situ red
The detection of external spectrum.Glass window positioned at side is held for the discharge scenario during observation experiment and tests specific shape
Condition.The gas passage at top provides inert gas and is passed through, and ensures the gaseous environment in spectral device, while channel side is also equipped with
Air gauge.
The cable passage of lower part of the housing point is located at different two sides, and channel inner cable is separately connected high-pressure polar plate and connects
Ground, cable are in insulating sleeve.Cooling water entrance is located at the two sides of earth cable respectively, and cooling water pipeline carries internal
The heat of reaction process exchanges heat through thus entrance.Lower gas passway is located at below high-tension cable, in spectral device
Thus air is located to be discharged.
Compared with the prior device compared with, the present invention has the advantages that
1. generate low temperature plasma in the form of double-dielectric barrier discharge, the insulator of medium and side is by catalyst
Completely cut off with electrode, avoids the interference of electrode surface high-voltage gradient and the interference of surface charge, while can generate stable
Surface plasma.
2. catalyst is all placed in region of discharge, and spherical medium is added in region of discharge, reduces discharge voltage, promote
Into surface-discharge, make discharge stream light propagation to catalyst layer upper surface, generates plasma-catalytic surface reaction in upper surface
Phenomenon.
3. heating is placed on grounding electrode side and side, the region near high-field electrode is avoided, for region of discharge
While domain provides certain temperature, safety ensure that.
4. realizing to catalyst heat pre-treatment, dielectric barrier discharge, Energetic Materials by In-Situ Diffuse Reflection testing process one
The solution of body simplifies the trivial operations degree that experimenter carries out test experience.
5. being applicable to the detection under various experimental conditions scene, including but not limited to heats and do not heat, generation of discharging
The experiment scene of plasma and condition of not discharging and combinations thereof.
6. providing additional watch window and air gauge, observed in real time convenient for researcher in discharge scenario and spectral device
Air pressure situation understands and controls experiment progress process.
Detailed description of the invention
Fig. 1 is front schematic view of the invention.
Fig. 2 is top view of the invention.
Fig. 3 is the cross-sectional view under the vertical view of internal-response device.
Appended drawing reference is as follows:
1- lower case, 2- upper end cover, 3- infrared light incident window, 4- infrared light exit window, 5- watch window, 6- gas
Entrance, 7- pressure gauge, 8- gas vent, 9- insulating layer, 10- insulating sleeve, 11- high-field electrode lead, 12- high-temperature insulation
Body, 13- high-field electrode, 14- grounding electrode, 15- medium, 16- grounding electrode lead, 17- temperature-resistant insulation layer, 18- bracket,
19- catalyst, 20- spherical medium, 21- electric heating layer, 22- thermocouple, 23- cooling water pipeline, the cooling water inlet 24-, 25- are cold
But water out, 26- seal threaded hole.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In the description of the present invention, it is to be understood that, term " center ", " longitudinal direction ", " transverse direction ", " length ", " width ",
The orientation or positional relationship of the instructions such as " thickness ", "upper", "lower", " axial direction ", " radial direction ", "vertical", "horizontal", "inner", "outside"
To be based on the orientation or positional relationship shown in the drawings, be merely for convenience of description of the present invention and simplification of the description, rather than indicate or
It implies that signified device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore should not be understood as
Limitation of the present invention.In addition, term " first ", " second " are used for description purposes only, it is not understood to indicate or imply phase
To importance or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be with
Explicitly or implicitly include one or more of the features.In the description of the present invention, the meaning of " plurality " is two or
Two or more, unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, term " installation ", " connected ", " connection ", " fixation " etc.
Term shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can be machine
Tool connection, is also possible to be electrically connected；It can be directly connected, two members can also be can be indirectly connected through an intermediary
Connection inside part.For the ordinary skill in the art, above-mentioned term can be understood in this hair as the case may be
Concrete meaning in bright.
It is specifically described first below in conjunction with attached drawing according to an embodiment of the present invention
Referring to figure one, figure two, device upper end cover 2 be in opposite two sides lay respectively infrared incident window 3 with it is red
Glass window mouth 5 is then placed on outer exit window 4, side.The pressure of gas access 6 and side is equipped at the top of device upper end cover 2
Power table 7,1 front of device lower case are to be located in the middle grounding electrode lead 16, the cooling water inlet 24 on both sides and cooling respectively
Water out 25.Device is surrounded by 4 sealing threaded holes, is sealed connection to crust of the device by screw.
Referring to figure one, figure three, the high-field electrode that 1 side of device lower case is equipped with gas vent 8 and is positioned above draws
Line 11, insulating layer 9 and insulating sleeve 10 provide the insulation protection between shell and contact conductor.The resistance to height of the main body of internal-response device
Warm 12 inner hollow of insulator, is inside placed with bracket 18.The top temperature-resistant insulation layer 17 and high-temperature insulation body of bracket 18
12 cooperations, the medium 15 of insulator body two sides is fixed.It is placed respectively between media of both sides 15 and insulator body high
Piezoelectricity pole 13 and grounding electrode 14.The embedded annular electric heating layer 21 of insulator, to heat the catalyst 19 on insulating layer；Insulating layer
Interior thermocouple 22 provides the measurement of temperature；Insulator surrounding is around cooling water pipeline 23.
Catalyst 19 and spherical medium 20 are placed in the sky of the insulating layer composition of tabular medium, the insulator of side and lower part
Between.
The work of the Energetic Materials by In-Situ Diffuse Reflection device of present invention generation and fortifying catalytic agent surface-discharge is described below
Process:
The pretreatment of catalyst is carried out first: opening upper end cover 2, spherical medium 20 and catalyst 19 are placed in high temperature resistant
On insulating layer 17, upper end cover 2 is placed, and pass through thread seal.Inert gas, the discharge dress of lower case 1 are passed through at the top of upper end cover 2
Set interior air.Energization electric heating layer 21, heatable catalyst power off after Chu Liwan and open cooling water cycling switch to urging
Agent 19 is cooled down.Temperature in reaction unit is read by thermocouple 22, it is to be cooled to follow to after preference temperature, closing cooling water
Ring.In special circumstances, it can be pre-processed by vacuumizing.
After pretreatment, infrared light is injected from infrared light incident window 3, in Infrared irradiation reaction unit after catalyst surface
It is projected by reflection from infrared light exit window 4.External equipment receives infrared light, carries out infrared spectroscopy detection.At this point, can incite somebody to action
Inert gas is switched to the gas containing reactant or probe molecule, and keeps continuing circulation status.
Grounding electrode 14 is grounded, high-field electrode 13 accesses high-voltage electricity, and dielectric barrier discharge, the area locating for catalyst occurs
Domain generates low temperature plasma.
The discharge scenario from watch window 5 carries out spectral detection after stablizing.
In the detection process, can different moments are detected at different conditions according to demand, to obtain required map.
Working mechanism based on the present apparatus can obtain the infrared inspection of any moment in plasma-catalytic reaction process
It surveys as a result, real-time plasma-catalytic surface reaction Energetic Materials by In-Situ Diffuse Reflection figure can be obtained.By to catalyst
Surface reaction tracking characterization, analyze infrared spectroscopy in molecular structure information variation, it is convenient to obtain Intermediates and
The information of product provides advantage for the anatomy of reaction mechanism.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
Centainly refer to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any
One or more embodiment or examples in can be combined in any suitable manner.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (10)
1. a kind of Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge, which is characterized in that including under
Shell (1) and upper end cover (2)；The lower case (1) and upper end cover (2) form closed space；
Infrared light incident window (3) and infrared light exit window (4), infrared incident and outgoing are offered on the upper end cover (2)
Unit is incident through infrared light incident window (3) and infrared light exit window (4) and is emitted；
High-temperature insulation body (12) are provided in the lower case (1)；The high-temperature insulation body (12) is hollow structure, hollow
It is provided in structure bracket (18), bracket (18) upper end is provided with temperature-resistant insulation layer (17), and temperature-resistant insulation layer is set on (17)
It is equipped with high-field electrode (13) and grounding electrode (14), medium (15) are provided between high-field electrode (13) and grounding electrode (14),
Catalyst (19) are provided between medium (15).
2. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 1,
It is characterized in that, is additionally provided with electric heating layer (21) in the high-temperature insulation body (12), be used for heatable catalyst (19).
3. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 1,
It is characterized in that, is additionally provided with spherical medium (20) between the medium (15), catalyst (19) are equipped on spherical medium (20).
4. the diffusing reflection infrared light in situ of generation and fortifying catalytic agent surface-discharge according to any one of claims 1 to 3
Spectral apparatus, which is characterized in that be provided with cooling water pipeline (23) on the outside of the high-temperature insulation body (12).
5. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 2,
It is characterized in that, the high-field electrode (13) connect with high-field electrode lead (11)；The grounding electrode (14) is drawn with grounding electrode
Line (16) connection.
6. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 1,
It is characterized in that, thermocouple (22) is installed in the temperature-resistant insulation layer (17).
7. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 1,
It is characterized in that, offers gas vent (8) on the lower case (1)；Gas access (6) are offered on upper end cover (2).
8. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 4,
It is characterized in that, opens up cooling water inlet (24) and cooling water outlet (25) on the cooling water pipeline (23).
9. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 1,
It is characterized in that, is also provided with watch window (5) on the upper end cover (2)；Pressure gauge (7) are provided at gas access (6).
10. the Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge according to claim 3,
It is characterized in that, medium (15) is aluminium oxide or quartz glass, and spherical medium (20) is alumina balls, glass marble, quartz ball, iron
Electric body.
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| CN201910790928.7A CN110514593A (en) | 2019-08-26 | 2019-08-26 | A kind of Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge |
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| CN204768268U (en) * | 2015-05-26 | 2015-11-18 | 浙江大学 | Pharmaceuticals industry waste gas treatment system |
| CN204911182U (en) * | 2015-08-17 | 2015-12-30 | 杭州科瑞特环境技术有限公司 | Ultraviolet ray - plasma is in coordination with degrading organic waste gas device |
| CN109187410A (en) * | 2018-08-30 | 2019-01-11 | 大连民族大学 | A kind of one-part form plasma-catalytic original position diffusing reflection infrared detecting device |
| CN109283151A (en) * | 2018-09-11 | 2019-01-29 | 浙江工商大学 | The device and method of dielectric barrier discharge is realized in a kind of pond in situ of the device of infrared analysis in situ |
| CN210537008U (en) * | 2019-08-26 | 2020-05-15 | 江苏大学 | In-situ diffuse reflection infrared spectrum device for generating and enhancing catalyst surface discharge |
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